DE102008008829A1 - Method for registration of real structure-information in solid crystal bodies by X-ray radiation, involves representing crystallographic real structure of solid crystal body by hard X-ray braking radiation on detector holding surface - Google Patents

Abstract

The method involves representing a crystallographic real structure of a solid crystal bodies (5, 51, 52) by a hard X-ray braking radiation on a detector holding surface (71). The crystal bodies have minimum thickness (D) depending on an atomic number and has a device (1), which has a micro-focus X-ray tube (2), crystal body holder (9) and a detector (7) with the detector holding surface . Independent claims are also included for the following: (1) a device for registration of real structure-information in solid crystal bodies by a X-ray radiation (2) an application of hard X-ray braking radiation in the energy area of 50 to 450 kilo-electron volts for simultaneous image superposition of information of solid crystal bodies.

Description

The The invention relates to a method and a device for registration of real structure information in massive crystal bodies by means of X-radiation, wherein the crystal bodies have a dependent of the atomic number minimum thickness, wherein the device at least from a microfocus X-ray tube, a crystal body holder and a detector with a Detector receiving surface in a natural atmosphere exists, with a radiation of the in the crystal body holder located crystal body to produce a radiographic Shadow image on the detector for registration of macroscopic Real structure of the crystal body performed becomes.

In The industry is working on the macroscopic and / or crystallographic defect structure of massive crystal bodies, as single crystals or as coarsely crystalline, out of a few crystallites existing body, especially in the form of components are trained to analyze with as little effort as possible, to ensure the quality of manufactured bodies bring about.

Under The macroscopic defect structure generally becomes voids and cracks, but also intentionally introduced cavities or additional body understood while the crystallographic Defect structure a statement about deviations of the real structure from the ideal structure of a crystal body.

in the The first case will be classical X-ray radiographic imaging in the form of an X-ray inspection with film, image plate (engl. image plate) or solid-state detector or computed tomography used. For the crystallographic analysis of the crystal bodies come z. As the single-crystal diffractometry, the Laue method, the Weissenberg process, the rotary crystal process and others Method of use. In the semiconductor industry comes if necessary even the long topography added.

The conventional Laue method is an X-ray diffraction method which uses polychromatic X-radiation in the form of Bremsstrahlung. In the diffraction on the single crystal body become point-like Reflexes that receive so-called Laue spots. Location and shape of the Spots are here indicators of the crystallographic Real Structure Review.

The Problems of the Laue method can be best described using the example of Show examination of single-crystal turbine blades. The same applies to the investigation of the quality of similar ones Components or grown crystal bodies.

The Investigations of components such. B. turbine blades are carried out in such a complex manner, that for example by means of X-radiation in the direction of return and with a surface detector, the component for registering the Laue interference first on the front and then on the back or at the same time "worn down." Positional and geometric changes of the Laue points must be constantly evaluated.

The Real structure information statement is not convincing because the layers of the defects are not the corresponding places in the bodies can be assigned and because of the low information depth the Laue interference does not capture the entire crystal volume can be. Due to the two-sided images, a high material and time required.

The High energy synchrotron diffraction methods and neutron diffraction techniques also very expensive.

Like a high-energy fine-focused electron beam is shot on a copper-monocrystal sphere in a high vacuum and the intensity of the X-radiation is detected on a film in radiation, is already in the document Determann, H .: About the directional distribution of the X-ray braking radiation of a massive anticode, Ann. Physics 30, 1937, p. 481 described. It shows lines and bands that are comparable to the Kikuchi images of the electron beam interferences, as they are also in the document Determann, H .: Kikuchi ribbons with X-rays, writings of the natural science. Company, Danzig, 1938 , are described.

In a similar direction, the results, which in the document Wolf, H.-Ch .: Hard X-ray Braking Radiation Source Interference, Ann. the Physics 6th Series, Volume 13, 1953, pp. 381-403 in which it is achieved with an imaging device grid source interference with hard X-ray braking radiation and this also an electron beam is used in a high vacuum.

The Problems of both solutions are that through the Use of electron beams in high vacuum with the described Devices no massive crystal bodies are tested in air can.

A preparation of interference diagrams with Bremsstrahlung in the range of low energies between 50 eV to 8 keV is in the document Brummer, O .: The production of "Kikuchi lines and bands" with relatively soft X-rays and the influence of crystal disturbances on these X-ray interferences, Z. Naturforschg. 13a, 1958, pp. 571-572 , described. It does not mention an X-ray micrograph and is not visible on the corresponding images.

• a) Es ist eine Strahlungsquelle mit genügend kleinem Brennfleck vorgesehen.
• b) Es ist ausdrücklich eine charakteristische Röntgenstrahlung bei einer Energie von 5 keV bis 20 keV für die gleichzeitige Belichtung der Weitwinkelinterferenzen einzusetzen.
• c) Die Dicke D der Kristalle muss der zur Anwendung kommenden charakteristischen Röntgenstrahlung so angepasst sein, dass sich Interferenzen genügend stark vom Untergrund abheben.
• d) Die Öffnung des Röntgenstrahlenkegels ist groß genug auszubilden, damit auch die Weitwinkelinterferenzen auftreten und registriert werden können.

A combination of the generation of wide-angle interference with a radiographic image is in the document Brummer, O .: On the simultaneous generation of X-ray interference and the X-ray shadow image of crystals, Z. Naturforschung. 15a, 1960, pp. 875-879 , described. The prerequisites for generating the X-ray interference shadow (RIS) diagrams are the following factors:

• a) It is provided a radiation source with a sufficiently small focal spot.
• b) It is expressly a characteristic X-ray radiation at an energy of 5 keV to 20 keV for the simultaneous exposure of the wide-angle interference use.
• c) The thickness D of the crystals must be adapted to the characteristic X-ray radiation used in such a way that interferences stand out sufficiently strongly from the ground.
• d) The opening of the X-ray cone is large enough to form, so that the wide-angle interference occur and can be registered.

In this is used to generate X-ray interference at the same time and the X-ray silhouette of crystals explicitly working only with characteristic radiation, which causes problems which consist in that the sample thickness D due to the absorption as thin as possible (D ≤ 50 μm to 300 μm) must be chosen so that the interference is still take off against the ground and be registered can. It is also necessary to use the anode material to choose accordingly.

One Another problem is that thicker components and in particular massive bodies must therefore be thinned whereby the process is no longer carried out nondestructive can be.

by virtue of the fact stated in the technical articles is simultaneous Image accumulation for thick and massive crystal bodies in the subsequent period has not been followed by the professional world.

A device for the production of wide-angle Rückstrahlaufnahmen with characteristic X-ray radiation is in the document DD 242 688 A1 The apparatus for investigating small crystal body regions serves to characterize crystallites in terms of orientation, lattice constants, real structure and anisotropic stresses. In this case, in the beam path of an electron beam, a cup which is open toward the electron beam source and is closed with respect to the crystal body with a metal foil is arranged.

A similar device for making wide-angle X-ray reflections is in the document DE 101 18 573 C1 described.

in the In the case of synchrotron beam diffraction methods it is expedient the crystal body time consuming layer by layer scan, which is similar to a tomography. An application of multi-beam interference is also eliminated because it is the investigation of partially strongly disturbed real crystals is.

Neutron interference shots In radiation have the problem that they are not so highly spatially resolved are about to make a real structure statement in staggered form to hit the entire thickness of the crystal.

