CN121250303A - A low-resistivity tungsten film, its preparation method, and a superatom beam assisted coating device - Google Patents
A low-resistivity tungsten film, its preparation method, and a superatom beam assisted coating deviceInfo
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- CN121250303A CN121250303A CN202511514069.0A CN202511514069A CN121250303A CN 121250303 A CN121250303 A CN 121250303A CN 202511514069 A CN202511514069 A CN 202511514069A CN 121250303 A CN121250303 A CN 121250303A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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Abstract
本发明提供了一种低电阻钨膜及其制备方法与超原子束辅助镀膜装置，所述的制备方法包括：提供基底；通过离子束溅射在基底表面形成β相钨沉积层；利用超原子束轰击所述β相钨沉积层进行局部热退火，得到α相钨膜层。本发明通过超原子束的轰击形成局部的脉冲高温，实现β相钨到低电阻率的α相钨，避免对膜层造成损伤，还提高了膜的致密性。
This invention provides a low-resistivity tungsten film, its preparation method, and a supra-atom beam assisted coating apparatus. The preparation method includes: providing a substrate; forming a β-phase tungsten deposition layer on the substrate surface by ion beam sputtering; and performing localized thermal annealing by bombarding the β-phase tungsten deposition layer with a supra-atom beam to obtain an α-phase tungsten film. This invention achieves the transformation from β-phase tungsten to low-resistivity α-phase tungsten through localized pulsed high-temperature bombardment with a supra-atom beam, avoiding damage to the film and improving its density.
Description
Technical Field
The invention belongs to the technical field of semiconductor material manufacturing, and relates to a low-resistance tungsten film, a preparation method thereof and a super-atomic beam auxiliary coating device.
Background
Currently, metal plating processes are commonly used for interconnect steps in semiconductor fabrication. As the dimensions of the metal lines or vias continue to shrink as the manufacturing process iterates, the dimensions of the metal begin to approach the mean free path of electrons in the metal. The traditional copper interconnection technology has the problem of overlarge resistance, and the increase of the resistance of the metal wire easily causes the increase of RC delay of the chip, influences the running speed of the chip and improves the power consumption.
Metals with lower bulk electron free ranges, such as tungsten, are beginning to be used in metal interconnect fabrication processes for such minute structures. However, the spontaneous crystal phase of the ultra-thin tungsten film is beta phase, which has much higher resistivity than alpha phase tungsten, and the transformation of beta phase to alpha phase is difficult, and high temperature treatment is generally required, which has negative effects on the chip.
Thus, low resistivity alpha phase tungsten films are produced within an acceptable temperature range and are very important for metal interconnect fabrication.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a low-resistance tungsten film, a preparation method thereof and a super-atomic beam auxiliary coating device, wherein local pulse high temperature is formed by radiation of super-atomic beams, so that beta-phase tungsten is converted into alpha-phase tungsten, and the resistivity of tungsten films is greatly reduced.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a low-resistance tungsten film, which comprises the steps of providing a substrate, forming a beta-phase tungsten deposition layer on the surface of the substrate through ion beam sputtering, and bombarding the beta-phase tungsten deposition layer by utilizing super-atomic beams to perform local thermal annealing to obtain an alpha-phase tungsten film layer.
According to the invention, in-situ treatment of the super-atomic beam is used for carrying out local thermal annealing in the film coating process, a high-temperature state is achieved on the surface of the nano-scale tungsten film, the transition from beta phase to alpha phase of the tungsten film is realized, the resistivity of the tungsten film is reduced, the problem of substrate damage caused by integral thermal annealing is avoided, and in addition, the in-situ local shallow surface layer thermal annealing effect of the super-atomic beam can enable each deposited film to have higher compactness, and the resistivity is further reduced.
In a preferred embodiment of the present invention, the α -phase tungsten film layer has a thickness of 5 to 300nm, for example, 5nm, 6nm, 10nm, 15nm, 20nm, 30nm, 35nm, 40nm, 45nm, 50nm, 100nm, 200nm or 300nm, but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned value range are applicable.
