BG110480A - Sensors for scanning probing microscopy, a method of three-dimensional measuing and a method for producing such sensors - Google Patents

Abstract

The invention refers to sensors for scanning probing microscopy (SPM), which offer high precision and resolution of measurement, a method for three-dimensional measurement with such sensors and a method for their production, which, by measuring the variations of the amplitude, the frequency, of the phase difference or of the tunnel current, find an application for the determination of the topography, the geometrical size or some other characteristic of objects in various fields of engineering. The sensors consist of a body, a micro bracket and a probing part, which have a common plane surfacewithin which at least one element is structured for functioning in the form of an orifice and/or a gutter, in which a heterogeneous probing element is positioned in the form of a carbon nanotube (CNT), a boron or boron nitride nanotube, a nanothread, a nanocrystal, etc., including such with a complex form, e.g. a cylinder with a sphere. The method of three dimensional measurement offers the possibility, by using sensors with elasticity in the three directions, with the usual technology of scanning probe microscopy , by measuring in a given point, to determine the characteristics of the samplein the three directions without rotating the sensor and/or the sample under study. The invention involves also a method for obtaining the sensors described in a reproducible and precise manner.

Description

The invention relates to scanning probe microscopy (SPM) sensors that provide high accuracy and resolution in measurement, a three-dimensional measurement method with similar sensors, and a method for obtaining them, by measuring changes in amplitude, frequency, phase difference, or tunneling currents are used to determine topographic relief, geometric size, or other characteristics of objects in various fields of technology. The sensors consist of a body, a microcontroller and a probe having a common planar surface, in which at least one hole-forming element and / or groove is formed, housing a heterogeneous probe element such as a carbon nanotube (CNT), boron or boronitride nanotube, nanowire, nanocrystal, etc., including a complex shape, such as a sphere cylinder. The three-dimensional measurement method makes it possible to use three-way elastic sensors using the usual scanning probe microscopy technique to determine, at a given point in time, the characteristics of the sample in the three directions without rotating the sensor and / or the test specimen. The invention also relates to a method for obtaining the sensors described in a reproducible and accurate manner.

claims, 30 figures

FIG. 9a!

SENSORS FOR SCANNING PROBE MICROSCOPY, THREE DIMENSION METHOD AND METHOD OF OBTAINING SUCH SENSORS

Field of application

The invention relates to scanning probe microscopy (SPM) sensors providing high precision and resolution in measurement, a three-dimensional measurement method with similar sensors and a method for producing them, by measuring changes in amplitude, frequency, phase difference or tunneling current find an application to determine topographic relief, geometric size, or other

characteristics of objects in various fields of technology. In particular, the invention relates to sensors using heterogeneous probe elements, a three-dimensional measurement method and a method for producing such scanning microscopy sensors for use in conventional atomic force microscopy (AFM) systems and scanning tunneling microscopy (STM).

BACKGROUND OF THE INVENTION

Scanning probe microscopy and its most commonly used forms, atomic force microscopy (AFM) and scanning tunneling microscopy (STM), are widely used modern methods for the study and formation of surface images, nanoblast analyzes, manipulations, and more. Image formation with SPM is done by recording the interaction between the sensor and the sample in a network of points pre-defined by the scanning system and typically SPM methods use sensors containing microcontrolls or other types of micromechanical elastic elements with probe elements (also called blades, probes). The microcontroller responds to small effects and thus converts the impact due to the test sample to a measurable amount by bending and changing the characteristics of mechanical oscillation or conducting electrical currents between the sample and the sensor. An example of such a commonly used sensor is shown in FIG. 1. This sensor has a body 1 from which is formed microcontroller 2 of length L, width W and thickness H. The microcontroller has one free end and a corresponding direction of deformation along the Z axis, and a probe end 3 with a probe is formed at its free end. element (probe) P that interacts with the test sample.

The free end of such a micro-bracket under the force F with a direction along the Z axis would deviate at a distance AZ, with the dependence between these two quantities:

F = k.AZ, (1) where k is the coefficient of elasticity, which is determined by the geometric dimensions and the material. For a homogeneous rectangular cross-sectional microconsole, k in a number of sources, for example, US patent 5345815, is described by the dependence

k = EWH ³ / (4L ³ ) _: (2) where E is the Young's modulus (which for silicon is: E = 1.9.10 ¹¹ N / m ² ).

In this case, the microconsole has a resonant frequency F _r of bending along the Z axis, which is

determined by the link:

F _r = ft 162 (E / p) ^{, / 2} .H.L ' ² (3)

Където ·} where p is the material density (for silicon p = 2.3 .10 kg.m ').

The type of interaction between the probe element P and the sample, which takes place in a plane parallel to the surface of the microcontroller, is determined by the shape and composition of the probe element. As a result of the interaction, the microcontroller bends and / or changes the amplitude of the AZ and its oscillation phase. The change in these parameters is detected by various detection methods, such as optical, capacitive, piezoelectric, piezoresistive, etc., known to those skilled in the art.

A number of methods have been developed to obtain probes of various sizes and shapes made of substrate material and physically coupled to the microcontroller. For example, such are disclosed in US Pat.

Typical of methods for producing such sensors is that the probe element is obtained by etching, which is carried out on a dominant part of the sensor surface, except for the probe zones; the sequence of technological steps is long, as the probe elements (probes) are usually first formed, and then the remaining micromechanical elements are obtained on the newly formed surface after etching. In addition, after receiving the structures for the probes, structures with protruding elements are processed, which necessitates the use of special equipment and materials in the next technological steps. In addition, as a consequence of the etching process, there are limitations to the shape and parameters of the blades, which shape is determined by the geometry and orientation of the etching mask, and by the anisotropy and the anisotropy.

9 9 9 9 9 9 99

9 9 9 9 9 9 9 9 99

999 99 9 999 99 9999 • 9 9 9 9 9 99

9 99 9 9 9 9 9 9 9 99 9 the selectivity of the processes used; probes obtained in one etching process are oriented in one direction and for technological reasons cannot be obtained simultaneously with probes with different orientation, which makes it practically impossible to obtain sensors with more than one probe.

To avoid some of the difficulties described above, micro-consoles have been developed that are located entirely in the plane of the substrate. Such utensils are disclosed, for example, in US Patents 5729026 and US 5856672, which use a blade microconsole obtained by photolithography and subsequent anisotropic wet etching without forming a structure beyond the plane of the microconsole. This microconsole can be bent

only in a direction perpendicular to the surface of the substrate, and the position of the blade in the plane of the substrate allows the use of the sensor only at a relatively large inclination to the plane of the specimen under study.

The resolution of a scanning microscope sensor depends on the shape and size of the probe element. A number of carbon nanotube integration (CNT) studies have been performed to substantially improve this resolution in recent years as probe elements. CNTs are the best known blades for their remarkable properties, such as: length to diameter ratio up to 1.10 ⁶ : 1; when defect-free they have great mechanical strength, good electrical and thermal conductivity, huge specific surface area (up to 100 m ² / g for single-wall carbon nanotubes - SWCNT), their properties can be changed by functionalization, and they themselves are chemically stable. It is also known that under certain conditions nanotubes with hemisphere-shaped ends are produced.

Numerous methods are known for obtaining nanotube AFM sensors, e.g. described in US Patents 6346189, US 6401526, US 6528785, US 6871528, US 7048903, US 7138627, all of which use already formed blades from the material of the microconsole, and nanotubes on the blades receive two main approaches:

- high-temperature or other controlled synthesis of nanotubes - in suitable environment on regions (islands) with catalytic properties for synthesis, which regions are located on the blades;

- securing (fixing) of pre-synthesized nanotubes to pre-prepared blades.

Common disadvantages of both the mentioned approaches for creating AFM sensors with nanotubes are the low reproducibility of the end results, due to the low reproducibility of the carbon nanotube detection and orientation processes used in these methods, and the need to use complex and specialized equipment.

For example, patent application US 2008121029 discloses a method of producing carbon nanotube AFM sensors, which sensors consist of a body, a micro-console extending over the body, and a probe-shaped, conical, pyramid-shaped probe section outside the plane of the micro-console. a prism on which a groove is made in the form of a slot, which may also represent an opening. A carbon nanotube is attached to the side wall of the slot.

The sensors obtained by this method are characterized by the fact that the surfaces of the structures on which the CNTs are attached conclude an angle with the plane of the surface of the substrate, which is strictly different from 0 ° and is determined by the slope under which it is formed (formed ) the probe section. The patent application describes several alternative examples of application of the method, from which it becomes clear that the possible angles of inclination of the CNT to the specified surface are defined by a limited number, and a specific, different technological approach is proposed for each particular inclination. In this sense, the method of the cited patent does not disclose a common approach for producing probes with probe elements at different angles, which is necessary in the first place for optimal measurement results, but also for a more efficient process of measurement. production.

The method of fixing the CNT in the aforementioned slot in the said request requires the use of specialized equipment, such as a scanning electron microscope, and the process of this fixation is not precise enough to provide a repeatability of the position of the fixation site, which makes the method difficult to perform. practically.

According to patent application US 2008011066, a method is known for obtaining an AFM sensor consisting of a sensor body, a microconsole, a convex tip and a blade (probe) probe, obtained entirely by photolithographic structuring. Silicon-on-insulator (SOI) plates were used to produce such a device, describing the possibility of obtaining microconsoles of various shapes entirely with photolithographic structuring. The development of modern lithographic methods guarantees the high accuracy and reproducibility of the received according to the cited application. · · · · · · 9 tt • · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · Elements within very wide size limits. However, the method requires special substrate material (SOI plates) and a relatively sophisticated technological sequence. Moreover, in the step of forming a probe element with a tip in a plane other than the initial plane of the substrate by an etching process, it is practically impossible to achieve sufficient reproducibility of the tip position of the probe element, due to the presence of the elongating binder element of the figure,

relative to other sensor elements.

In said patent application US 2008011066, the use of CNTs for AFM sensor blades is mentioned only in the prior art, but as a probe element, which according to the inventors is problematic. This patent neither mentions nor implies that it is possible to form and use grooves and / or holes in the probe, further oriented in a specific manner, as an element to serve for CNT blade insertion.

In patent application WO 2009/000885, a method is disclosed for producing micro-cantilever sensors, which are a bimorphic flat-shaped structure. The blades are shaped by a photolithographic process and are etched strictly along the axis of the microcontroller, and the deformation of the microcontroller is by a bimorph thermocouple and an additional heating element that regulates the length of the microcontroller. In the operating position, this sensor is positioned vertically relative to the surface of the test specimen, the height actuation of the specimen surface being via the heating element. In this case, the preferred deformation plane of the microconsoles is perpendicular to the surface of the substrate. According to the description, the preferred blades are CNTs attached to the end of the probe element. However, this application neither discloses any method of fastening these CNTs as an element of the claimed sensors, nor does it mention or suggest the possibility of using ditches and / or openings for such purpose.