A method and apparatus for examining the crystallographic quality of objects having a crystal structure by excitation of Kikuchi pseudo-lines in the surrounding sphere are disclosed in the document DE 690 03 270 T2 described. The method relates to the production of an image of Kikuchi pseudo-lines of a monocrystalline structure with a photon beam. The device has an X-ray generator with a maximum of 0.1 mm microfocus and a structural unit which has in succession a luminous force amplifier, a video recorder or an image receiver and a movable support for the objects to be tested, wherein the support is arranged between the microfocus and the luminous intensity amplifier ,

One Problem is that an image of Kikuchi pseudo lines from diffracted electrons, regardless of the exciting type of photon. There will be an X-ray tube for generating X-ray photoelectrons used in the object that interfere and the Kikuchi pseudo lines produce. The crystal body to be tested must apparently be rotated several times in other angular positions to a "new Image "A Performance of the Process - Generation of electrons in the object - is in the direction of radiation only on very thin objects or exclusively on surfaces possible.

It is a method for radiographic inspection of an object with a crystal lattice in the document US Pat. No. 6,295,335 B1 described. It includes steps for diffracting the object with electromagnetic radiation to obtain a radiographic image of the object on a display device up. The display device contains, according to an exposure, the radiographic image that is a composite image. This image results from a relative displacement of the object. The displacement makes it possible to reproduce the object at a significant attenuation of the parasitic elements, which result from diffraction of the electromagnetic radiation at the crystal lattice of the object. An intensity-enhancing collimator and a postfilter element are used.

One Problem is that the procedure exclusively the improvement of radiography is used. The by fluorescence excitation generated secondary radiation in the crystalline object becomes in the sense of radiographic imaging as disturbing - as "parasitic element "- denotes, and the method shows a possibility the damping.

Another method for detecting absorption, refraction and scattering patterns of an object by independently analyzing, registering, digitizing and combining the images is in the document WO 98/16817 A1 The images reach an upper and a lower angular position of a "rocking curve" of a crystal analyzer An x-ray beam generated by a conventional device may be passed to either a Bragg-type crystal analyzer or a Laue-type crystal analyzer Absorbance, refraction, and scattering effects are detected on an optical disk and then digitized, and the digitized images are simultaneously resolved, preferably on a pixel-by-pixel basis, to obtain a combined visible image, which analyzes a "rocking curve." The device contains the crystal analyzer for this purpose.

One The problem is that the method for detecting refractive and spreading patterns, the method of improving exclusively a radiographic image is used by known scattering effects how small angle and Compton scattering are kept low and so a radiographic contrast enhancement occurs. An illustration The crystallographic real structure does not take place because there is no diffraction effect is used.

• 1. Bereitstellen eines Strahlbündels einer harten Strahlung,
• 2. Einbringen eines asymmetrischen Einkristall-Monochromators in den Strahlengang, wobei das daran reflektierte Strahlbündel ein flächenförmiges Strahlbündel einer im Wesentlichen parallel gerichteten, aber leicht divergierenden Strahlung ist, die einen spezifischen Divergenzwinkel besitzt,
• 3. Durchstrahlen des Objektes mit dem flächenförmigen Strahlbündel, so dass die Strahlung durch das Objekt hindurchgeht,
• 4. Einbringen eines Kristall-Analysators in den Strahlengang strahlabwärts des Objektes an eine Position, in der die Braggsche Reflexion des flächenförmigen Strahlbündels wirksam ist, das auf den Kristall-Analysator auftrifft, um das Strahlbündel zu beugen und ein gebeugtes Strahlbündel und ein durchgelassenes Strahlbündel zu bilden, wobei die Anordnung so ist, dass der Winkelbereich der Reflexion von den wirksamen Kristallflächen des Analysators um den exakten Braggschen Reflexionswinkel herum zumindest zweimal so groß ist wie der Divergenzwinkel des flächenförmigen Strahlbündels, das durch den Einkristall-Monochromator gebildet wird, und
• 5. Registrieren des gebeugten Strahlbündels oder sowohl des durchgelassenen als auch des gebeugten Strahlbündels an einem punktsensitiven Strahldetektor.

Another method for obtaining an image of an internal structure of an object is in the document DE 692 28 285 T2 described, wherein the method comprises the following steps:

• 1. providing a beam of hard radiation,
• 2. introducing an asymmetric monocrystal monochromator into the beam path, the beam reflected therefrom being a sheet-like beam of substantially parallel, but slightly divergent, radiation having a specific divergence angle,
• 3. irradiating the object with the sheet-like beam, so that the radiation passes through the object,
• 4. placing a crystal analyzer in the beam path downstream of the object to a position in which the Bragg reflection of the sheet-like beam is incident on the crystal analyzer to diffract the beam and add a diffracted beam and a transmitted beam the arrangement being such that the angular range of the reflection from the effective crystal faces of the analyzer about the exact Bragg reflection angle is at least twice the divergence angle of the sheet-shaped ray formed by the single crystal monochromator, and
• 5. Register the diffracted beam or both the transmitted and the diffracted beam at a point-sensitive beam detector.

One The problem is that the source is an X-ray source is used with continuous radiation, however, to be Generation of diffraction interferences asymmetric single crystal monochromators used both before and after the object that diffracts required discrete wavelengths by rotation steer to the object and parallelize the x-ray beam. Farther is a radiographic through the use of monochromators Picture of the object to be examined impossible.

Furthermore, an X-ray topography system is in the document US 2003/0108152 A1 described, wherein the system includes an X-ray tube, which generates X-rays, which on a limited area of an object, for. B. a silicon wafer act. A detector is arranged to capture the beam after transmission through the object or after reflection on the object. The detector has an array of pixels adapted to the beam surface to produce a digital image on said restricted area. A relative incremental shift between the x-ray tube and the object produces a series of digital images that are combined together. In optional embodiments, x-ray optics are incorporated to create a parallel beam to avoid image duplication, or the effect of image duplication is eliminated by software.

One problem is that the X-ray beam is not shot perpendicularly but at an angle of less than 90 ° to the object. Furthermore, the jet after emerging from the Röh parallelized by the subsequent X-ray optics. The parallel beam is trapped by a beam stopper after passing through the object and deflected and directed at a certain angle to the detector. Furthermore, it is necessary in the method and apparatus to perform relative movements between the object and the source to obtain the desired result images. This is an X-ray topography method.

A method for non-destructive analysis and an associated analyzer is in the document US 2004/0196957 A1 which are capable of obtaining a high-contrast image within an object easily and in a manner by shifting when an object is irradiated with homogeneous, collimated X-rays.

One Problem is that the device with parallel rays is working. The object is a crystal for the parallelization of the radiation upstream. The x-ray beam does not strike upright the object. The radiation is transmitted through the object sent through an analysis crystal before it influenced that Radiation hits the detector.

The Problems of the above methods are that none with a single procedure the macroscopic and crystallographic Real structure by obtaining volume information in compact form Crystal bodies and components simultaneously and without any Movement of the device components using hard bremsstrahlung allowed to map.

Of the The invention is therefore based on the object, a method and a device for registering real structure information in massive crystal bodies by means of X-radiation indicate that are designed so that the real structure of massive crystal bodies non-destructive, displayed simultaneously, quickly and largely visually and an immediate assessment of the real structure for X-ray microscopic and crystallographic characterization can be made. It should be especially inside the massive crystal body the crystallographic defects as well as the location and extent of the the production of resulting defect cavities, bound Foreign particles as well as intended voids and crystal body changes can be detected reproducibly and evaluated after loading.