In one embodiment of the present invention, the specific resistance of the α -phase tungsten film layer is 7 to 20 μΩ·cm, and may be, for example, 7 μΩ·cm, 8 μΩ·cm, 9 μΩ·cm, 10 μΩ·cm, 11 μΩ·cm, 12 μΩ·cm, 15 μΩ·cm, 16 μΩ·cm, 18 μΩ·cm, or 20 μΩ·cm, but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned numerical ranges are similarly applicable.
In one embodiment of the present invention, the diameter of the substrate is 4 to 12 inches, for example, 4 inches, 5 inches, 6 inches, 7 inches, 8 inches, 9 inches, 10 inches, 11 inches, or 12 inches, but the present invention is not limited to the recited values, and other values not recited in the range of values are equally applicable.
In one embodiment of the invention, the substrate is rotated during the ion beam sputtering and local thermal annealing.
In one embodiment of the present invention, the rotation speed is 0.1 to 200rpm, and may be, for example, 0.1rpm, 1rpm, 5rpm, 10rpm, 20rpm, 50rpm, 60rpm, 90rpm, 100rpm, 120rpm, 130rpm, 150rpm, 160rpm, 180rpm or 200rpm, but not limited to the values listed, and other values not listed in the range of values are equally applicable.
In one embodiment of the present invention, the angle between the rotation normal of the substrate and the incident super-atomic beam is 0 to 90 °, for example, 0 °, 5 °, 10 °,20 °, 25 °, 30 °, 45 °, 50 °, 60 °, 65 °,70 °, 75 °, 80 ° or 87 °, but the present invention is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In one embodiment of the invention, the substrate is heated during the ion beam sputtering and local thermal annealing.
In one embodiment of the present invention, the heating temperature is room temperature to 500 ℃, for example, 25 ℃, 30 ℃, 37 ℃, 60 ℃, 90 ℃, 100 ℃, 120 ℃, 150 ℃,200 ℃, 240 ℃, 300 ℃, 350 ℃, 280 ℃, 400 ℃, 450 ℃ or 500 ℃, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In a preferred embodiment of the present invention, the ion beam sputtering process uses an ion beam having a flux of 10 to 800mA, for example 10mA、20mA、50mA、100mA、150mA、200mA、250mA、300mA、350mA、400mA、450mA、500mA、550mA、600mA、650mA、700mA、750mA、780mA mA or 800mA, but the present invention is not limited to the listed values, and other values not listed in the range are equally applicable.
In one embodiment of the present invention, the energy of the ion beam used is 200 to 2000eV, for example, 200eV, 300eV, 500eV, 600eV, 800eV, 1000eV, 1200eV, 1500eV, 1600eV, 1800eV, 1900eV or 2000eV, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In one embodiment of the present invention, the deposition rate of the β -phase tungsten deposition layer is 0.1 to 20nm/min, for example 0.1nm/min、1nm/min、2nm/min、4nm/min、5nm/min、6nm/min、8nm/min、10nm/min、12nm/min、15nm/min、16nm/min、18nm/min or 20nm/min, but the deposition rate is not limited to the recited values, and other values not recited in the range of values are equally applicable.
As a preferable technical scheme of the invention, the proportion of the super atoms in the super-atom beam is >90%.
In one embodiment of the invention, the number of elementary particles in a single super atom is greater than or equal to 50, the elementary particles being single atoms or molecules. For example, the number of elementary particles in a single super-atom may be 50, 100, 500, it being understood that the super-atom beam includes several super-atoms, the number of elementary particles in each super-atom not being completely uniform, but being greater than 50 elementary particles. Individual superatoms below the base particle can be removed by magnetic screening.
In one embodiment of the present invention, the flux of the super-atomic beam is 1 to 200 μa, for example, 1 μa, 5 μa, 10 μa, 15 μa, 20 μa, 30 μa, 40 μa, 45 μa, 50 μa, 60 μa, 65 μa, 70 μa, 80 μa, 85 μa, 90 μa, 100 μa, 150 μa or 200 μa, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In one embodiment of the present invention, the energy of the super-atomic beam is 1 to 60keV, for example, 1keV, 5keV, 10keV, 15keV, 20keV, 25keV, 30keV, 35keV, 40keV, 45keV, 50keV, 55keV, 58keV or 60keV, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In one embodiment of the present invention, the super-atomic beam includes any one atom or a mixed gas atom of at least two atoms of Ar, SF 6、NF3, or N 2.