The currently known sensors, having one direction of measurement, find application in conventional scanning probe microscopy methods, which typically use one or two axis scanning systems for surface scanning. The signal from the one-way sensor is used to construct an image of the scanned surface of the object under study, which reflects the interaction of the probe element during scanning with the sample. This type of system examines specimens for which the area of their scanning surface is predetermined, and the direction to reach it is known, and the steepness of the profile of the elements in the same area is limited. When it is necessary to obtain images of portions of the surface of the sample with a complex shape or high steepness, as well as to obtain two- and three-dimensional profiles, the samples are rotated with respect to the measurement direction of the sensor so as to compensate for the impossibility to access these areas from the surface conditioned by the modern sensors and scanning systems used. Thus, because of this restricted access, rotations (displacements) must be made in addition to moving one direction to reach the point to create a three-dimensional image at any point on the surface of the sample in which the measurement is performed. ) to examine each of the other two directions at the same point, including sometimes having to change the sensor when it does not allow such measurement after rotation.

In the patent application US 2008083270 disclosed a system and method for multidimensional

recording and measuring forces for the purpose of multi-directional scanning probe microscopy, in particular a CNT system and method. Characteristic of this measurement method is that it performs displacements on the tip of the probe element in different directions, using different modes of oscillation of the microcontroller - bending and twisting. To obtain a CNT probe at controllable positions with controllable parameters, catalytic synthesis is used on a prepared MEMS structure described in patent US 6146227 of the same inventor. Notwithstanding the idea of a probe portion with several probe elements, illustrated in FIG. 20 of patent application US 2008083270, this application and patent US 6146227 do not disclose any way of obtaining such MEMS with CNTs located on different surfaces of the probe - such a technical solution is absent in these documents. Moreover, as explained in FIG. 20 and FIG. 21 in application US 2008083270, this is an embodiment in which a cylindrical symmetry CNT oscillator is implemented, while the probe part, much less the microcontroller, is not subject to oscillation and this makes it impossible to differentiate the measurement result with the same a probe as shown in FIG. 21, in more than one measurement direction.

Therefore, there is a need to create a micro-console scanning microscope sensor with a probe element providing a high resolution

the ability by which the sensor to perform measurements with high accuracy at the desired angle from the test specimen. In addition, this sensor needs to be improved and its capabilities expanded to overcome the impossibility of

the same sensor to take measurements in two and three directions at one measuring point. There is also a need for an adequate three-dimensional measurement method, using sensors with such advanced capabilities, to quickly and easily make three-dimensional (and two-dimensional) accurate measurements with the usual scanning probe microscopy technique at any particular point measurement without the need for additional steps in the second direction or a new measurement for the third direction to collect all the data at the measured point from the surface and to obtain the complete profile or dimension PhD research model options currently available measuring methods do not provide. There is also a need to develop a common, easy-to-implement and reproducible method to obtain the desired sensor with controllable elastic characteristics and not only with one but also with multiple probe elements at different angles to the axis of the microcontroller, so that to put into practice the advanced capabilities and high resolution and accuracy of the sensor sought.

Description of the invention

Definitions

Unless expressly stated otherwise, certain definitions apply to the description of the present invention and the appended claims, as follows.

The term "functionalizing element" as used herein means a portion of the probe portion formed concave with a constant cross-sectional shape, the slope of the walls and the dimensions of the functionalizing element being sufficient to accommodate a portion of an elongated heterogeneous probe element through self-positioning. The functional element may be an opening or a ditch. In both cases, after placing a heterogeneous probe element in the functionalizing element, the heterogeneous probe element is positioned or self-positioned in a pre-selected position. The functionalizing elements are obtained by masking etching into the single crystalline silicon pad, with or without additional auxiliary layers.

The term "composite groove" as used herein means any indentation that results from at least two separate, independent etching processes, the second of which only covers the bottom of the indentation obtained during the first etching.

The term "heterogeneous probe element" (or only "probe element"), for the purposes of the present description and claims, means an element used to register a particular interaction made from a material other than that of the substrate, such as carbon, boron, boron nitride, zinc oxide and the like, in the form of nanotubes, nanoparticles, Snanonishka, nanocrystals and the like. The heterogeneous probe element may be used as obtained or may be composed of separately obtained heterogeneous moieties, and may also be pretreated to have certain physical, chemical and / or biological properties. In any case, the heterogeneous probe element has a characteristic interaction with the test specimen resulting in a mechanical response of the sensor and / or electrical signal.

The term "elastic micromechanical element" as used herein means a mechanical element of dimensions in the micro or nanometric range, which, because of its shape and the material from which it is made, during conversion with the test specimen converts this interaction into an elastic mechanical deformation. In this specification, depending on the context, examples of elastic micromechanical elements are both the microcontroller and the probe part separately and both together.

The term " elastic micromechanical structure " means an elastic micromechanical element in the intermediate state at the time of its preparation, in which it is already formed on the surface of the monocrystalline silicon substrate common to the sensor of the present invention, or not yet separated by volume or the process of receiving it has not been completed otherwise.

The term "direction of measurement" refers to the process of measurement by the forced oscillation of an elastic micromechanical element with a variable frequency in the frequency range including a resonant oscillation frequency of the elastic micromechanical element. The direction in which, during the measurement in said frequency range, the elastic micromechanical element trembles with resonant frequency is the direction of measurement. When the term "resonant frequency" is used in the present description, "frequency", it should be understood that it refers to the resonance in a bending mode in a given direction of an elastic micromechanical element. Unless otherwise stated, the natural frequency is usually within the frequency range used to operate it.

The terms "control" and "operating" amplitudes refer to the different amplitudes used in different modes by the three-dimensional measurement method according to the invention. The "control" amplitude is large in value, while the "operating" amplitude is small in value.

The term "measuring point" means the position of the sensor relative to the C specimen in which the measurement is made. A "measurement point" is a part of a network of points characteristic of any scanning system, on which the surface of the sample is crawled in accordance with the algorithm of motion of the sensor and / or the sample inherent in the scanning system.

Brief description of the invention

In a first aspect, the present invention relates to a scanning probe microscope sensor comprising a co-formed body with a single crystalline substrate extending from it a micro-console and extending from the free end of the micro-console a probe portion with a probe element. The sensor has a flat probe portion that is flush with the body and the microcontroller, representing their common flat lateral surface. The probe portion includes a free probe end with at least one concave shaped functional element formed therein, in which a long heterogeneous probe element is housed. On the microcontroller and / or probe part for each measurement direction with the scanning probe microscope sensor, there is a separate section with selected geometric dimensions that determines the individual static and dynamic bending characteristics of the microcontroller and / or probe part of the sensor in said direction of measurement. The selection of these geometric dimensions defining the elastic characteristics of the microcontroller and / or the probe portion of the sensor is made in accordance with the resonance frequency differences that are a preferred part of this aspect of the invention.

In other embodiments, the invention discloses scanning probe microscopy sensors with more than one functionalizing element and, respectively, located in

their probe elements having suitably selected geometrical parameter ratios of the elastic micromechanical element of the sensor that allow measurements to be made in more than one direction.

According to the invention, in the scanning probe microscope sensors, elongated heterogeneous probe elements selected from a nanotube, nanowire, carbon, boron or boron nitride nanoparticle, or nanocrystalline zinc oxide, preferably a single nanotube or bundle, are used as probe elements each selected from a single-wall or multi-walled carbon nanotube; boron or boron nitride nanotube. The probe elements may be composed of heterogeneous parts with a spherical, pyramidal or multi-pyramidal configuration, or may be further functionalized for specific applications, including those made with increased electrical conductivity.

In a second aspect, the invention discloses a method of three-dimensional measurement with a scanning probe microscope, on the surface of a sample, in which the sensor and / or the examined sample are moved relative to each other by the scanning microscope system to reach any point from the surface at which performs measurement. According to the invention, a sensor is used with one microcontroller and one probe part having a common flat surface and with individual dynamic bending characteristics without twisting in each of the X, Y and Z directions, which characteristics are different from each other in detection; and the probe portion of the sensor is provided with one or more heterogeneous probe elements, the number of which is sufficient to allow measurement in each of the X, Y and Z directions. During the measurement, the scanning probe microscopy technique and the step-by-step sample controlled displacement reaches a measuring point and then settles into a stationary position. In this position, the surrounding surface located around the probe portion to which the probe reaches during vibration in each of the X, Y, and Z directions is subjected to measurement. The measurement process is carried out without moving the sensor and / or sample by adjusting the microcontroller and the oscillating probe portion, which are implemented sequentially with a working amplitude and / or a control amplitude for each of the X, Y and Z directions and with a frequency in the range containing the resonant frequency for that measurement direction. Data on the result of the interaction with the sample change to

the amplitude, frequency, phase difference or other measured physical quantity shall be counted and processed to obtain the corresponding three-dimensional characteristic of the sample.

In a third aspect, the present invention relates to a method for producing a scanning probe microscope according to the first aspect of the invention, wherein on a single-crystal silicon wafer with orientation (100) having a p-type alloy with a specific resistance of 0.1 to 20 Q.cm or with n-type doping and a specific resistance of 0.003 to 20 Q.cm, at least one upper auxiliary layer is formed and then photolithographically defined surface structuring is performed. Optionally, the surface structuring process may be preceded by the formation on the surface of the plate of at least one concave shaped member for functionalization with a depth of indentation less than the thickness of the free probe end, and then the surface structuring is performed jointly to this concave shaped at least one functional element. In this surface etching by etching, the body of the sensor, the micro-console extending from it, the probe part and, optionally, a centrally arranged concave shaped element for functionalization with a depth of indentation equal to the thickness of the free probe, are simultaneously formed in one plane simultaneously. so that a body and a flat elastic structure are obtained with at least one concave shaped functional element. They undergo structuring of the posterior surface of the silicon substrate, followed by bulk etching and release of the entire sensory structure, while forming an auxiliary planar support structure. In a further step of obtaining the sensors, a heterogeneous elongated probe element is positioned in the at least one concave shaped functional element, which is positioned or self-positioned to the bottom of the concave shaped functional element and fixed to the bottom, finally releasing the finished one auxiliary planar support structure.

In a preferred embodiment of the method for producing scanning probe microscopes according to the invention, at least one concave shaped functional element formed on the surface of the plate is less than the thickness of the free probe end, and is obtained before the process of surface structuring by photolithography followed by at least one etching process.