• – mittels Einsetzens einer unmittelbar hinter dem Strahlaustritt der Mikrofokus-Röntgenröhre angeordneten Blende, deren Blendenloch einen zur Einstellung einer Strahldivergenz ausgebildeten Durchmesser hat,
• – durch eine Einstellung eines Abstandes R₂ zwischen dem Kristallkörper und der Detektoraufnahmefläche, wobei der Abstand R₂ mindestens das Zwanzigfache der Entfernung des Kristallkörpers vom Strahlaustritt der Mikrofokus-Röntgenröhre beträgt,
• – durch eine Einstellung der Belichtungszeit t der Mikrofokus-Röntgenröhre, wobei die eingestellte Belichtungszeit t von der Ordnungszahl des Materials des Kristallkörpers, von der Dicke D des Kristallkörpers und von der Empfindlichkeit des Detektors abhängt, und
• – durch eine Einstellung der Beschleunigungsspannung U der Mikrofokus-Röntgenröhre, die eine Intensität des Primärröntgenstrahls erzeugt, bei der die Intensität des Maximums des Primärröntgenstrahls durch die Absorption des Kristallkörpers um mindestens 25% verringert ist, wobei eine Einstellung des Verhältnisses zwischen der die radiographische Schattenabbildung erzeugenden Reststrahlintensität und der Interferenzstrahlintensität durchgeführt und somit ein registrierfähiges Kontrastbild zeitgleich zwischen den Interferenzlinien und der radiographischen Schattenabbildung herbeigeführt wird.

The object is solved by the features of claims 1, 10 and 20. The method for registering real-structure information in X-ray massive crystal bodies, wherein the crystal bodies have a minimum thickness D dependent on atomic number, is provided with a device comprising at least a microfocus X-ray tube, a crystal body holder, and a detector having a detector receiving surface realizes a natural atmosphere, wherein a radiation of the crystal body located in the crystal body holder for generating a radiographic shadow image on the detector for registration of the macroscopic real structure of the crystal body is performed,
wherein according to the characterizing part of patent claim 1
linear brake-beam interferences that can be registered on the detector mounting surface to represent a crystallographic real structure of the massive crystal body by hard X-ray braking radiation in a wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , from which the massive crystal body filters out the wavelength λ required exactly for diffraction at its network planes, The line-shaped brake beam interferences simultaneously superimpose the radiographic shadow image generated by a remaining residual beam intensity, whereby an intensity enhancement of the line-shaped brake beam interferences is brought about by means of the following steps:

• By inserting a diaphragm arranged immediately behind the beam exit of the microfocus X-ray tube, the aperture hole of which has a diameter designed to set a beam divergence,
• By adjusting a distance R ₂ between the crystal body and the detector receiving surface, wherein the distance R _{2 is} at least twenty times the distance of the crystal body from the beam exit of the microfocus X-ray tube,
• By adjusting the exposure time t of the microfocus X-ray tube, the set exposure time t depending on the atomic number of the material of the crystal body, the thickness D of the crystal body and the sensitivity of the detector, and
• By adjusting the acceleration voltage U of the microfocus X-ray tube, which produces an intensity of the primary X-ray beam in which the intensity of the maximum of the primary X-ray beam is reduced by at least 25% by the absorption of the crystal body, wherein an adjustment of the ratio between the radiographic shadow image generating Residual beam intensity and the interference beam intensity performed and thus a registerable contrast image is brought about at the same time between the interference lines and the radiographic shadow image.

The Irradiation is done with hard X-ray braking radiation in one Energy range of 50 keV to 450 keV performed.

to simultaneous image overlay of the shadow image and the Bremsstrahlinterferenzlinien to a registerable Contrast image is for the microfocus X-ray tube set an exposure time t in the minute range.

Optional can predetermined crystal regions of the crystal body by means of an xy manipulator unit on the crystal body retaining crystal body holder are scanned.

An increase in the image overlay on the surface of the detector can be carried out to adjust the distance R ₂ by a distance adjusting device with which the detector or the detector receiving surface is adjusted relative to the microfocus X-ray tube.

When massive crystal bodies can be monocrystalline or coarsely crystalline crystal bodies.

The solid crystal bodies may have a minimum thickness D in the range of a few millimeters to a few centimeters, wherein the introduced into the device and the minimum thickness D having crystal body of the hard X-ray braking radiation of the range of Δλ ≈ 1.0 to 1.3 λ _min exactly Beu Filter out the appropriate wavelength for generating the linear brake jet interference itself.

at Radiation of coarsely crystalline, consisting of single crystals Crystal bodies serves the aperture in combination with a Crystal body movement by means of the xy manipulator unit the probing and imaging of single crystals.

parts the diffraction cone for linear brake jet interference, the outside of the superimposed with interference lines Silhouette exist, exclusively contain those Information of the crystallographic real structure as opposed to the diffraction cones in the contrast image, the radiographic shadow image and the crystallographic real structure, both Diffraction cone types simultaneously on the detector receiving surface be registered.

• – eine Mikrofokus-Röntgenröhre, die einen direkten Primärröntgenstrahl mit harter Röntgenbremsstrahlung in einem Energiebereich von 50 keV bis 450 keV liefert,
• – eine Kristallkörper-Halterung zur Halterung des zu untersuchenden Kristallkörpers,
• – einen Detektor mit einer Detektoraufnahmefläche, die in einem Abstand R₁ vom Strahlaustritt der Mikrofokus-Röntgenröhre aus entfernt angeordnet ist, wobei der Kristallkörper zur Erzeugung einer radiographischen Schattenabbildung auf dem Detektor zur Registrierung der makroskopischen Realstruktur des Kristallkörpers durchstrahlt wird,

zur Realisierung des vorgenannten Verfahrens,
wobei im Kennzeichenteil des Patentanspruchs 10
zur Erzeugung von registrierfähigen linienförmigen Bremsstrahlinterferenzen auf der Detektoraufnahmefläche unmittelbar hinter dem Strahlaustritt der Mikrofo kus-Röntgenröhre und dem gehalterten Kristallkörper ein Intensitätsverstärker in Form einer Blende zur Reduktion seitlicher Streustrahlung sowie zur Strahldivergenzeinstellung eingebracht ist, wobei die Blende mit einem Lochdurchmesser im Millimeterbereich versehen ist,
dass ein Abstand R₂ zwischen dem Kristallkörper und der Detektoraufnahmefläche vorgesehen ist, der zumindest das Zwanzigfache der Entfernung des Kristallkörpers vom Strahlaustritt der Mikrofokus-Röntgenröhre beträgt, und
dass eine Beschleunigungsspannung U der Mikrofokus-Röntgenröhre vorgesehen ist, die eine Strahlintensität nach dem Kristallkörper erzeugt, bei der die Intensität des Maximums des Primärröntgenstrahls durch die Absorption des Kristallkörpers um mindestens 25% bezüglich des zugehörigen Intensitätsmaximums verringert ist, wobei ein Verhältnis zwischen der die radiographische Schattenabbildung erzeugenden Reststrahlintensität und der Interferenzstrahlintensität eingestellt ist, mit dem ein auf der Detektoraufnahmefläche registrierfähiges Kontrastbild zwischen Interferenzlinien und radiographischer Schattenabbildung anzeigbar ist.An apparatus for registering real structure information in massive crystal bodies with X-radiation, wherein the crystal bodies have a minimum thickness D dependent on the atomic number, in a natural atmosphere

• A microfocus X-ray tube providing a direct primary x-ray beam with hard X-ray braking radiation in an energy range from 50 keV to 450 keV,
• A crystal body holder for holding the crystal body to be examined,
• A detector having a detector-receiving surface, which is arranged at a distance R ₁ from the beam exit of the microfocus X-ray tube, wherein the crystal body is irradiated for generating a radiographic shadow image on the detector for registration of the macroscopic real structure of the crystal body,

for the realization of the aforementioned method,
wherein in the characterizing part of claim 10
for generating registrable line-shaped Bremsstrahlinterferenzen on the detector receiving surface immediately behind the beam exit of the Mikrokus X-ray tube and the content Erten crystal body an intensity enhancer in the form of a diaphragm for reducing lateral stray radiation and the Strahldivergenzeinstellung is introduced, the aperture is provided with a hole diameter in the millimeter range,
that a distance R _{2 is provided} between the crystal body and the detector receiving surface, which is at least twenty times the distance of the crystal body from the beam exit of the microfocus X-ray tube, and
in that an acceleration voltage U of the microfocus X-ray tube is provided which produces a beam intensity after the crystal body in which the intensity of the maximum of the primary X-ray beam is reduced by the absorption of the crystal body by at least 25% with respect to the associated intensity maximum, wherein a ratio between the radiographic Shadow image generating residual beam intensity and the interference beam intensity is set, with which a recordable on the detector receiving surface contrast image between interference lines and radiographic shadow image can be displayed.