In one embodiment of the invention, the super-atomic beam includes fluorine-based gas atoms.
In one embodiment of the present invention, the number of fluorine atoms in the fluorine-based gas atoms is 5% -60%, for example, 5%, 10%, 14%, 15%, 18%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55% or 60%, but the present invention is not limited to the recited values, and other non-recited values within the range of the recited values are equally applicable.
The invention utilizes the transverse sputtering effect of the super atomic beam to planarize the surface of the wafer, improves the compactness of the film, reduces the resistivity caused by surface electron scattering, and further improves the crystallization state of the alpha-phase tungsten film, thereby reducing the resistivity.
As a preferable technical scheme, the preparation method further comprises the step of carrying out surface modification treatment on the super-atomic beam radiation substrate before the ion beam sputtering.
In one embodiment of the present invention, the surface modification treatment time is 10 to 180s, for example, 10s, 20s, 30s, 50s, 60s, 90s, 100s, 120s, 150s or 180s, but the present invention is not limited to the recited values, and other non-recited values within the range are equally applicable.
In one embodiment of the present invention, the flux of the super-atomic beam used for the surface modification treatment is 1 to 100 μa, and may be, for example, 1 μa, 5 μa, 10 μa, 15 μa, 20 μa, 30 μa, 40 μa, 45 μa, 50 μa, 60 μa, 65 μa, 70 μa, 80 μa, 85 μa, 90 μa, 100 μa, 150 μa, or 200 μa, but is not limited to the values listed, and other values not listed in the range are equally applicable.
In one embodiment of the present invention, the super-atomic beam energy used in the surface modification treatment is 1 to 60keV, and may be, for example, 1keV, 5keV, 10keV, 15keV, 20keV, 25keV, 30keV, 35keV, 40keV, 45keV, 50keV, 55keV, 58keV or 60keV, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In one embodiment of the invention, the super-atomic beam includes fluorine-based gas atoms.
In one embodiment of the present invention, the number of fluorine atoms in the fluorine-based gas atoms is 5% -60%, for example, 5%, 10%, 14%, 15%, 18%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55% or 60%, but the present invention is not limited to the recited values, and other non-recited values within the range of the recited values are equally applicable.
The invention removes the damaged layer on the surface of the substrate by utilizing the mild treatment effect of the super atomic beam, so that the surface of the wafer generates suspension chemical bonds, the adhesive force of the subsequent coating is improved, and the conductivity of the metal interconnection is improved.
As a preferred embodiment of the present invention, the preparation method further comprises degassing the provided substrate.
In one embodiment of the invention, the degassing treatment mode comprises the steps of placing the substrate in a vacuum chamber, vacuumizing to a first pressure, then inflating the vacuum chamber to a second pressure, heating the substrate, then performing heat preservation treatment, and then recovering the pressure in the vacuum chamber to the first pressure.
According to the invention, the substrate is baked after the atmosphere is filled into the vacuum chamber, so that the moisture on the surface of the substrate can be removed, and the coating yield is effectively improved. In addition, the invention can empty the impurity gas released by the substrate wafer in the heating process by switching the pressure in the vacuum chamber, and improve the vacuum degree in the chamber, thereby ensuring the continuity of the air pressure among the chambers in the transferring process.
In a preferred embodiment of the present invention, the first pressure is 1×10 -6 to 0.1Pa, for example, 1×10-6Pa、5×10-6Pa、1×10-5Pa、5×10-5Pa、1×10-4Pa、5×10-4Pa、1×10-3Pa、5×10-3Pa、1×10-2、5×10-2 Pa or 0.1Pa, but the present invention is not limited to the values listed, and other values not listed in the range are equally applicable.