In another particularly preferred embodiment of the method for obtaining a scanning probe microscope, a single-crystal silicon wafer with a n-type doping and a resistance of from 1 to 20 Q.cm is used, which further comprises pre-constructed and galvanically coupled doped piezoresistive and strong conducting areas. In this case, during the surface structuring, in the process of photolithography, the sections with selected geometrical dimensions of the microcontroller and the probe part are combined with the alloyed areas. Subsequently, piezoresistors are formed in the subsequent masking etching process from these alloyed areas. Further, the production method continues with metallization processes in which, in contact with the highly conducting areas, on the probe part, the microcontroller and the sensor body, connecting metal paths are obtained with terminals for connection to an electrical metering system.

These and other features of the invention and its advantages are explained in detail in the following by way of description and by way of examples which illustrate it without limitation.

Description of the attached figures

Figure 1. shows an axonometric view of a classic micro-console sensor known in the art in scanning probe microscopy.

In FIG. 2. shows an axonometric view of a microcontroller subjected to a force

any direction known in the art.

In FIG. 3. shows a view of a single-direction micro-console sensor along the X-axis with a functional V-groove element.

In FIG. 4. shows a view of a micro-console sensor with a single axis of measurement along the X-axis and with a probe element having an angle of 120 ° with the micro-console axis.

FIG. 5. is a view of a single-axis micro-console sensor along the Z axis with an element for the functional opening of a straight triangular prism.

FIG. 6 is a plan view of a micro-console sensor with one direction of measurement along the X axis and with two probe elements joining different angles with the probe axis.

FIG. 7a, 76, 7b and 7d show variants of sensors of the invention with two measurement directions, of which FIGS. 7a is a view of a sensor with two probe elements along the X and Z axes; 7b is a plan view of a sensor with two probe elements along the X and Y axes; FIG. 7c

is a top view of a sensor with three probe elements along the X and Y axes, the measurement on the Y axis can be done in the opposite and the opposite direction; and Fig. 7d is a plan view of a sensor with three probe elements of different orientation in the XY plane.

FIG. 8a and 86 show variants of sensors of the invention with three measurement directions, of which Fig. 8a is a plan view of a sensor with three probe elements along the X, Y and Z axes; and Fig. 8b is a top view of a sensor with four probe elements along the X, Y and Z axes, the measurement on the Y axis can be done in the forward and reverse directions;

In FIG. 9a shows an axonometric view of a sensor with three measurement directions with four probe elements in three axes: X, Y, and Z, and the measurement on the Y and Z axes can be done in the forward and reverse directions. FIG. 96 shows the frequency response of the normalized amplitude of the mechanical oscillations of the sensor of FIG. 9a in the three directions.

In FIG. 10a shows an axonometric view of a sensor with three measurement directions with a single probe element and piezoresistive vibration detection. FIG. 106 presents an equivalent wiring diagram for connecting the piezoresistors in this sensor; FIG. 10c shows the frequency response of the resistors of the series-connected piezores, and in FIG. South shows examples of probe elements of the sensor of FIG. 10a.

In FIG. 11 shows a structure of a micromechanical sensor for scanning probe microscopy with a functional element aperture in the form of a right triangular prism,

after completion of the surface structuring step.

In FIG. 12a, FIG. 126, FIG. 12b-1 and FIGS. 12c-P show various embodiments of receiving ditches.

FIG. 13a shows the structures of elements of a micromechanical sensor for scanning probe microscopy after completing the surface structuring step obtained jointly for functionalizing elements. FIG. 136 shows such structures in the embodiment of a piezoresistive sensor.

In FIG. 14a shows an axonometric view of a probe portion with a probe end, to which in magnified detail in FIG. 146 and FIG. 14c shows a joint arrangement of the functional elements V-shaped and composite grooves respectively at the probe end.

· · · · - - · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

FIG. 15a shows an axonometric view of the probe portion, and FIG. 156 is a cross-sectional view of the probe end in positioning, including self-positioning, of the probe element in the functional element of the V-groove.

In FIG. 16a is a top view, and in FIG. 166 and FIG. 16c is a cross-sectional view of the probe end of a sensor with a fixed probe element after positioning, including self-positioning, to the two types of grooves, respectively.

Main features and advantages of the invention

A. High precision and resolution sensor

A major feature and advantage of the sensors obtained according to the present invention is that they have a variety of shape and orientation microcontroller elements and probe parts, and their probe elements have a precisely controlled position and length of extension from the probe ends and with a large diameter to A length leading to a resolution of better than 1 nm for microscopic measurements with sensors.

A second main feature of the sensors according to the present invention is that they have micro-console elastic elements that can be bent as desired in one, two

or three directions, which allows one sensor to measure in each of these directions, depending on the application selected. This unexpected and exceptional advantage of the sensors of the present invention is explained by the principle model shown in FIG. 2 and is further demonstrated in the variants of the sensors of the invention. As illustrated in FIG. 2, when the microcontroller 2 bends under the influence of a force of modulus F and components F _x and F _z on the X and Z axes, this force causes displacements at its free end AX and ΔΖ, respectively on the X and Z axes. similarly to equation (1), the dependences are valid:

F _x = k _x .AX, (4)

F _z = k _z .AZ, (4>) where k _x is the coefficient of elasticity on the X-axis, ak _z is the coefficient of elasticity of the microconsole on the Z-axis, which is determined by the geometric shape and material properties. For a homogeneous rectangular-section microcontroller, similar to equation (2), for k _x and k _z , the dependences apply:

k _x = Ea _z .a _x ³ / (4f), (5) • · · * ♦ · · · • »· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

k _r = E. a _x . a // (4 /), (5 ') where a _x and a _z are the microconsole height and thickness parameters respectively.

Moreover, analogous to equation (3), the microcontroller has resonant bending frequencies / _ohms along the X axis and f _oz bending along the Z axis, which are determined according to the equations:

f _ox = 0.162. (E / p) ^t . and _x . I- ² , (6) f _n = 0.162. (E ^/ p) ^I / ² .a _z .f ² (6).

In the case of force with the same modulus components E _x and E _{o, the} ratio between the deformations АХ and AZ, respectively on the axes X and Z, is determined by the equality

ΛΧ / ΛΖ = α ² / α ² (7)

For the ratio of the resonant bending frequencies along the axes X and Ζ, the dependence fox / foz ⁼ l _x / a _g (8) holds.

Therefore, by appropriately selecting the parameters a _y a _g a _d and I, predefined values of the elastic parameters of the microcontroller, such as the coefficient of elasticity and resonance frequency, can be achieved in the He Z directions.

For microconsoles with a more complex shape, it is convenient to sometimes use appropriate characteristic parameters instead of geometric parameters, such as characteristic lengths such as 1 _X and 1 _Y , where the dependencies (5), (5 '), (6), (6') , (7) and (8) remain in force, introducing only an appropriate proportionality factor. Where necessary, the relation between the values of the characteristic parameters and the actual geometrical parameters can be deduced on a case-by-case basis. In the present description, for the sake of clarity, the following dependencies are used to explain the principles underlying the invention.

Similarly, when it is desired to measure in the Y-axis direction, by bending the elastic micromechanical elements along the X-axis and selecting the values of their width and thickness parameters, bending of the probe part with predefined characteristics on the Y and Z axes is realized.

In the sensors of the present invention, which contain both X-axis and Y-axis elastic elements arranged on a common flat surface, by bending the values of the respective parameters, a bending of the probe end with pre-set axis characteristics is achieved. X, Y and Z.

* 4 · 4 ·

4 * ·· · · · »•» ·· 44 «44 *« · 4 * 44

4 4 »4 4 ·· * 4 * 4 ·· ·· * 4 · 4 ··

In addition, it has surprisingly been found that the flat elastic micromechanical element made according to the present invention, which has two or three degrees of bending freedom, and can perform measurements in two or three measurement directions, respectively, with periodic variable-frequency impact a frequency range containing a resonant frequency converts the bending action with the largest amplitude in the direction in which it resonates. Thus, with one sensor and one uniaxial harmonic oscillator, samples can be analyzed in two or three directions of measurement, each direction of resonant deformation being uniquely determined by one corresponding resonant frequency. Therefore, the sensors of the present invention having two and three degrees of bending freedom can be measured extremely simplified, facilitated and rational, since at each measurement point with a change only in the frequency and amplitude of the oscillation, without having to rotate the sensor and / or the sample, or changing the sensor, all directions in which the elastic micromechanical element is able to bend are investigated. Including, unlike existing known SPM sensors that interact with the test sample in a plane parallel to the plane of their substrate, the sensors obtained by the method described in this invention can interact as through a plane parallel to the plane of the substrate , and through planes perpendicular to

the surface of their substrate, i.e., they are optionally sensitive in one, two or three axes.

Another advantage of the flat sensors obtained by the method of the present invention is the ability to position heterogeneous probe elements of suitable shape and properties, both in any direction in the plane of the substrate (plate) and perpendicular to that plane. This eliminates the need for etching of the dominant part of the blade surface, and thus creates the unexpected possibility, through a simplified sequence of process steps, of using commonly used materials and equipment to obtain sensors with extremely reproducible parameters due to the reproducibility of the positioning, orientation and desired optimum propagation length beyond the probe end of the probe elements.

An important advantage of the sensors according to the present invention is the ability to use a variety of probe elements housed in the same functional elements, whereby the type of probe elements is not determinative but only their geometrical parameters are relevant.

B. Three-dimensional measurement method

In modern methods of scanning probe microscopy, the measurement of sensor motion relative to the sample follows an algorithm of crawling the surface of the sample over a network of points determined by the scanning system used. Point-by-point crawling is characterized by 6 _lt steps identical or different for each scanning direction. This crawl is also customary in the method of the present invention. During the three-dimensional measurement according to the present invention, the sensor used, the elastic micromechanical element of which possesses the characteristics described in the invention, is brought to a forced torsion mode without twisting. Characteristic of this process is that the amplitude of oscillation of the free end of a micromechanical element with a probe depends on the intensity of the periodic impact on the sensor. On the other hand, under the same other conditions, the amplitude of the forced oscillation of an elastic element oscillating with a variable frequency in the range of about

the resonance is significant, e.g. up to more than one hundred times the amplitude of the same oscillation outside the said range. In other words, for a fixed intensity of periodic impact, changing only the frequency of the forced oscillations of the elastic micromechanical element having elasticity in all three directions X, Υ and Ζ, only at frequencies close to (or in the range of) any of the resonant , it will flicker with increased amplitude in the corresponding direction. Therefore, at a sufficiently close distance from the probe element of the test sample, an interaction will occur between them only in one of the mentioned resonance frequency ranges. As a result of the interaction, the characteristics of the oscillations that are recorded and / or electric tunneling current change. In this case, there is an unambiguous relationship between the frequency at which the interaction is recorded and the direction in which the interaction occurred - this is the previously known direction in which the elastic micromechanical element resonates for a given frequency.