The Aperture is made of a highly absorbent material.

The Aperture can be a lead aperture.

Furthermore is a lead sheet on the back of the detector for shielding arranged.

A connected to the microfocus X-ray tube Control device is available, which is used to set the exposure time t for performing the simultaneous image overlay to the registerable contrast image and setting the acceleration voltage U of the microfocus X-ray tube is provided.

The crystal body holder for the crystal body is optionally equipped with an xy manipulator unit to include all predetermined areas of Kris tallkörpers in the registry hen and / or single crystallites in the investigation of coarsely crystalline crystal bodies to probe.

Of the Detector can be an X-ray film, a solid state detector, an image plate or a screen / CCD camera unit.

To avoid an over-radiation of the image centers at the shortest distance R ₁ to the microfocus X-ray tube and at the same time the impact of the primary X-ray residual intensity can optionally be introduced into the beam path of the primary X-ray beam between the crystal body holder and the detector, an absorption filter.

The Absorption filter can be a geometrically formed body, preferably a hemisphere or a spherical segment.

A the filter associated with the absorption filter can from a material which only slightly absorbs the X-ray radiation used, preferably carbon fiber reinforced plastic, so that the image overlay the shot to the registerable contrast image is not disturbed.

The use of hard X-ray braking radiation in the energy range of 50 keV to 450 keV for the simultaneous image superposition of information of solid crystal bodies having a number dependent on the atomic number D, takes place in a natural atmosphere according to the aforementioned method and the aforementioned device according to the characterizing part of Claim 20,
by means of a direct radiation to generate a radiographic shadow image for registration of the macroscopic real structure of the massive crystal body and
by means of a generation of a shadow image registerable contrast having Bremsstrahlinterferenzlinien for registration of the crystal lographic real structure of the massive crystal body on a detector and for visual or scanning related evaluation.

The non-destructive method is explained in more detail below:
During the direct transmission, an enlarged radiographic shadow image (for example a defect structure) and the registration of a diffraction information (crystallographic parameters) z. B. a few millimeters to a few centimeters thick and large-area crystal body simultaneously imaged in a shot and performed with exposure times t in the minute range by means of microfocus X-ray tube.

Accordingly, the X-ray beam of the microfocus X-ray tube is used, which is directed through a directly arranged at the beam exit lead aperture on the immediately following, monocrystalline or coarse crystalline, valid as a test sample crystal body. The microfocus X-ray tube uses its hard bremsstrahlung. At a distance R ₁ , whose magnitude may be from a few millimeters to several 100 millimeters, away from the beam exit of the microfocus X-ray tube, there is a detector, for. As an X-ray film, which is shielded at its rear with a lead sheet. Instead of the X-ray film, alternatively, a corresponding solid state detector or an image plate can be used. The crystal body holder can optionally be supplemented by an xy manipulator unit to remove all areas of interest of the crystal body, which may be desirable for larger test samples.

The Procedure starts with the switching on of the mentioned Radiation source, z. B. the microfocus X-ray tube, in the lower minute range. The associated and accurate Exposure times t depend on the beam energy, the Atomic number of the crystal material, the crystal body thickness and the detector sensitivity.

On the said way become simultaneously adjustable on the detector enlarged X-ray shadow micrograph as well as line-shaped Bremsstrahlinterferenzen the irradiated Crystal body area in the form of the registerable Contrast image accumulated.

The method is based on the use of hard X-ray brake radiation just above the wavelength λ _min , for example in the wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , and does not use the longer wavelength characteristic radiation of an X-ray tube. The massive crystal body "filters" and monochromatizes to a certain extent even the wavelength required for diffraction at its lattice planes from the continuous brake spectrum Δλ.

The Invention allows a non-destructive working Combination method, which in direct transmission and simultaneously an enlarged radiographic shadow image to determine the macroscopic defect structure and the registration a diffraction information by means of linear brake jet interference to determine crystallographic parameters thicker, in particular some Millimeters to a few centimeters thicker and larger, massive crystal body at the same time in a receptacle uses.

Because no electron beam with vacuum conditions is needed, the invention makes it possible to study in air and thus also in larger ones and massive crystal body performing components.

Around all areas of interest or areas of the crystal body or abzufahren the component, the crystal body optionally "scanned" with the xy manipulator unit.

One further advantage over the frequently used Laue method (surface analysis up to approx. 300 μm Depth) is that the location of the defects in the invention Method over the entire crystal body thickness D can be traced.

Around the procedural exuberance of the picture centers in shortest distance to the X-ray source and at the same time at the point of impact of the primary X-ray residual intensity To avoid, optionally, a gradient absorption filter, for. B. a hemisphere or a spherical segment, in the X-ray beam additionally introduced. Order the representation not in addition to bother, that can be needed filter-holder device from a used X-radiation only low absorbing material (eg. B. carbon fiber reinforced plastic) exist.

The inventive method provides in the transmission direction Real structure information about the total crystal body thickness and over a larger crystal area.

The inventive method is subject to in the industrial testing practice serious limitations, that the crystal body thickness D due to the absorption as possible thin (D ≤ 50 μm to 300 μm) must not be chosen, as it is in contrast takes the opposite route, based on the use of hard X-ray braking radiation based and thick, massive crystal bodies in the form of samples or Components in their total crystal body thickness D one non-destructive investigation.

Essential is the use of hard X-ray brake radiation in Energy range from 50 keV to 450 keV for direct transmission massive crystal body for simultaneous image overlay a radiographic shadow image for registration of the macroscopic defect structure of the crystal body and a generation of linear Bremsstrahlinterferenzen for registration of the crystallographic Defect structure of the crystal body on a detector for visual or scanning related evaluation.

The Invention allows that in the prior art mentioned restrictions on the to be irradiated Thickness of the crystal bodies are bypassed as the process in the range of high energies between 50 keV to approx. 450 keV and thus works in the area of hard X-ray braking radiation. As a result, also thick and massive components can be examined radiographically become.