In one embodiment of the present invention, the second pressure is 50 to 5000Pa, for example, 50Pa, 100Pa, 200Pa, 500Pa, 1000Pa, 1500Pa, 2000Pa, 2500Pa, 3000Pa, 3500Pa, 4000Pa, 4500Pa or 5000Pa, but the present invention is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In one embodiment of the present invention, the substrate is heated to 60 to 400 ℃, for example, 60 ℃,70 ℃,80 ℃,90 ℃,100 ℃, 120 ℃, 150 ℃, 200 ℃, 250 ℃, 280 ℃, 300 ℃, 320 ℃, 350 ℃, 380 ℃ or 400 ℃, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In one embodiment of the present invention, the time of the heat-preserving treatment is 5 to 300s, for example, 5s, 10s, 20s, 50s, 100s, 120s, 150s, 180s, 200s, 240s, 250s, 260s, 270s, 280s, 290s or 300s, but the present invention is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
In a second aspect, the present invention provides a low-resistance tungsten film, which is manufactured by the manufacturing method of the low-resistance tungsten film in the first aspect.
The alpha phase in the tungsten film accounts for more than 90 percent.
The low-resistance tungsten film can be applied to interconnection of semiconductor chips, is beneficial to reducing power consumption and prolonging the service life of the semiconductor chips.
The invention provides a super-atomic beam auxiliary coating device which is used for the preparation method of the low-resistance tungsten film in the first aspect and comprises a cavity, a sputtering source, a super-atomic beam source and a super-atomic beam source, wherein a target material and a substrate are arranged in the cavity at intervals, the sputtering source is arranged on the cavity wall of the cavity and is used for emitting ion beams to the target material to form sputtering atoms, the sputtering atoms are deposited on the surface of the substrate to obtain a beta-phase tungsten deposition layer, and the super-atomic beam source is arranged on the cavity wall of the cavity and is used for emitting super-atomic beams to the substrate.
Compared with the prior art, the invention has the beneficial effects that:
According to the low-resistance tungsten film, the preparation method and the super-atomic beam auxiliary coating device provided by the invention, after coating, super-atomic beam in-situ treatment is carried out, local pulse high temperature is formed on the surface of the film under the low-temperature condition, so that the phase transformation of the tungsten film is realized, the material damage is avoided, the resistivity is greatly reduced, and the density of the film layer is improved.
Drawings
FIG. 1 is an X-ray diffraction pattern of the film obtained in example 1.
FIG. 2 is an X-ray diffraction pattern of the film obtained in example 8.
FIG. 3 is an X-ray diffraction phase analysis chart of the film produced in comparative example 1.
Detailed Description
It is to be understood that in the description of the present invention, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first", "a second", etc. may explicitly or implicitly include one or more such feature.
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings.
In one embodiment, the invention provides a method for preparing a low-resistance tungsten film, which comprises the following steps:
step one, providing a substrate.
The substrate used as a carrier of the coating layer has good mechanical strength, thermal stability and chemical stability, and can be selected according to the coating property and actual requirements, for example, the diameter of a wafer can be 4-12 inches, the surface is free from defects, the flatness is high, so that a uniform coating layer is deposited on the surface in the coating process, and the product quality is improved.
In some embodiments, the method of making further comprises degassing the provided substrate.
The method for degassing treatment comprises the steps of placing a substrate in a vacuum chamber, vacuumizing to a first pressure, then inflating the vacuum chamber to a second pressure, heating the substrate to 60-400 ℃, then performing heat preservation treatment for 5-300 seconds, and then recovering the pressure in the vacuum chamber to the first pressure. The first pressure is 1X 10 -6 -0.1 Pa, and the second pressure is 50-5000 Pa. The traditional pretreatment processes such as cleaning or photoetching are easy to introduce water vapor on the surface of the substrate or cause photoresist pollution, and cause adverse effects on the subsequent coating of the surface of the substrate, thereby causing the problem of electric connection virtual connection. The invention adopts a heating and baking mode under atmosphere, which can avoid the problems, is beneficial to improving the yield of products and reduces the energy consumption.
And secondly, forming a beta-phase tungsten deposition layer on the surface of the substrate through ion beam sputtering.