In the method of three-dimensional measurement according to the present invention, forced oscillation is used to cause the elastic element to bend with two substantially different magnitudes (magnitudes) of amplitudes: 1) "control", large in value, used ♦ »• 9

to initially detect the interaction between the probe element and the scanned surface, and 2) a "working" one that is 10 to 200 times smaller than the control amplitude, preferably about 100 times smaller, used for surface scanning high resolution. Both oscillation amplitudes are obtained by varying the intensity of the periodic impact.

The relation between the amplitude of the forced oscillation and its frequency for a given intensity of external influence is described by a continuous function. This makes it possible to determine the difference Mi between the amplitudes of the forced oscillations with a frequency equal to the resonance one and with frequencies outside the range of the resonance in the ith direction of measurement normalized to the intensity of the impact. This value for each measurement direction is characteristic of the sensor and is used to determine step A, the scanning system in the direction in question, when initially reaching the surface, keeping the ratio:

At = sM _t (9) where ε is the coefficient characterizing the relationship between the displacement step A · from the scanning system and the difference Mi between the amplitudes in each particular direction / in which accidental contact is avoided.

When scanning a high resolution surface in each of the

the three possible directions, the intensity and frequency of the forced oscillation at a frequency close to the resonance one, are chosen so that the oscillation with controlled amplitude is performed.

When measuring with a sensor capable of bending in all three directions by the three-dimensional measurement method of this invention, two operating modes are used in succession: 1) a mode of reaching a measuring point in which the sensor is forced to oscillate in the frequency ranges including the resonance frequencies for each of the scanning directions X, Y and / or Z. Initially, the amplitude of this oscillation changes from operating to control, and after reaching a magnitude customary for the measuring system used and at Sllovia that is not registered with the interaction model simultaneously flicker sensor starts to move relative to the sample to reach a point in which registers interaction. The direction of the recorded interaction is then determined by the frequency range in which this interaction is achieved, and the oscillation amplitude changes again from the control. · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · Working, and moving continues in the defined direction until reaching the measuring point, which is the first point reached at which the interaction of the probe with the sample at oscillation with operating amplitude; and 2) a measurement mode in which, at the point reached, its surrounding surface is measured, with the sensor and / or sample stationary. For this purpose, after reaching the measuring point, oscillations of working amplitude and frequency range containing the resonant frequency for that direction are initially made in the measurement direction, determining the value of the quantity characterizing the interaction of the probe element with the sample surface. Further, the scan is continued in the perpendicular directions in the manner described for the first direction, while at the same time accounting for and processing the data of the resulting change in amplitude, frequency, phase difference, or other measured physical quantity for interaction with the sample. of the corresponding three-dimensional characteristic of the specimen.

A significant and unexpected advantage of the measurement method described so much is that oscillations of different amplitudes can be applied at each measurement point - from operating to control and without rotating or changing the sensor by varying the intensity of the periodic influence and / or frequency range at one point all directions in the oscillation figure can be investigated when oscillating the micromechanical elastic part with the probe element (s). This provides the necessary information for both the object under study and the execution of the sample scan algorithm. Thus, according to the three-dimensional measurement method of the present invention, a sample for each point can be comprehensively examined in a single, simple and convenient measurement process with a single sensor. At the same time, flexible measurement algorithms are used, which are not limited by the shape of the specimens and are operated without the need for prior information about them, as in the methods used so far, requiring approximately known for example distance, profile inclination, concave shape, etc. .

In this way, by means of the three-dimensional method with the sensor of the present invention, using at each point of the scanning network the combination of oscillations with different amplitudes in different directions in the bending mode, scans and characterizes samples with a surface in any direction of measurement j with profile steepness limited only by the ratio of the mentioned difference in amplitudes Mi and the step of scanning in the transverse direction φ ± /.

Thus, by using flat elastic micro-console structures, in which elements with precisely defined dynamic elastic characteristics and sensitivity in three directions can be created, it is possible to realize this simple and convenient method of three-dimensional measurement of the surface of samples.

C. Method for obtaining sensors for scanning probe microscopy

The main technological and systemic advantage of the method for producing the sensors according to the invention is that since the body, the microcontroller and the probe part are obtained in the plane of the plate, the method allows to use the usual photolithographic structuring, and in doing so can to produce various, including multiple, different probe elements on a single micro-console sensor according to the intended application of the sensor and the entire measuring system. Also, the basic parameters of the micromechanical elements obtained by the method, namely a _x , 1 _X , and _y and 1 _Y , are determined by a single photolithographic process and do not depend on the displacement between different photolithographic levels. Insofar as photolithography techniques used in practice allow these parameters to be obtained with sufficient uniformity on a single plate and reproduced from plate-to-plate with high accuracy, this creates the possibility of producing high-precision sensors used. for high-resolution scanning microscopy with reproducible setpoints.

Another significant advantage of the method described for the production of micro-cantilever or other deformable elements of micromechanical sensors is that it allows to obtain simultaneously elements with different ratios between their geometric characteristics a _x , 1 _x , a _y , 1 _Y and a _g , and hence to realize sensors having a direction of measurement along each of the X, Υ and Ζ axes, with a corresponding different frequency range.

Another advantage of the method according to this invention is that since there are no convex structures in the sensor acquisition process, the mounting of the probe elements is performed uniformly on the upper surface of the sensor by uncritical positioning or self-positioning, and subsequent fixation. At the same time, the method allows the use of probe elements with extremely high values of • · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · The ratio of longitudinal / transverse size, their length extending beyond the probe end 1 _P, varies widely, without the need for it. different treatment of the sensory structure.

Examples of carrying out the invention

A. Scanning probe microscopy sensor

Example 1 - One-way sensor

In FIG. 3 shows an example of a preferred embodiment of a scanning probe microscope according to the present invention with one measurement direction, which consists of a body 1 extending from it a micro-console 2 and a probe part 3. The probe part 3 extending from the microcontroller at a distance of l _t outside the body 1, with a probe element 4, permits interaction through a surface perpendicular to the plane of the plate.

The micro-bracket 2 according to the invention has a micro-bracket connecting part 5 which unites it with the body 1 and has a height a _x that may be smaller than in the present example or equal to the height of the micro-bracket 2. The free end of the micro-bracket 2 is connected to the probe portion 3 extending therefrom, the axes of these two elements intersect at point C defining the characteristic length of the microcontroller / _x> which represents the distance of the intersection point C from the body 1. When said two elements are coaxial, laid the point C is defined by the position of the probe element 4.

The probe portion has a free probe end 6 in which a functional element is arranged in the form of a V-shaped groove 7 intersecting the surrounding wall 8.

The body 1, the microcontroller 2 and the probe part 3 with the free probe end 6 are formed simultaneously from a common single crystal semiconductor substrate of silicon, and are located in a plane representing their common flat lateral surface, free of convex parts. This flat microconsole 2 is characterized by the fact that when its geometric characteristics obey the ratio:

a _d > 2.a _x (10) where a _x is the height of the micro-console connecting part 5, and aa _z is the thickness of the micro-console 2, then this micro-console, according to dependences (7) and (8), has a larger deformation AX and respectively, a lower resonant frequency of oscillation along the X axis, compared

with those of the Z axis. This makes it possible, by selecting the appropriate values of the parameters a _g , a _x and 1 _X , an elastic micromechanical element in a given frequency range of measurement, to have only one resonant frequency and, accordingly, one direction of measurement along the axis X , in which the probe element 4 is provided in the measuring direction.

According to the present invention, the probe elements 4 used in the sensors are stand-alone, finished elongated elements with an extremely small radius or cross-sectional size and a diameter-to-length ratio of about 1: 500 to 1: 5000. The probe elements are heterogeneous - they are made of a material other than the substrate material, which may be carbon, for example, single-walled (SWCNT) or multi-walled (MWCNT) cylindrical carbon nanotubes (CNTs), but other elongated heterogeneous carbon elements may be used e, boron or boron nitride

material, such as nanoparticles or nanowires, zinc oxide nanocrystals and the like. Any elongated heterogeneous elements or bundles thereof, including complex configuration elements, for example a nanotube ending in a sphere, a pyramid, a multi-pyramidal shape or the like, which may be composed or produced in a single process by heterogeneous elements, may be suitable also that the heterogeneous probe elements are pre-treated to have certain physical, chemical and / or biological properties. In the present example, the probe element is a conductive single-walled carbon nanotube having a diameter-to-length ratio of about 1: 500. In other preferred embodiments of the invention, the use of SWCNT bundles is preferred.

The self-elongated heterogeneous probe element 4, placed in the functional element V-shaped groove 7, intersects unilaterally the surrounding wall 8 of the protruding portion of the free probe end 6. The V-shaped groove is obtained as a result of its orientation in the process of production in the direction { 110} on the single crystal support. The orientation of the probe element 4 coincides with the orientation of the functional element V-groove 7, and the positioning accuracy of said probe element is determined by the accuracy of receipt of the functional element.

This embodiment of the sensor is particularly suitable for measuring specimens for which the probe element is substantially orthogonal to the test surface of the specimen.

· «

Another embodiment of a one-way sensor is shown in FIG. 4. It consists of a microconsole 2 with a characteristic length of 1 _X and a _{x a} size of the microconsole connecting part 5, and a probe part 3 with a free probe end 6. In this embodiment, the probe part 3 and the functional element - composite groove 9 with a depth d _t , are oriented such that the axis of the probe portion 3 concludes with the axis of the microcontroller 2 an angle β, which can be of arbitrary value in the range of 30 ° to 180 °, and in the present example, the angle β is preferably equal to 120 ° . This embodiment of the sensor is particularly suitable for measuring specimens for which it is essential to have direct visual observation of the area of interaction of the probe element with the specimen.

In FIG. 5 shows another embodiment of the sensor according to the invention, with a probe element 4 arranged perpendicular to the plane of the common flat surface of the sensor in an aperture functionalizing element 10. Similarly, the sensor consists of a body 1 extending from it a microcontroller 2 united with the body 1 by means of the micro-console connecting portion 5, and extending from the micro-console 2 the probe part 3, which are located in a plane representing their common flat lateral surface having no protruding parts. Flat microconsole 2 is characterized by the fact that when its geometric characteristics obey the ratio:

a _x > 2.a _g (11) where a _x is the width of the micro-console connecting part 5 and α _ζ is the thickness of the micro-console 2, then this micro-console, according to the dependences (7) and (8), has a greater displacement the free end Λ Ζ and, accordingly, a lower resonant frequency of oscillation on the axis Ζ, than those on the X axis. This is made possible by the selection of appropriate values of the parameters a _g , a _x and 1 _X , the elastic micromechanical element in a frequency range of measurement shall have only one resonant frequency and one direction of measurement respectively the axis Ζ in which the probe element is oriented in the direction of measurement.