The Invention is based on an embodiment by means of explained in more detail several drawings.

she demonstrate:

1 Representations of the device for registration of real structure information in massive crystal bodies by means of hard X-ray braking radiation on an X-ray film, wherein

1a a schematic representation of the device and

1b are an intensity (I) X-ray wavelength (λ) curve with the X-ray brake radiation range used according to the invention,

2 an evaluable and recordable contrast image recording according to the invention on an X-ray film of a massive NiAl crystal body with the two image areas - radiographic shadow image and brake beam interference lines - of the registerable contrast image,

3 a schematic representation of real structure information on an X-ray film of a massive TbNi ₂ B ₂ C crystal body with macroscopic pores (voids) and without crystal defects,

4 a schematic representation of real structure information on an X-ray film of a massive TbNi ₂ B ₂ C crystal body with local defects in a lattice plane -. B. a Kleinwinkelkorngrenze - and without macroscopic pores,

5 a real recording of the real structure information on a massive TbNi ₂ B ₂ C crystal body by means of hard X-ray braking radiation after the transmission, wherein

5a a picture of the crystal body with voids and interference lines and

5b an enlarged section of the picture in 5a represent the same crystal body,

6 a schematic representation of real structure information on a single-crystal turbine blade of CMSX-6 without macroscopic pores (voids) and without crystal defects,

7 a schematic representation of real structure information on a single crystal turbine blade of CMSX-6 without macroscopic pores (voids) and with disturbances in the crystal structure - with increased dislocation density - and

8th a real-time acquisition of real-structure information by means of hard X-ray brake radiation on a single-crystal turbine blade made of CMSX-6 without macroscopic pores (voids) and with crystal defects - with increased dislocation density.

• – eine Mikrofokus-Röntgenröhre 2, die einen direkten Primärröntgenstrahl 31 mit harter Röntgenbremsstrahlung 20 in einem Energiebereich von 50 keV bis 450 keV liefert,
• – eine Kristallkörper-Halterung 9 zur Halterung des zu untersuchenden Kristallkörpers 5, 51, 52,
• – einen Detektor 7 mit einer Detektoraufnahmefläche 71, die in einem Abstand R₁ vom Strahlaustritt 21 der Mikrofokus-Röntgenröhre 2 aus entfernt angeordnet ist, wobei der Kristallkörper 5, 51, 52 zur Erzeugung einer radiographischen Schattenabbildung auf dem Detektor 7 zur Registrierung der makroskopischen Realstruktur 13, 13' des Kristallkörpers 5, wie in 3 gezeigt ist, durchstrahlt wird.

The following are the 1 with the 1a . 1b considered together. In 1 . 1a is a device 1 for registration of real structure information in massive crystal bodies 5 . 51 . 52 represented, which have a minimum thickness D dependent on the atomic number, shown in a natural atmosphere, wherein the device 1 includes

• - A microfocus X-ray tube 2 that have a direct primary x-ray 31 with hard X-ray braking radiation 20 in an energy range from 50 keV to 450 keV,
• - a crystal body holder 9 for holding the crystal body to be examined 5 . 51 . 52 .
• - a detector 7 with a detector receiving surface 71 which emerges from the jet at a distance R ₁ 21 the microfocus X-ray tube 2 is located away from, wherein the crystal body 5 . 51 . 52 to generate a radiographic shadow image on the detector 7 to register the macroscopic real structure 13 . 13 ' of the crystal body 5 , as in 3 is shown, is irradiated.

According to the invention for the production of registerable line-shaped, in the 2 to 8th shown, brake jet interference 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' on the detector receiving surface 71 immediately behind the jet exit 21 the microfocus X-ray tube 2 and the salient crystal body 5 . 51 . 52 an intensity amplifier in the form of a diaphragm 4 for reducing lateral scattered radiation and for setting a beam divergence 6 introduced, with the aperture 4 provided with a hole diameter in the millimeter range,
wherein a distance R ₂ between the crystal body 5 . 51 . 52 and the detector receiving surface 71 is provided and at least twenty times the distance of the crystal body 5 . 51 . 52 from the beam exit 21 the microfocus X-ray tube 2 is, and
wherein an acceleration voltage U of the microfocus X-ray tube 2 is provided, which has a beam intensity after the crystal body 5 . 51 . 52 generated at which the intensity of the maximum of the primary x-ray beam 31 by the absorption of the crystal body 5 . 51 . 52 is reduced by at least 25% with respect to the associated intensity maximum, wherein a ratio between the residual beam intensity generating the radiographic shadow image 3 and the interference beam intensity is set with the one on the detector receiving surface 71 registrable in 2 shown contrast image 30 between interference lines 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' and radiographic shadow illustration 13 . 13 ' can be displayed.

The on the detector receiving surface 71 registrable linear brake jet interference 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' to illustrate the crystallographic real structure of the massive crystal body caused by hard X-ray brake radiation 20 in an in 1b shown wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , from which the massive crystal body 5 . 51 . 52 filters out the wavelength λ required exactly for diffraction at its network planes.

In 2 is a recordable contrast image 30 on a detector receiving surface 71 for a NiAl crystal body. In the middle area 22 The image overlay is both the radiographic shadow image and the crystallographic real structure in the form of the line-shaped Bremsstrahlinterferenzen as a registerable contrast image 30 illustrated, wherein on the detector receiving surface 71 at the edge 23 Parts of the diffraction cone 6 '' in continuation of the superimposed Bremsstrahlinterferenzen the contrast image 30 are registered, which contain only the crystallographic real structure.

In the 1 shown aperture 4 consists of a highly absorbent material and represents a lead aperture.

A lead sheet 8th can on the back 10 of the detector 7 be arranged for shielding.

It's one to the microfocus X-ray tube 2 connected control device 17 provided for adjusting the exposure time t for performing the simultaneous image superimposition and for adjusting the acceleration voltage U of the microfocus X-ray tube 2 is provided.

A crystal body holder 9 is for the massive crystal body 5 . 51 . 52 provided, which optionally with an xy manipulator unit 11 is equipped to all predetermined areas of the crystal body 5 . 51 . 52 to include in the registry and / or to probe single crystallites in the study of coarsely crystalline crystal bodies.

The detector 7 . 71 may be an X-ray film, a solid-state detector, an optical disk or a fluorescent screen / CCD camera unit.

To avoid over-radiation of the image centers at the shortest distance R ₁ to the microfocus X-ray tube 2 and at the same time at the point of impact of the primary X-ray residual intensity optionally an absorption filter (not shown) in the beam path of the primary X-ray beam 31 between the crystal body holder 9 and the detector 7 . 71 be introduced.

The Absorption filter can be a geometrically formed body, preferably a hemisphere or a spherical segment.

A the filter associated with the absorption filter can from a material which only slightly absorbs the X-ray radiation used, preferably carbon fiber reinforced plastic, so that the accumulation of recording for the recordable Contrast image is not disturbed.

The method for registration of real structure information in massive crystal bodies with an X-ray 31 , where the crystal bodies 5 . 51 . 52 have a dependent of the atomic number minimum thickness D, with the aforementioned device 1 at least from a microfocus X-ray tube 2 , a crystal body holder 9 and a detector 7 with a detector receiving surface 71 exists, is realized in a natural atmosphere,
wherein a radiation of the in the crystal body holder 9 located crystal body 5 . 51 . 52 to generate a radiographic shadow image on the detector 7 . 71 to register the macroscopic real structure 13 . 13 ' of the crystal body 5 . 51 . 52 is carried out.