The orientation of the probe element 4, as shown in the enlarged axonometric part of FIG. 5 is determined by the arrangement of the element for functionalizing an aperture 10 in the form of a triangular prism having an inclination of the surrounding walls defined by the etching process. As is known to those skilled in the art, etching methods exist, such as 99 · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·

for example, τ. so-called Bosch process that produces a reproducible vertical slope with an accuracy of better than ± 2 °.

In FIG. 6 is an illustrated variant of the sensor, which, although having two elements for functionalizing component ditches 9 and 9 'and having two probe elements 4 and 4', has a substantially different application based on the fact that the probe elements have a common intersection point A 'on its axes beyond the probe part 3 in the direction of measurement of the sensor. When this intersection A 'is the point of interaction with the test specimen, such a sensor is suitable for simultaneously measuring two characteristics of the specimen, or for measuring the effect of the presence of one probe on the signal of the other, and of measuring the effect of the presence of the sample on the interaction between the probes. For this purpose, the two probe elements 4 and 4 ', at angles 0 and 0' relative to the axis of the probe portion, respectively 5G and 37 ', are different in appearance and properties when the sensor is intended to measure two different characteristics of the but may also be identical in cases where the method of examining the sample is based on its influence on the interaction between the two probes. As in the previous embodiment, the lengths of the probe members 4 and 4 'are predetermined. In this example, it is not necessary to differentiate the interaction of the two probe elements, since the measurement is only in one direction.

© Example 2 - sensor with two measurement directions

In FIG. 7a is an illustrated variant of a sensor of the present invention having a micro-console having a characteristic length 1 _X in the direction Υ and height a _x of the micro-console connecting portion 5, and the probe part 3 with a free probe end 6 having two functional elements: a functionalizing element V-shaped groove 7 and functional element aperture 10.

This sensor variant is characterized by the fact that the relations (10) and (11) are not simultaneously fulfilled, and the two parameters a _x and a _d are approximately equal but different, ie:

a _x »a _g , noa _x / a _g (12), where a _x and α _ζ are respectively the height and thickness of the micro-bracket, as indicated in FIG. 7a and the enlarged detail thereto.

«4

444 * · 4 »·· • 4 4 4 44 4 * 444 • *« «· · * ··· · · * 4 * 4 · * 4 44 * 4

4444 44 44 ·· ·· 44

In this embodiment, at a given thickness a _o by a suitable selection of the characteristic length 1 _X and height a _x , the desired elastic characteristics of the sensor whose microcontroller 2 has approximately equal bends in the X and направ directions are achieved. Including, the parameters are chosen so that the ratio:

β.ίΛτaz), in which y is a coefficient in the range of 0.1 to 10, preferably 0.2 to 1.0,

characterizing the method for recognizing the measurement direction from the frequency response of a selected parameter (e.g., the amplitude of the forced oscillation) in bending of a micromechanical element, which is known in each particular measurement case, f _ox is the resonant frequency of the microconsole 2 when bending. its free end in the direction X, f _oz is the resonant frequency of the microconsole 2 when bending its free end in the Z direction, and Q is the average of the quality factor of the microconsole for the directions of measuring X and Z. Thus, the microconsole 2 with the free probe end 3, for which both relations (12) and (13) are fulfilled simultaneously, have bending resonance frequencies f _ox and f _oz along the X and Z axes, which are close in value , but clearly discernible. Accordingly, a sensor with such a construction of the microcontroller 2 and the free probe end 3 with two probe elements 4 and 4 ', as shown in FIG. 7a, has two measurement directions along said axes and with it at each point on the grid of scans can be made in these two directions.

Additionally, each bending of the microcontroller 2 and displacement of its free end 3 in the plane XZ can be represented as an equivalent sum of components along the two mutually perpendicular measurement directions - X and Z. Any oscillation with frequency / of such microcontroller can be considered as the sum of two independent oscillations with the same frequency in both directions, the ratio of the amplitudes of the two components being constant for each frequency f outside the resonance range f _ox and f _oz . Accordingly, for two measurement directions in the specified frequency range, the normalized oscillation amplitude in the resonance direction is greater than the normalized amplitude in the non-resonance directions. Thus, when in the direction of measurement, the probe element interacts with the test object

in a different way compared to the interaction in another direction by another probe element located on the same microcontroller. As a result, the nature of the oscillation changes and / or an electric tunnel current is recorded.

When the axis of the probe part 3 concludes with the axis of the microcontroller 2 an angle β equal to 90 ° and the two axes are oriented in the direction {NO}, the only functional element in which the probe element oriented along the axis X is located is the functionalizing element V a ditch 7 with depth d _t and the other element for functionalizing aperture 10 is a right triangular prism, as shown in Fig. 7a. When said orientation is different, the functional element for measuring along the X axis will be a composite groove.

Another preferred embodiment of the invention is shown in FIG. 76. In this case, the sensor has a microcontroller 2, a probe part 3 with perpendicular axes (angle β - 90 °) and two functional elements V-shaped grooves 7 and 7 \ These elements are located at the free probe end 6 of the probe part 3, which in this embodiment is formed by an additional expanded portion located in the same plane. The functional elements of the V-shaped grooves 7 and 7 'are oriented such that the axes of the two probe elements 4 and 4' having a thought intersection A falling in the central part of the probe part 3 are angled 0 and 0 'relative to the axis of the probe portion 3, and may be from 0 ° to 180 °, respectively.

Examined by itself, the probe portion 3, with a rectangular narrowing probe portion 11, of a width a _y , a free probe end 6 with an additional extended section and a characteristic length 1 _Y , defined as the distance of point A from the beginning of the microcantle 2, for which is fulfilled by the ratio Arg.au (10 ') has a higher normalized bending along the axis Υ and, accordingly, a lower resonant oscillation frequency on this axis, compared to those on the axis Ζ, which allows measurements on both axes to be be amplitude and frequency differentiated and. For a given thickness a ₂ , the elastic characteristics of this variant of the sensor according to the invention, including the resonant bending frequency f _oy of its probe portion 3 along the Y axis, are determined by the width a _y and the characteristic length / _y .

Thus, the microconsole 2 with the probe portion 3 of the sensor shown in FIG. 76, in which the relations (10) and (10) are simultaneously observed at the suitably selected parameters a _y , 1 _X and 1 _Y have, on the X axis, close but different resonance frequencies. In addition, any deformation in the plane XY can be represented as an equivalent sum of the components of the two mutually perpendicular measurement directions, respectively, of X and Y. Therefore, for a given frequency range of measurement, with suitably selected values of the parameters _x and _y , 1 _X and 1y, an elastic micromechanical element is obtained with various, including close values of the resonant frequencies f _ox and f 'y of the mechanical oscillations in the X and Y. directions. is independent oscillations with the same frequency in both directions, the ratio of the amplitudes of the two components being constant for each frequency f outside the resonance range f _ox and f _oy . Accordingly, for two measurement directions in the specified frequency range, the normalized oscillation amplitude in the resonance direction is greater than the normalized amplitude in the non-resonance directions. Thus, in this direction, which is the direction of measurement, the probe element interacts with the object being studied in a different way compared with the interaction in another direction performed by another

a probe element located on the same microconsole.

When the axes of the functionalizing elements are oriented in the direction {110} of the silicon single crystal substrate, the cross-sectional shape of these two functionalizing elements are V-shaped grooves 7 and 7 '. Since the probe elements 4 and 4 'are heterogeneous and there is no limit to their type, they may be the same or different in appearance and size. In the specific example, as shown in FIG. 76, lengths of the probe elements 4 and 4 \ representing single-conductive carbon nanotubes are such that they extend beyond the probe portion of the predetermined distance 1 _pixels and 1ru from an imaginary intersection point A on their axes, oriented such that point A to fall in the central part of the probe part 3.

Thus, it is possible to use the described sensor to scan and characterize specimens with variable surface area in each of the X Y directions with a profile steepness limited by the ratio of the difference in amplitude in the respective direction and the scanning step in the transverse direction, as described

above.

A third embodiment of the invention with two measurement directions is shown in FIG. 7c. In this case, the sensor has a microcontroller 2 and a probe portion 3 with perpendicular axes (angle β = 90 °) and three functional elements arranged parallel to the plane of the plate, which are respectively positioned at the probe end 6, which has two additional extended sections. The axes of the three probe elements 4, 4 * and 4 "having an intersecting intersection point A are at an angle θ, θ 'and Θ" relative to the axis of the probe portion 3, and are 90 ° or 180 °, respectively. Since the functional elements are oriented in the {110} direction, they are V-shaped grooves of 7, 7 'and 7, respectively. Although this sensor has three probe elements, it can measure in two directions, and therefore two of the probe elements are coaxial but in a mutually opposite direction to its axis.

A fourth embodiment of the invention with two measurement directions is shown in FIG. 7d. In this case, the sensor has a microcontroller 2 and a probe part 3 with perpendicular axes (angle β = 90 °) and three functional elements arranged parallel to the plane of the plate in the common surface, which are respectively placed in a probe end 6 with two additional extended portions . The functionalizing elements are oriented such that the axes of the three probe elements 4, 4 'and 4 "having a thought intersection A are arranged at an angle θ, Θ'μ Θ" with respect to the axis of the probe part 3, and may be from 0 ° to 180 °, respectively. When at least one probe element is oriented in a direction other than {110}, the functional elements are integral grooves 9, 9 'and 9', which can also be arranged in a metal layer. Although this sensor has three probe elements and no two of them are coaxial, as explained above, it can measure in two directions, respectively X and съответ.

Example 3 - sensor with three measurement directions

In FIG. 8a shows a variant of a sensor according to the invention having three probe elements. The probe elements 4 and 4 'are arranged in a plane parallel to the plane of the plate, similar to that shown in FIG. 76 sensor, and the probe element 4 "'is perpendicular to said plane. The microconsole 2 has a characteristic length of 1 _X in the Υ direction and the height a _x of the microconsole connecting part 5 and has a probe part 3 · · · · · · · · · · · · · · · · · »· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · Β · · · · · · · · having a width a _y and a characteristic length 1 _y . Two additional extended sections are formed in the free probe end 6 and three functional elements are created, two of which are V-shaped grooves 7 and 7 ', and one is an opening 10 that is oriented so that the axes of the probe elements 4, 4 'and 4 "' conclude with the axis of the probe part 3 angles θ, θ 'and 0"' equal to 180 ° or 90 °, respectively. When necessary or preferred, the functional elements are V-grooves, their axes are oriented respectively in the direction {110} of the silicon single crystal support. The three probe elements 4, 4 'and 4 "' extend beyond the grooves, respectively, in each of the directions X, Y and Ζ at distances of 1 _px , 1 _PU and / _p . As in Example 2, the heterogeneous probe elements may be the same, including in terms of their electrical conductivity, or different in type and size, with their propagation lengths predetermined relative to the intersection A of the axis of the probe elements 4, 4 '. and 4 ”. As a general preferred variant, different heterogeneous probe elements are suitable to be used when investigating the topography and orientation of magnetic domains or thin multilayer structures with different properties of the individual layers, for example, electrical conductivity, magnetic permeability, leading to different structure properties in different directions.