• – mittels Einsetzens einer unmittelbar hinter dem Strahlaustritt 21 der Mikrofokus-Röntgenröhre 2 angeordneten Blende 4, deren Blendenloch 12 einen zur Einstellung einer Strahldivergenz 6 ausgebildeten Durchmesser hat,
• – durch eine Einstellung eines Abstandes R₂ zwischen dem Kristallkörper 5, 51, 52 und der Detektoraufnahmefläche 71, wobei der Abstand R₂ mindes tens das Zwanzigfache der Entfernung des Kristallkörpers 5, 51, 52 vom Strahlaustritt 21 der Mikrofokus-Röntgenröhre 2 beträgt,
• – durch eine Einstellung der Belichtungszeit t der Mikrofokus-Röntgenröhre 2, wobei die eingestellte Belichtungszeit t von der Ordnungszahl des Materials des Kristallkörpers 5, 51, 52, von der Dicke D des Kristallkörpers 5, 51, 52 und von der Empfindlichkeit des Detektors 7, 71 abhängt, und
• – durch eine Einstellung der Beschleunigungsspannung U der Mikrofokus-Röntgenröhre 2, die eine Intensität des Primärröntgenstrahls 31 erzeugt, bei der die Intensität des Maximums des Primärröntgenstrahls 31 durch die Absorption des Kristallkörpers 5, 51, 52 um mindestens 25% verringert ist, wobei eine Einstellung des Verhältnisses zwischen der die radiographische Schattenabbildung erzeugenden Reststrahlintensität 3 und der Interferenzstrahlintensität durchgeführt und somit ein registrierfähiges Kontrastbild 30 zeitgleich zwischen den Interferenzlinien und der radiographischen Schattenabbildung herbeigeführt wird.

According to the invention on the detector receiving surface 71 registrable line-shaped brake jet interference 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' to show a crystallographic real structure of the massive crystal body 5 . 51 . 52 by hard X-ray braking radiation 31 in a wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , from which the massive crystal body 5 . 51 . 52 which filters out exactly to the diffraction required at its network levels wavelength λ generates, with the line-shaped Bremsstrahlinterferenzen 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' by a remaining residual beam intensity 3 simultaneously superimposed radiographic shadow image, wherein an intensity enhancement of the line-shaped Bremsstrahlinterferenzen 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' by means of the following steps:

• - By inserting a directly behind the jet outlet 21 the microfocus X-ray tube 2 arranged aperture 4 , whose aperture hole 12 one for setting a beam divergence 6 has trained diameter,
• By adjusting a distance R ₂ between the crystal body 5 . 51 . 52 and the detector receiving surface 71 , wherein the distance R _{2 at} least twenty times the distance of the crystal body 5 . 51 . 52 from the beam exit 21 the microfocus X-ray tube 2 is,
• By adjusting the exposure time t of the microfocus X-ray tube 2 , wherein the set exposure time t of the atomic number of the material of the crystal body 5 . 51 . 52 , of the thickness D of the crystal body 5 . 51 . 52 and the sensitivity of the detector 7 . 71 depends, and
• - By adjusting the acceleration voltage U of the microfocus X-ray tube 2 giving an intensity of the primary x-ray 31 generated at which the intensity of the maximum of the primary x-ray beam 31 by the absorption of the crystal body 5 . 51 . 52 is reduced by at least 25%, with an adjustment of the ratio between the residual beam intensity producing the radiographic shadow image 3 and the interference beam intensity and thus a registerable contrast image 30 at the same time between the interference lines and the radiographic shadow image is brought about.

The Irradiation with hard X-ray braking radiation is in one Energy range of 50 keV to 450 keV performed.

For simultaneously mapping the shadow image and the brake beam interference lines to the registerable contrast image 30 is for the microfocus X-ray tube 2 set an exposure time t in the minute range.

Optionally, predetermined crystal regions of the crystal body 5 . 51 . 52 by means of an xy manipulator unit 11 at the crystal body 5 . 51 . 52 retaining crystal body holder 9 be scanned.

An enlargement of the image overlay on the surface 71 of the detector 7 can be performed by a distance adjustment (not shown) for adjusting the distance R ₂ , with which the detector 7 . 71 relative to the microfocus X-ray tube 2 is set.

As a massive crystal body 5 . 51 . 52 Monocrystalline or coarsely crystalline crystal bodies can be used, the crystal bodies 5 . 51 . 52 have a minimum thickness D in the range of a few millimeters to a few centimeters.

In a radiation of coarsely crystalline, consisting of single crystals crystal bodies 5 . 51 . 52 serves the aperture 4 in combination with a crystal body movement by means of the manipulator unit 11 the probing and mapping of single kris metals.

The parts of the diffraction cone 6 '' that are outside the diffraction cone 6 ' of the contrast image 30 at the edge 23 the contrast picture 30 contain only the information of the crystallographic real structure, in contrast to the diffraction cones 6 ' in contrast 30 containing the radiographic shadowing and the crystallographic real structure, both diffraction cone types 6 ' . 6 '' simultaneously on the detector receiving surface 71 can be registered.

The use of hard X-ray braking radiation 20 in the energy range from 50 keV to 450 keV
for the simultaneous imaging overlay of information of massive crystal bodies 5 . 51 . 52 having a minimum thickness D dependent on atomic number, in a natural atmosphere according to the method and the apparatus,
by direct irradiation to generate a radiographic shadow image for registration of the macroscopic real structure 13 . 13 ' of the massive crystal body 5 . 51 . 52 and
by means of a generation of shading contrasting, registerable contrast having Bremsstrahlinterferenzlinien for registration of the crystallographic real structure 16 . 14 '' . 15 '' of the massive crystal body 5 . 51 . 52 on a detector 7 and for visual or scanning related evaluation.

The method begins with the turning on of said X-ray source, a microfocus X-ray tube 2 , in the lower minute range.

One to the microfocus X-ray tube 2 connected control device 17 is for setting the exposure time t for performing the simultaneous image superposition.

In the manner described are on the detector 7 . 71 simultaneously an enlarged X-ray shadow microscopy image as well as by diffraction cone 6 ' . 6 '' in the 1a marked X-ray brake beam interference of the irradiated crystal body region of the solid crystal body 5 . 51 . 52 can be registered.

To carry out the method according to the invention is from the microfocus X-ray tube 2 delivered hard X-ray brake radiation 20 used as in the in 1 . 1b illustrated X-ray spectrum 18 contained and in contrast to the characteristic radiation used in the prior art 19 is shown.

The 3 shows a schematic representation of real structure information on an X-ray film 71 from a massive TbNi ₂ B ₂ C crystal body 51 with macroscopic pores (voids) 13 . 13 ' and without crystal defects.

In this case, inside the TbNi ₂ B ₂ C crystal body 51 microscopic cavities 13 . 13 ' or voids are shown as a form of the macroscopic defect structure. The lines of brake radiation interference 14 . 15 on the other hand, as a form of the crystallographic real or defect structure, recorded simultaneously in transillumination, become sharp and uninterrupted next to and through the microscopic voids 13 . 13 ' represented through. This means that the inner surfaces of the cavities 13 . 13 ' are occupied by atoms that attach to the bulk material without crystal defects in the form of the crystallographic defect structure. In this case, it would have to turn on the inside of the TbNi ₂ B ₂ C crystal body 51 To close existing defects, a comparison of pycnometric density measurements with X-ray over a precision lattice constant determination specific density no physically correct result. The device according to the invention 1 does not have these limitations and provides all relevant data, most of which are already visually visible.

The 4 shows a schematic representation of real structure information on the X-ray film 71 from a massive TbNi ₂ B ₂ C crystal body 51 with local crystal defects and without macroscopic pores. The sharp interference lines 14 . 15 but have an interference line break 16 on, the local defects in a lunar system - z. B. a Kleinwinkelkorngrenze - in massive TbNi ₂ B ₂ C crystal body 51 , indicates.

The 5 shows real images of the real structure information according to the inventive method after irradiation by means of hard X-ray braking radiation on the massive TbNi ₂ B ₂ C crystal body 51 , in which 5a a picture of the TbNi ₂ B ₂ C crystal body 51 with voids 13 and interference lines 14 . 15 (strengthened) and 5b an enlarged section of the picture in 4a same TbNi ₂ B ₂ C crystal body 51 with the enlarged blower 13 and the interference 14 . 14 and 14 ' . 15 ' (both highlighted). The crystal body thickness D of the TbNi ₂ B ₂ C crystal body 51 is for example 5 mm and the diameter of the pictures in 5a and 5b imaged crystal body area is 9 mm.

The 6 shows a schematic representation of real structure information on a single crystal turbine blade 52 from CMSX-6 without macroscopic pores (voids) and without crystal disturbances The lack of crystal disturbances leads to sharp interference lines 14 . 15 leads.

The 7 shows a schematic representation of real structure information on the same single-turbine turbine blade 52 from CMSX-6 without macroscopic pores (voids) and with disturbances in the crystal structure - with increased dislocation density -, which in the admission as blurred interference lines 14 '' . 15 '' (Band interferences) are shown.

The 8th shows a real recording of real structure information according to the inventive method after irradiation by means of hard X-ray braking radiation 20 on the single-crystal turbine blade 52 from CMSX-6 without macroscopic pores (voids), but with crystal disruption - with increased dislocation density - due to the blurred interference lines 14 '' . 15 '' are displayed as already in 7 is shown schematically.

The method is used for nondestructive characterization of the quality of massive crystal bodies 5 . 51 . 52 , which are associated with metals, semiconductors, intermetallic compounds, organic crystals and ionic crystals.

The method is based on the use of hard X-ray brake radiation just above the wavelength λ _min , for example in the wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , and does not use the longer wavelength characteristic radiation of an X-ray tube. The massive crystal body 5 . 51 . 52 "Filters" and monochromatizes to a certain extent even the wavelength λ required for diffraction at its network planes from the continuous brake spectrum Δλ.

Especially massive silicon single crystal blocks (engl. ingots) as starting material for microelectronic wafers and solar technology, piezocrystals, single crystal turbine blades and alloy crystal bodies can be the real structure information by registering simultaneous image accumulation detected and immediately either visually or by a high-resolution Scanning be evaluated. But not only on defect structures but also in extension to an intended inner Formation of the crystal bodies can be massive Crystal bodies targeted dimensioned and from the melt drawn cavities and / or during the melt given bodies on their training, their Location as well as their defects within the crystal body checked become.

1

contraption

2

Microfocus X-ray tube

3

residual radiation

30

registered enabled contrast image

31

Primary X-ray

32

linear Brake beam interference outside of the contrast image

4

Lead pinhole

5

crystal body

51

TbNi ₂ B ₂ C crystal body

52

turbine blade

6

Beam divergence cone

6 '

diffraction cone of the superimposed contrast image

6 ''

diffraction cone outside the superimposed contrast image

7

detector

71

Detector receiving surface

8th

lead sheet

9

Crystal body holder

10

back

11

manipulator unit

12

aperture hole

13

cavity

13 '

cavity

14

sharp interference line

14 '

sharp interference line

14 ''

blurry interference line

15

sharp interference line

15 '

sharp interference line

15 ''

blurry interference line

16

Interference line break

17

control device

18

X-ray spectrum

19

characteristic radiation

20

hardness Bremsstrahlung

21

beam exit

22

middle Area of recording

23

border area the recording

D

Crystal body thickness

R ₁

distance between the beam exit and the detector

R ₂

distance between crystal body and detector

U

acceleration voltage

t

exposure time

x, y

shift coordinates

λ

wavelength

Δλ

Wavelength range

QUOTES INCLUDE IN THE DESCRIPTION

This list The documents listed by the applicant have been automated generated and is solely for better information recorded by the reader. The list is not part of the German Patent or utility model application. The DPMA takes over no liability for any errors or omissions.

Cited patent literature

• - DD 242688 A1 [0018]
• - DE 10118573 C1 [0019]
• - DE 69003270 T2 [0022]
• - US 6295335 B1 [0024]
• WO 98/16817 A1 [0026]
• - DE 69228285 T2 [0028]
• US 2003/0108152 A1 [0030]
• US 2004/0196957 A1 [0032]

Cited non-patent literature

• - Determann, H .: About the directional distribution of the X-ray braking radiation of a massive Antikatode, Ann. Physics 30, 1937, p. 481 [0010]
• - Determann, H .: Kikuchi bands with X-rays, writings of the natural sciences. Company, Danzig, 1938 [0010]
• - Wolf, H.-Ch .: Lattice-source interference of hard X-ray Bremsstrahlung, Ann. Physics 6th Series, Vol. 13, 1953, pp. 381-403 [0011]
• - Brummer, O .: The production of "Kikuchi lines and bands" with relatively soft X-rays and the influence of crystal disturbances on these X-ray interferences, Z. Naturforschg. 13a, 1958, pp. 571-572 [0013]
• - Brummer, O .: On the simultaneous generation of X-ray interference and the X-ray shadow image of crystals, Z. Naturforschung. 15a, 1960, p. 875-879 [0014]

Claims (20)