In FIG. 86 and FIG. 9a shows a variant of a sensor with four probe elements arranged in three mutually perpendicular axes. In this case, too, when the axis of the microcontroller 2 and the axes of the functionalizing elements are oriented in the direction {110} of the silicon single crystal substrate, the functionalizing elements are V-shaped grooves of 7, 7 'and 7, respectively. Because of the ability to accurately control the position of each of the functional elements and the probe elements provided by the present invention, they may be obtained such that the axes of the functional elements of the V-shaped grooves 7, 7 'and 7 "have in common thought intersection A into which an element for functionalizing an aperture 10 is formed, representing a right triangular prism arranged so that the axis of the probe element 4 '' inserted therein passes through said intersection point A. Moreover, the probe elements 4, 4 ', 4 ”and 4”' is extended beyond the elements functionalization, respectively, in each of the axes X, Υ, Ζ, such as axes Υ and Ζ are located in the downlink and uplink, and their edges are located at distances of length l _{px, py} l, lp. _y , l _pz and 1p. _d determined from the intersection A of the four probe elements. As in the previous examples,

· « e • »· • • · • • · • ♦ · · • ··· • · · ·· * • • • · · ··· ♦

«·» «· · · • * · · • · · · · · · · · ·

heterogeneous probe elements 4, 4 ', 4' and 4 '' may be selected to be the same, including in terms of their electrical conductivity, or different in length and appearance.

In FIG. 9a shows an axonometric view of a scanning sensor in the X, Y, and Z directions in which heterogeneous probe elements may have the same or different propagation lengths from the total intended intersection A of their axes to the edges of each of the extending probe elements . Since the distance from the intersection point A to the end of the corresponding probe element and the distance of interaction between the probe element and the sample are known, this makes it possible to calculate the geometric shape of the test sample in the corresponding direction. Also, the detected signal is used to correct the translational translation of the sensor in the measurement direction, to maintain a constant value of the amount characterizing the interaction with the sample, in the specific example it is the forced oscillation phase, but may also be the amplitude or frequency.

Figure 96 shows the type of frequency dependence of the normalized differences in the amplitudes M1. Similar to the previous examples, the frequency at which it is

a registered change in mechanical oscillation or a tunnel current is detected, recognition of the direction of interaction of the probe element with the specimen is achieved.

This sensor is suitable for probing complex three-dimensional samples.

Surprisingly, for the sensors of this invention, it has been found that with a single micromechanical element, the profile of one-dimensional, two-dimensional or three-dimensional objects can be determined, the dimension of the determination coinciding with the number of measurement directions. As long as the elastic characteristics of the sensors in each of these directions can be altered by the geometric parameters of the microcontroller in the different directions, the corresponding natural frequencies in these directions can be set to be close, but uniquely different.

In FIG. 10a shows an axonometric view of an integrated scanning microscope sensor with three measurement directions, similar to that shown in FIG. 9a, which sensor has only one heterogeneous probe element selected alternatively from the heterogeneous probe elements 4, 12 or 12 'shown in FIG. South. To record the interactions of this probe element, piezoresistive sensor elements are used in each of the three measurement directions, which include five highly alloyed regions 13, which make galvanic contact with the corresponding edges of successively connected regions with piezoresistive properties 14, 14 'and 14'. These sensing elements change the value of the flexural resistance of the probe end in the corresponding X, Y, and направ directions. In the readings of FIG. 10a, the three piezores 14,14 'and 14' are connected in series by four contact openings 15 and three metal paths 16 to the contact pads 17 and 17 '. In this variant of connection, measurement with an external measuring device is only the sum of the resistance value of the three piezo resistors, but other ways of connection are possible, depending on the application

of the sensor.

FIG. 106 illustrates an electrical wiring diagram of the three piezoresistors shown in FIG. 10a, and the type of RMS of the resistance Rn-ir measured between terminals 17 and 17 'is shown in Fig. 10c. As can be seen, this resistance has three expressed maxima, corresponding to the resonant bending frequencies of the micromechanical construction of the sensor. With the same oscillation amplitudes in different directions, these maxima may be the same or different depending on the parameters of the piezo resistors, their location on the elastic trace elements and the method of production. Regardless of the ratios of changes in the values of the individual resistances, by measuring the impedance Rn.n <, the above-described changes in the oscillations of the micromechanical elements as a result of the interaction of the probe element with the sample in each of the measurement directions can be recorded. In a preferred embodiment of the invention, the changes in piezo resistor values at the same amplitudes of displacement of the free end of the microcontroller in the X, Y, and Z directions are the same.

The variants of heterogeneous probe elements shown in FIG. South illustrate some preferred embodiments, for example, a heterogeneous probe element 4 representing a hemispherical end CNT, 12 is a heterogeneous probe element made up of coupled cylindrical and spherical parts, and 72 'is a heterogeneous probe element made up of micro / nanocrystalline coupled cylindrical part properties and pyramidal or multi-pyramidal shape.

• · · ·

• · · · ·

The resolution of the sensor with probe element 12 is determined by the diameter of the sphere and such a sensor is suitable for measuring the dimensions of three-dimensional objects of unknown shape. The resolution of the probe element 12 'is determined by the radius of curvature of the pyramidal tips of the micro / nanocrystal.

Similar to the previous examples, the frequency at which a change in the oscillation characteristics or a tunneling current is detected by measuring the total resistance is obtained, recognizing the direction of interaction of the probe element with the sample. Since the extension length of the probe element beyond the functional element is known, this makes it possible, by measuring with this sensor, to determine the geometric shape of the test specimen in the respective directions, with a resolution determined by the diameter of the probe element.

In addition, in another preferred embodiment of the invention, each of the sensors described in Examples 1, 2 and 3 and illustrated in Figures 3, 4, 5, 6, 7a, 76, 7b, 7d, 8a, 86 and 9a, may be provided with piezoresistors, further included in its elastic micromechanical element, with the corresponding, clear to those skilled in the art, the adaptation conditioned by the particular sensor construction, as disclosed above.

B. An example of performing a three-dimensional method with a scanning microscope sensor

At the beginning of the three-dimensional measurement process, a scanning probe microscope system equipped with a three-probe sensor having one microcontroller and one probe portion having a common flat surface, with individual dynamic bending characteristics without twisting in each X direction, Y and Z, which are distinguishable from each other by detection, are in the initial position relative to the specimen. The probe portion of said sensor must be provided with a sufficient number of heterogeneous probe elements to provide measurement in each of the X, Y and Z directions. This may be like a sensor having a heterogeneous probe element which is sensitive in the three measurement directions X, Y and Z, such as the sensor of the present invention shown in FIG. 10a and other types of sensors, such as variants of sensors of the invention, in which the probe portion may be provided with three or four heterogeneous probe elements, such as the sensors shown in FIG. 8a, 86 and 9a. Then

the system is set to reach a measurement point across the network from scan points and is forced to vibrate with an amplitude that changes from operating to control. When registering the first interaction of the probe element is the sample whose frequency range in which this interaction is registered determines its direction j, where j ex, y or z, and stops the forced oscillation with a control amplitude. The mode of reaching the measurement point in the established direction of interaction j is then continued, but already with the operating amplitude. This process continues until the interaction with the sample is recorded when the movement of the sensor and / or sample from the scanning system is stopped. The position thus obtained from the sensor is the measuring point at which the sensor and the sample remain stationary and goes into measurement mode in the direction of reaching the point. For this purpose, the sensor is periodically exposed to a working amplitude in the j direction and the value of the physical quantity characterizing the interaction is determined. The sensor is then switched to the jitter mode in the perpendicular directions j ± l, varying the intensity and / or frequency range of the impact so that the oscillation amplitude in these directions changes smoothly from operating to control to eventually detect interaction with the sample. Thus, while maintaining the constant selected physical quantity, the sample is scanned according to the selected measurement algorithm. By analyzing the actuator control signal, which maintains a constant value of the quantity characterizing the interaction between the probe element and the sample, the properties of the surface of the sample in the respective direction are investigated. The data on the resulting change in amplitude, frequency, phase difference, or other measured physical value, such as tunneling current, are read and processed to obtain the corresponding three-dimensional characteristic of the sample.

In a preferred embodiment of the three-dimensional measurement method of the test sample, the physical quantity characterizing the interaction is maintained constant by controlling the intensity of the corresponding periodic impact.

C. Example of a method for producing a high-resolution scanning microscope sensor

The method of obtaining sensors for scanning probe microscopy according to the present invention is three-step and therein for the substrates from which the sensors are obtained, • r

use silicon wafers with orientation (100), having a p-type of doping and a specific resistance in the range of 0.1 to 20 Q.cm, or a p-type of alloying with a specific resistance in the range of 0.003 to 20 Ω.αη, as their main technological section is orientation [110].

P-doped monocrystalline silicon wafers are used when the sensors they receive according to the present invention are intended for use in scanning systems with optical detection of the interaction between the probe element and the sample, or tunnel current sensing systems.

When it is desired to obtain piezoresistive scanning probe microscopy sensors, mono-crystalline silicon wafer substrates with an alloy tip and specific resistance in the range of 1 to 20 Q.cm, on which surface highly alloyed regions are preformed be obtained by various methods known to those skilled in the art and in galvanic contact with them piezoresistive areas located on the surface and / or in ditches obtained by, for example, the method disclosed in patent application BG 110397.

Each plate prior to performing the processes of the process of the present invention, as is customary in the art, must be prepared by pretreatments, including chemical treatments known to those skilled in the art, to perform subsequent oxidation, etching, etc. processes on them. ., as described below in the embodiment of the method.

Surface structuring

According to the present invention, in the first step of the method, the pad is subjected to surface structuring processes. For this purpose, two-sided oxidation of the silicon wafer 18 is initially carried out, forming a layer of silica 19, which is used as a mask in subsequent surface and bulk structuring processes. The silicon wafer thus treated is then subjected to structuring processes through a photolithographic mask to form elastic structures by sequentially etching the silica layer and the substrate in the shaded regions 25 to a predetermined depth _g , as shown in FIG. 11.

In this structuring, the structures of the micromechanical elements are simultaneously obtained and shown in FIG. 11 element for opening aperture

10, when provided. This may be the only element for opening 10, as in the embodiment, shown in FIG. 5, or one of the functional elements as in the embodiments shown in Figures 7a, 8a, 86, and

9a. When sensors are provided with elements for the functionalization of the openings 10, the etching process is selected and carried out at the stage of surface structuring so that the walls are as close as possible to perpendicular to the surface of the plate, since the slope of the opening walls subsequently determines the slope of the displacement in him

heterogeneous probe element.