Method for registering real-structure information in massive crystal bodies by means of X-radiation ( 31 ), whereby the crystal bodies ( 5 . 51 . 52 ) have a minimum thickness (D) dependent on the atomic number, with at least one microfocus X-ray tube ( 2 ), a crystal body holder ( 9 ) and a detector ( 7 ) with a detector receiving surface ( 71 ) existing device ( 1 ) in a natural atmosphere, wherein a radiation of the in the crystal body holder ( 9 ) located crystal body ( 5 . 51 . 52 ) for generating a radiographic shadow image on the detector ( 7 . 71 ) for the registration of the macroscopic real structure ( 13 . 13 ' ) of the crystal body ( 5 ), characterized in that on the detector receiving surface ( 71 ) registrable line-shaped brake beam interference ( 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' ) to illustrate a crystallographic real structure of the massive crystal body ( 5 . 51 . 52 ) by hard X-ray braking radiation ( 31 . 20 ) in a wavelength range of Δλ ≈ 1.0 to 1.3 λ _min , from which the massive crystal body ( 5 . 51 . 52 ) which filters out exactly the wavelength (λ) required for the diffraction at its network planes, whereby the line-shaped brake beam interferences ( 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' ) by a remaining residual beam intensity ( 3 ) superimposed radiographic shadow image simultaneously, wherein an intensity gain of the line-shaped Bremsstrahlinterferenzen ( 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' ) is brought about by means of the following steps: - by inserting one immediately behind the jet outlet ( 21 ) of the microfocus X-ray tube ( 2 ) arranged aperture ( 4 ), whose aperture hole ( 12 ) one for setting a beam divergence ( 6 ) has formed diameter, - by adjusting a distance (R ₂ ) between the crystal body ( 5 . 51 . 52 ) and the detector receiving surface ( 71 ), wherein the distance (R ₂ ) at least twenty times the distance of the crystal body ( 5 . 51 . 52 ) from the jet outlet ( 21 ) of the microfocus X-ray tube ( 2 ) by adjusting an exposure time (t) of the microfocus X-ray tube ( 2 ), wherein the set exposure time (t) of the atomic number of the material of the crystal body ( 5 . 51 . 52 ), of the thickness (D) of the crystal body ( 5 . 51 . 52 ) and the sensitivity of the detector ( 7 . 71 ), and - by adjusting the acceleration voltage (U) of the microfocus X-ray tube ( 2 ) containing an intensity of the primary x-ray beam ( 31 ), at which the intensity of the maximum of the primary x-ray beam ( 31 ) by the absorption of the crystal body ( 5 . 51 . 52 ) is reduced by at least 25%, wherein an adjustment of the ratio between the residual beam intensity generating the radiographic shadow image ( 3 ) and the interference beam intensity and thus a registerable contrast image ( 30 ) is caused at the same time between the interference lines and the radiographic shadow image. Method according to claim 1, characterized in that the irradiation of the crystal bodies ( 5 . 51 . 52 ) with hard X-ray braking radiation ( 31 . 20 ) is performed in an energy range of 50 keV to 450 keV. A method according to claim 1, characterized in that for the simultaneous image superposition of the shadow image and the Bremsstrahlinterferenzlinien to registerable contact image ( 30 ) for a microfocus X-ray tube ( 2 ) an exposure time (t) in the minute range is set. A method according to claim 1 to 3, characterized in that optionally predetermined crystal regions of the crystal body ( 5 . 51 . 52 ) by means of an xy manipulator unit ( 11 ) at the crystal body ( 5 . 51 . 52 ) holding crystal body holder ( 9 ) are scanned. Method according to Claims 1 to 4, characterized in that an enlargement of the image overlay on the surface ( 71 ) of the detector ( 7 ) is performed by a distance adjusting device for adjusting the distance (R ₂ ) with which the detector ( 7 . 71 ) relative to the microfocus X-ray tube ( 2 ) is set. Process according to claims 1 to 5, characterized in that as massive crystal bodies ( 5 . 51 . 52 ) monocrystalline or coarsely crystalline crystal bodies are used. Process according to claim 6, characterized in that the crystal bodies ( 5 . 51 . 52 ) have a minimum thickness (D) in the range of a few millimeters to a few centimeters. A method according to claim 6 or 7, characterized in that when irradiated by coarsely crystalline, consisting of single crystals crystal bodies ( 5 . 51 . 52 ) the aperture ( 4 ) in combination with a crystal body movement by means of the xy manipulator unit ( 11 ) of probing and imaging of single crystals. A method according to claim 1, characterized in that parts of the diffraction cone ( 6 '' ) for linear brake jet interference ( 32 ) outside the contrast image ( 30 ) at the edge ( 23 ) of the recording, the diffraction cones ( 6 '' ) contain exclusively the information of the crystallographic real structure, in contrast to the diffraction cones ( 6 ' ) in the contrast image ( 30 ) containing the radiographic shadow image and the kristallo graphic real structure in the registerable contrast image ( 30 ), both diffraction cone types ( 6 ' . 6 '' ) simultaneously on the detector receiving surface ( 71 ). Contraption ( 1 ) for registration of real structure information in massive crystal bodies by means of X-radiation ( 31 ), whereby the crystal bodies ( 5 . 51 . 52 ) have a minimum thickness (D) dependent on the atomic number, in a natural atmosphere, comprising - a microfocus X-ray tube ( 2 ) providing a direct primary x-ray ( 31 ) with hard X-ray braking radiation ( 20 ) in an energy range from 50 keV to 450 keV, - a crystal body holder ( 9 ) for holding the crystal body to be examined ( 5 . 51 . 52 ), - a detector ( 7 ) with a detector receiving surface ( 71 ), which at a distance (R ₁ ) from the beam exit ( 21 ) of the microfocus X-ray tube ( 2 ) is removed from, wherein the crystal body ( 5 . 51 . 52 ) for generating a radiographic shadow image on the detector ( 7 ) for the registration of the macroscopic real structure ( 13 . 13 ' ) of the crystal body ( 5 ) is irradiated, for the realization of the method according to claim 1 to 9, characterized in that for the generation of registerable line-shaped Bremsstrahlinterferenzen ( 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' ) on the detector receiving surface ( 71 ) immediately behind the jet exit ( 21 ) of the microfocus X-ray tube ( 2 ) and the salient crystal body ( 5 . 51 . 52 ) an intensity amplifier in the form of a diaphragm ( 4 ) for the reduction of lateral scattered radiation and for setting a beam divergence ( 6 ), wherein the diaphragm ( 4 ) is provided with a hole diameter in the millimeter range, that a distance (R ₂ ) between the crystal body ( 5 . 51 . 52 ) and the detector receiving surface ( 71 ), which is at least twenty times the distance of the crystal body ( 5 . 51 . 52 ) from the jet outlet ( 21 ) of the microfocus X-ray tube ( 2 ), and that an acceleration voltage (U) of the microfocus X-ray tube ( 2 ), which has a beam intensity after the crystal body ( 5 . 51 . 52 ), at which the intensity of the maximum of the primary x-ray beam ( 31 ) by the absorption of the crystal body ( 5 . 51 . 52 ) is reduced by at least 25% with respect to the associated intensity maximum, wherein a ratio between the residual beam intensity generating the radiographic shadow image ( 3 ) and the interference beam intensity is adjusted, with the one on the detector receiving surface ( 71 ) recordable contrast image ( 30 ) between interference lines ( 14 . 15 . 14 ' . 15 ' . 14 '' . 15 '' ) and radiographic shadow image ( 13 . 13 ' ) can be displayed. Device according to claim 10, characterized in that the diaphragm ( 4 ) consists of a highly absorbent material. Device according to claim 11, characterized in that the diaphragm ( 4 ) is a lead aperture. Apparatus according to claim 10, characterized in that a lead sheet ( 8th ) on the back side ( 10 ) of the detector ( 7 ) is arranged for shielding. Apparatus according to claim 10, characterized in that a to the microfocus X-ray tube ( 2 ) connected control device ( 17 ) for adjusting the exposure time (t) for performing the simultaneous image overlay to the registerable contrast image (16). 30 ) and for adjusting the acceleration voltage (U) of the microfocus X-ray tube ( 2 ) is provided. Apparatus according to claim 10, characterized in that the crystal body holder ( 9 ) for the crystal body ( 5 . 51 . 52 ) optionally with an xy manipulator unit ( 11 ) to all predetermined areas of the crystal body ( 5 . 51 . 52 ) and / or to probe single crystallites in the investigation of coarsely crystalline crystal bodies. Apparatus according to claim 10, characterized in that the detector ( 7 . 71 ) is an X-ray film, a solid-state detector, an optical disk, or a screen / CCD camera unit. Apparatus according to claim 10 to 16, characterized in that to avoid an over-radiation of the image centers at the shortest distance (R ₁ ) to the microfocus X-ray tube ( 2 ) and at the same time at the point of impact of the primary X-ray residual intensity ( 3 ) an absorption filter in the beam path of the primary x-ray beam ( 31 ) between the crystal body holder ( 9 ) and the detector ( 7 . 71 ) is introduced. Device according to claim 17, characterized in that the absorption filter is a geometrically formed body, preferably a hemisphere or a spherical segment. Device according to claim 17 or 18, characterized in that a filter holder device associated with the absorption filter consists of a material which only slightly absorbs the used X-ray radiation, preferably carbon fiber-reinforced plastic, so that the image superposition during the recording of the registerable contrast image ( 30 ) is not disturbed. Use of hard X-ray braking radiation ( 20 ) in the energy range of 50 keV to 450 keV for the simultaneous image superposition of information of massive crystal bodies ( 5 . 51 . 52 ) having a minimum thickness (D) dependent on atomic number, in a natural atmosphere according to the method of claims 1 to 9 and the device according to claims 10 to 19, by direct irradiation of the crystal body ( 5 . 51 . 52 ) for generating a radiographic shadow image for registration of the macroscopic real structure ( 13 . 13 ' ) of the crystal body ( 5 . 51 . 52 ) and by means of a generation of contrasting radiographic shadow lines for radiographic shadow imaging for registering the crystallographic real structure ( 16 . 14 '' . 15 '' ) of the crystal body ( 5 . 51 . 52 ) on a detector ( 7 . 71 ) and for visual or scanning related evaluation.