In a particularly preferred alternative embodiment of the method of the invention, in contrast to methods known previously and practiced in the art, when it is contemplated to use probe elements arranged in a plane parallel to the plane of the substrate, firstly on the prepared single-crystal silicon wafer, functional elements V-shaped or composite grooves, of suitable dimensions and orientation over selected areas of the surface of the pad. This is done on a pre-prepared single crystalline silicon pad 18, as shown in FIG. 12a, additional layers for functionalization are grown and deposited, and the substrates are first subjected to high temperature oxidation on both sides, which can be done in any manner known to those skilled in the art. The thickness of the silica layer 19 is such that it performs the function of a mask for the surface and bulk structuring of silicon according to the description of the method of the invention below.

In a preferred embodiment of the method, for the production of randomly oriented heterogeneous probe elements disposed on the surface of the sensor micro-console, as shown in FIG. 12a, two thin layers 20 and 20 'are applied to the layer of silicon dioxide 19 on the face of the substrate by a suitable, customary, physical or chemical process to form a groove, but in some cases it is desirable be more than two. The thin layers 20 and 20 'in the present case are titanium with a thickness of 20 nm and gold with a thickness of 200 nm, and a photoresistive layer is applied to these layers. Other materials may also be used, e.g. conductive, such as titanium nitride, imparting conductive properties to the surface of the single crystalline silicon wafer. Then, an appropriately oriented photolithographic mask is structured to produce an opening with the desired • in the photoresist.

rectangular shape and orientation. A controlled sequential etching of the resulting layers is then carried out through the mask thus obtained to obtain the desired section profile of the functionalizing element, forming a composite groove 21 of size g in the surface layers 20 and 20 ', as shown in FIG. 12a. In addition, each upper layer is a mask for etching of the next layer below, thus obtaining the desired shape of the composite groove. The thickness of the layers, the size g of the auxiliary groove 21 and its orientation with respect to the other micromechanical elements of the sensor are determined by the size of the heterogeneous probe elements to be used in the particular sensor according to its application, as well as by other specific requirements thereto. Such are, for example, the requirements for wetting the surface of the material while fixing the heterogeneous probe element to the corresponding permissible maximum temperature known to those skilled in the art.

The orientation of this structure with respect to the crystallographic directions of the silicon substrate 18 is arbitrary.

In a preferred embodiment of the groove functionalization processes shown in FIG. 126, when it is desired to obtain V-shaped grooves 7, a photoresist is applied to the single-crystalline silicon substrate with the built-in oxide layer 19, which is used as an etching mask. The desired photolithographic mask is then structured, and the images from which the functional elements will be obtained are oriented in the {110} direction of the single crystalline silicon substrate. The layer of silicon dioxide 19 is then etched through this mask, the size of the photolithographic mask a being transferred to the layer of dioxide, and a window 22 of rectangular shape of size a and orientation of its sides in the directions {110} of the monocrystalline silicon substrate are obtained, as is shown in FIG. 126. The thus obtained structured layer of silica is a mask for the subsequent etching of the grooves 7 in the silicon pad to a predetermined depth. In this preferred embodiment, the functional elements to be obtained are V-shaped self-limiting ditches. The preparation process is self-limiting when wet anisotropic etching of the monocrystalline silicon substrate with orientation (100) into potassium hydroxide (KOH) occurs. This groove is characterized by the fact that its walls have a crystallographic orientation <111>, its bottom is parallel to the surface of

the substrate and its depth d _t is determined by the size a specified in photolithographic structuring.

In another preferred embodiment of the first step of the method of the invention shown in FIG. 12c-1 and FIG. 12c-P, where it is desired to obtain a sensor with heterogeneous probe elements arranged in a random direction in a plane parallel to and below the level of the surface of the plate, wherein the functional element is a composite groove on the prepared single crystal a silicon substrate with a built-in oxide layer is applied a photoresistive etching mask. Analogously to the previous embodiment, photolithographic structuring of a rectangular b-shaped etching mask of arbitrary orientation is then performed so that the image is oriented in the desired direction for the application of the sensor, as shown in FIG. 12v-1. The size b is determined mainly by the diameter of the probe element that is desired to be mounted in the functional element. The silica 19 is then etched through the available mask, whereby the size of the mask b is transferred to the structured layer of silica, forming a window 23, and the dioxide is used as a mask for subsequent etching of the groove in the single crystalline silicon substrate. The silicon pad 18 is then etched isotropically through the thus obtained mask of a structured layer of silica 19 having aperture size b, wet or dry, respectively, to form a region 24, whereby the size of this area expands to the size b 'as shown in FIGS. 12c-P.

Subsequently, anisotropic dry etching is carried out through the same silica mask, whereby a window 23 of size b is projected onto the bottom of the area 24, thus forming a secondary groove 23 'which is part of the bottom of the composite groove 9 , as shown in the enlarged detail of FIG. 12c-P. Second etching is performed at low pressure, such as reactive ion etching (RIE).

For the functional element of the composite groove 9 obtained by means of the mask with an aperture 23, it is essential that its axis is of arbitrary orientation, its depth d _t is determined by the characteristics of the probe element 4 and the function of the sensor, and its bottom is parallel to the surface of the pad.

Further, an essential process of alignment is performed for the method of the invention, in which the photolithographically determined image in a photoresist is aligned with the already existing functional elements so that the elements for

functionalize to intersect unilaterally the surrounding walls of the corresponding protruding portions of the probe end.

Where it is desired to obtain piezoresistive scanning probe microscopy sensors and, accordingly, n-type alloy plates are used in which surface high-alloyed areas and piezoresistive areas in galvanically contacted ditches have been obtained in advance by photolithographic placement for etching on the surface of the plate in the implementation of all of the above variants of the method of obtaining elements for functionalization, further combining of these masks to piezoresistive and highly alloyed areas obtained previously on the silicon wafer.

In FIG. 13a shows the structure obtained after performing surface structuring processes, whereby individual elements such as the body 1, the microconsole 2, the probe end 6 and the functional element 10 are formed simultaneously by vertical etching in the shaded regions 25 to a predetermined depth a _z through combined with pre-received ditches 7 or 9, photolithographically defined mask.

In a variant of the method for producing piezoresistive detection sensors similar to that shown in FIG. 10a sensor, additionally providing for the alignment of the micromechanical elements of the microcontroller 2 with the connecting part 5 and the probe end 3, to the highly alloyed regions 13 and to the regions with piezoresistive properties 14, as shown in FIG. 136.

Since the alignment between the two photolithographically structured layers forming the combined elastic structures allows for wide tolerance, the sensors thus obtained have reproducible parameters.

It will be appreciated by those skilled in the art that these processes can be accomplished in various ways, and in the method of the invention it is preferable to use a conventional positive photoresist applied by the conventional centrifugal spreading method. The type and shape of the possible specially shaped flat elastic elements which may be obtained at this stage are not limited.

Obtained after the etching depth d _t elements for functionalization in the form of V-shaped or 7 compound 9 ditches on newly formed flat elastic

micromechanical structures lying in one plane are shown in axonometric form in FIG. 14a and the enlarged details of FIG. 146 and FIG. 14c. As already stated, when the groove axis is in the {110} direction, such groove is V-shaped, while in all other cases it is composite.

The cross-sectional view of the V-shaped groove 7 surrounding wall 8 of the free probe end 6 is shown in FIG. 146. An essential feature of the method of the invention is that the depth of the V-shaped grooves d, and the position of the probe element determined by it, are determined by their width a. In particular, when the width of the zone in the silicon dioxide given by photolithographic structuring is of size a and the etching depth of the microcontroller a _z is such that the equality a _r = a is valid. tg 54.7 ° (14) then in this case the depth d _t of the groove 7 is equal to half the thickness of the micro-bracket a _z .

As a result, the method of this invention created the unexpected possibility of obtaining grooves with reproducible parameters, including a horizontal bottom, at a predetermined distance from the surface of the substrate, in the middle at a thickness a _z of the free probe end 6.

The cross-sectional view of the component groove 9 surrounding wall 8 of the free probe end 6 is shown in FIG. 14c. An essential feature of such a structure obtained by the method of the present invention is that its orientation may be arbitrary. This produces a common planar structure of the probe end 6 with the functional groove element 9. This combined structure allows the installation of a variety of heterogeneous probe elements arranged in different directions having different functional characteristics.

In a preferred embodiment of the method of the invention, when the sensor comprises both a functional element V-shaped groove 7 or a compound groove 9, and an opening 10 in the form of a right triangular prism as the sensors shown in FIG. 7a, FIG. 8a, FIG. 86 and FIG. 9a, the functional element of the aperture 10 is aligned with the functionalities of the grooves so that in the aperture 10 there is a planed intersection point A of the axes of the functionalizing grooves already created on the processed single crystalline silicon structure and the sequential etching of the silicon layer and the pad is made to the specified depth a _z . Further, the elastic structure thus obtained is treated similarly to the other sensors of the present invention.

When it is desired to obtain sensors for scanning probe microscopy with piezoresistive detection, after performing the processes described above, metallization processes are further carried out, in which contact metal paths are obtained on the probe part, microcontroller, and body of the sensor in contact with the probe part, microcontroller conclusions. These metallization processes are performed in ways known to those skilled in the art.

Bulk microstructuring of elastic micromechanical structures

The thus treated single crystalline silicon structure is subjected to photolithographic structuring processes of the silicon dioxide layer on the back surface of the substrate, subsequent bulk etching on the back side of the silicon wafer to achieve a predetermined thickness of the residual layer and release of the elastic elastic elements from the elastic elastic elements a foundation that can be done in any manner known in the art. In addition, during the bulk structuring, an auxiliary supporting planar structure is obtained, which laterally connects and holds the individual sensors to each other, normally obtained simultaneously on one substrate in one technological cycle.

Positioning and positioning, including self-positioning of heterogeneous probe elements with subsequent fixation to the bottom of the functional elements

In the functionalizing elements of the elastic micromechanical elements obtained in the previous step, the heterogeneous probe elements are then inserted and self-positioned, and then the heterogeneous probe elements are fixed to the bottom of the functionalizing elements.

The implementation of the process of inserting and positioning probe elements in the functional elements is possible in a variety of ways known to those skilled in the art. In FIG. 15a shows a particularly preferred method of producing a sensor with a longitudinal heterogeneous probe element, using a functional element V-shaped groove 7. In the groove, a heterogeneous probe element 4 of cylindrical shape and of small diameter, in the case of a carbon nanotube, is inserted into the groove (CNT) or a bundle of such nanotubes. Other elements may be used, for example boron or boron nitride nanotubes, nanocrystals, nanowires, nanowires, or complex configuration elements having an elongated cylindrical portion. Since the diameter of the carbon nanotube is multiple, typically several hundred to a thousand times smaller than the width a of the groove, the nanotube is positioned at the bottom of the groove or self-positioned and falls on that bottom itself, as shown in FIG. 156. In the particularly preferred self-positioning variant, it is sufficient before positioning the carbon nanotube probe element to be positioned relative to the width of the carbon nanotube.

the ditch with an accuracy equal to half the size a.

Similarly, the positioning of the elongated cylindrical heterogeneous probe element is carried out when the formed functional element in the elastic micromechanical element is a composite groove 9. It is sufficient before positioning that the pipe is positioned with respect to the width of the groove to an accuracy equal to half. of the size b 'of the compound groove.

The positioning of the heterogeneous probe elements in the functionalities of the apertures 10 is carried out by initially orienting the sensor vertically so that the inner edge of the prismatic aperture containing the point A through which the probe element will pass is at the lowest position relative to the surrounding walls of the hole. The probe element is then inserted with the selected micromanipulator into the orifice and positioned or self-positioned to the lowest located inner edge. However, it is sufficient before positioning the nanotube to be positioned with respect to the hole with an accuracy equal to half the size of the side of the prism.

After placing the elongated cylindrical heterogeneous probe elements, they are fixed to the bottom of the ditches by applying a suitable coating 26. It is necessary for the coating 26 to have good adhesion to the material of the functional element - the ditches 7, 9 or the opening 10, as shown in FIG. 16a.

When positioning the heterogeneous probe element 4 along the axis of the functional element 7, 9, or 10, a length of 1 _P of the portion of the probe element 4 extending beyond the probe end is pre-set.

In a preferred embodiment of the method of the invention shown in FIG. 166, the coating 26 is deposited in the groove 7 on the already positioned and positioned at its bottom

cylindrical probe element 4. Depending on the ease of implementation, the fixation of the probe elements can be accomplished optionally by different methods and by using an appropriate amount of material for each probe element.

Similarly, in another preferred embodiment of the method, the CNTs, CNT bundles or other probing elements 4 having suitable properties are fixed by applying a suitable coating 26 having good adhesion to the material of the composite groove 9, as is shown in FIG. 16c. Depending on the ease of implementation, the fixation of the probe elements may be optionally accomplished by different methods and by using a suitable amount of coating material for each probe element 26.

Probe elements may be mounted on the functional elements including by known state-of-the-art fixation methods such as local electron beam welding in the scanning electron microscope camera and any other known and applicable method. These alternatives are particularly used to realize the attachment of the probe element 4 '' to the openings 10 in the form of a right triangular prism.

In this manner, arbitrary stand-alone probe elements or bundles of such elements having suitable application-specific properties may be affixed and fixed. In addition, different probe elements can be mounted in the micro-console structures with their associated functional elements.

Finally, the ready-made sensors are separated from the supporting auxiliary planar structure, which can be done in various ways known in the art.

A scanning probe microscope sensor comprising molded

Claims (13)

A scanning probe microscope sensor comprising molded Claims jointly with a single-crystal support body extending from it a micro-console and extending from the free end of the micro-console a probe part with a probe element, characterized in that the probe part is flat and in alignment with the body and the micro-console representing them common flat lateral surface; the probe portion comprising a free probe end having at least one concave shaped functionalizing element formed thereon, in which a heterogeneous probe element is arranged, the axis of which is arranged parallel to or on a common flat surface, and on the microcontroller and / or on the probe part for each X, Y and / or Z direction of measurement with the micromechanical probe sensor, there is a separate section with selected geometric dimensions, determining individual dynamic and static bending characteristics. and the microcontroller and / or probe portion in the appropriate direction of measurement. A scanning probe microscope sensor according to the preceding claim, characterized in that the concave shaped functionalizing member is a groove with a depth less than the thickness of the free probe end, or an opening with a depth equal to the thickness of the free probe end, wherein the groove shape is V-shaped or composite, said groove having a lengthwise cross-section and lying parallel to the plane of the common flat surface; and the opening is in the form of a right triangular prism, and is perpendicular to the plane of the common plane surface, wherein each concave shaped functional element has a wall inclination and a cross-sectional dimension sufficient to provide self-positioning of the cavity element placed in the concave functional element . A scanning probe microscope sensor according to claims 1 and 2, characterized in that there are geometric dimensions of the detached portions of the microcontroller and / or the probe portion, determining individual resonant frequencies for each X, Y and / or Z measurement direction, which for each two measurement directions are selected according to the resonance frequency difference dependencies: • * • 9 Y · Q '(foj ~ foj + 1) —foj foj / foj + i ⁼ a _o j / a _o j + i, in which γ is a coefficient in the range of 0.1 to 10, preferably 0.2 to 1.0, characterizing the selected a method for recognizing the direction of measurement by frequency response when bending a micromechanical elastic member; foj is the resonant frequency of the microcontroller or probe portion when bending in the j direction; foj + i is the resonant frequency of the microcontroller or probe portion when bending in the j + 1 direction; Q is the average of the quality factor of the microcontroller and / or the probe part for the measurement directions / and y + /; a _O j and a _O j + i are the defining geometric dimensions of the microcontroller and / or the probe part, respectively. A scanning probe microscope according to any one of the preceding claims, characterized in that two functional elements are formed on the free probe end, the axes of which are at an angle less than 180 ° with an intersecting intersection point beyond the probe end in the direction of measurement. A scanning probe microscope sensor according to claims 1, 2 and 3, characterized in that the probe portion is provided with a connecting part joining the free probe end and the microcontroller, and at least one additional laterally expanded portion in the free probe end with a second functionalizing element formed thereon, in which a heterogeneous probe element is placed, wherein the axes of the two functionalizing elements are arranged at an angle of less than 180 ° with an intersecting intersection in the central portion just on the free probe end. A scanning probe microscope sensor according to claim 5, characterized in that the additional laterally extending portions with the functional elements formed thereon are two, with elongated heterogeneous probe elements placed therein, such that the axes of the three functional elements have in common an intersecting point intersecting the central portion of the free probe end, and each of the elongated heterogeneous probe elements concludes with an axis of the microcontroller an angle in the range of 0 ° to 180 °. A scanning probe microscopy sensor according to claims 5 and 6, characterized in that an element for functionalization is formed in the central region of the free probe end in the form of an opening into which the intended intersection of the axes of the other functional elements falls. and the axis of the heterogeneous probe element extending into the aperture extending at least unilaterally from it passes through the intended intersection of the axes of the other functional elements. A scanning probe microscope sensor according to any one of the preceding claims, characterized in that it is provided with one to four, optionally identical or different, elongated heterogeneous probe elements with a longitudinal axis of symmetry and a ratio of average transverse size to length in the range of 1:10 to 1: 5.10, selected from a nanotube, nanowire, carbon, boron or boronitride or nanocrystalline nanoparticle, or composed of heterogeneous spherical, pyramidal or multi-pyramidal parts, or having an additional specific function lysed, preferably are single nanotube or a bundle of homogeneous nanotubes, each representing a single-or polyhedral carbon nanotube including conductive; or boron nanotubes; or boron-nitride tubes. A scanning probe microscope sensor according to any one of the preceding claims, characterized in that the selected geometric sections further comprise: piezoresistors converting the deflection of the free probe end and / or the microcontroller in each measurement direction into an electrical quantity, located in the plane of the common plane surface and in planes perpendicular to it; and highly alloyed regions through which the piezoresistors are in galvanic contact with metal paths formed on the body, microcontroller and probe part, the metal paths being provided with terminals for connection to an electrical measurement system. 10. A method of three-dimensional measurement with a scanning probe microscopy sensor on a surface of a sample, in which the sensor and / or the examined sample are moved relative to each other by the scanning microscopic system to reach any point on the surface in which the measurement is performed, characterized by with the use of a sensor with one microcontroller and one probe portion having a common flat surface and individual dynamic bending characteristics without twisting in each of the X, Y and Z directions, which characteristics are different ne of another № upon detection; the probe portion being provided with one or more heterogeneous probe elements sufficient to provide measurement in each of the X, Y and Z directions, whereby, upon reaching the respective point from the measuring surface, the sensor and the sample are fixed in motion. position and measure the surface of the probe surface, stepwise in each of X, Y and Z directions, without moving the sensor and / or sample, by adjusting the microcontroller and probe part in a vibrating manner sequentially with operating amplitude and control amplitude for each of the X, Y, and Z directions and with a frequency in the range containing the resonant frequency for that measurement direction, and the data of the resulting change in amplitude, frequency, phase difference or other measured physical quantities are counted and processed to obtain the corresponding three-dimensional characteristic of the sample, Method for the production of a scanning probe microscope according to any one of claims 1 to 9, characterized in that it has a p-type alloy with a specific resistance of 0.1 to 20 on a single-crystal silicon wafer with orientation (100). Q.cm, or with n-type doping and a specific resistance of 0.003 to 20 Q.cm, the processes of: forming at least one upper auxiliary layer are successively performed; surface structuring, optionally photolithographically coupled to a pre-formed at least one concave shaped element for functionalization with a depth of indentation less than the thickness of the free probe end, after which the plate is etched, in which plane simultaneously forming the body of the sensor, the microcontroller extending from it, the free probe end and optionally, a centrally located concave shaped element for functionalization with a depth of indentation equal to the thickness of the free probe end, yielding a body and a flat elastic structure with at least one concave shaped functional element, which is subjected to the structuring of the rear surface of the silicon substrate with subsequent bulk etching and release of the entire sensor structure , while forming an auxiliary planar support structure; thereafter, a heterogeneous elongated probe element is placed in the at least one concave shaped functional element to be positioned or self-positioned to the bottom of the concave shaped functional element and fixed to the bottom; and finally the ready sensor is released from the auxiliary planar support structure. A method for producing a scanning probe microscopy sensor according to claim 11, wherein the at least one concave shaped element functionalized with a thickness less than the thickness of the free probe end is formed on the surface of the plate prior to the surface process structuring by photolithography followed by at least one etching process. Method for the production of a scanning probe microscope according to claims 11 and 12, characterized in that a single-crystal silicon wafer with a n-type doping and a resistance of from 1 to 20 Q.cm is used, which further comprises pre-built on it and galvanically coupled alloyed piezoresistive and highly conductive regions, to which, during surface structuring in the process of photolithography, the sections with selected geometrical dimensions of the microcontroller and the probe part are combined, and in the subsequent mask earlier etching of these doped areas are formed piezorezistori then perform processes for plating, in which, in contact with silnoprovodyashtite areas on the probe part, Micro-and the sensor body is obtained connecting the metal tracks with leads.