In the ion beam sputtering process, a target material is required to be provided, and an ion beam source is utilized to emit ion beams to bombard the target material, so that sputtering atoms are generated by the target material, the substrate is used as a receptor, and the sputtering atoms are deposited on the surface of the substrate to form a tungsten film layer. The sputtered atoms are tungsten. The flow rate of ion beam used for ion beam sputtering is 10-800 mA, the energy is 200-2000 eV, and the deposition rate of the film layer is 0.1-20 nm/min. The target may be a pure tungsten target or a tungsten alloy target commonly used by those skilled in the art. The pure tungsten target has high purity, low resistivity and strong adhesion of tungsten alloy target. And in the ion beam sputtering and local thermal annealing processes, the substrate is rotated and/or heated, wherein the rotation speed is 0.1-200 rpm, and the heating temperature is room temperature-500 ℃. The beta-phase tungsten deposition layer is of a metastable state structure, so that the resistivity of the beta-phase tungsten deposition layer is higher, the internal stress of the beta-phase tungsten deposition layer is larger, the film is easy to curl, crack or peel off from a substrate, and the product yield is reduced. If beta-phase tungsten is converted into alpha-phase tungsten, the quality of the film layer is greatly improved.
In the preparation process, the substrate can be fixed on a fixed chuck which is well known to a person skilled in the art, the fixed chuck has the functions of rotation, heating, tilting and the like, and in the preparation process of the tungsten film, the substrate can be driven to rotate and tilt and is heated.
And thirdly, bombarding the beta-phase tungsten deposition layer by using a super atomic beam to carry out local thermal annealing to obtain an alpha-phase tungsten film layer.
The super atom is a group of atoms formed by gathering tens, hundreds and thousands of basic particles, has the characteristics of high energy, high speed and large collision section, is generated by an ultrasonic nozzle known by a person skilled in the art, forms high-energy super atom beams after ionization, acceleration, magnetic screening, shaping and other processes, and irradiates on the surface of a substrate at a certain incident angle. The proportion of super atoms in the super atom beam is >90%. The number of basic particles in a single super atom is more than or equal to 50. The super-atom beam refers to the sum of super-atoms, and other atoms or ions that do not form super-atoms. The flux of the super atomic beam is 1-200 mu A, and the energy is 1-60 keV. the super atomic beam irradiates a beta-phase deposition layer on a substrate, and forms local pulse high temperature under the low temperature condition so as to convert beta-phase tungsten into alpha-phase tungsten. Compared with the traditional integral thermal annealing, the local thermal annealing of the super-atomic beam can avoid causing chip damage, and the thin film deposited on each layer has higher compactness due to the in-situ local shallow layer thermal annealing effect, so that the resistivity is further reduced. The alpha-phase tungsten is of a steady-state structure, has high purity and low resistivity, and is particularly 7-20 mu omega cm, and the alpha-phase tungsten also releases the internal stress of the film, so that a uniform film with strong adhesive force and compactness is easy to form. The super-atomic beam comprises any one atom or at least two mixed gas atoms of Ar, SF 6、NF3 or N 2, such as Ar super-atomic beam, SF 6 super-atomic beam, NF 3 super-atomic beam, N 2 super-atomic beam, ar super-atomic beam doped with SF 6, ar super-atomic beam doped with NF 3, N 2 super-atomic beam doped with NF 3 or, N 2 superatomic beam doped with SF 6. And in the super-atomic beam radiation process, the substrate is rotated and/or heated, wherein the rotation speed is 0.1-200 rpm, and the heating temperature is room temperature-500 ℃. The included angle between the rotation normal line of the substrate and the incident super-atomic beam is 0-90 degrees. The transverse sputtering effect of super atomic beams is utilized to planarize the metal surface, improve the compactness of the film, reduce the resistivity improvement caused by surface electron scattering, further improve the crystallization state of the tungsten film by utilizing the local thermal annealing effect, and optimize the resistivity. The super-atomic beam includes fluorine-based gas atoms. The fluorine-based gas atom is preferably Ar containing SF 6 or NF 3. In the treatment process, tungsten and fluorine-containing gas are subjected to reactive sputtering to form WF 4 gas reactant, and the thickness of a damaged layer can be effectively reduced by the intervention of the reactive gas, so that the size of crystal grains is increased, and the resistivity is reduced. The number of fluorine atoms in the fluorine-based gas atoms accounts for 5% -60%, and the speed of the reactive etching tungsten can be changed by adjusting the fluorine-containing proportion.
In some embodiments, the method further comprises performing a surface modification treatment with a super-atomic beam radiation substrate prior to the ion beam sputtering. The surface modification treatment time is 10-180 s. The flux of the super-atomic beam adopted in the surface modification treatment is 1-200 mu A, and the energy of the super-atomic beam is 1-60 keV. The damaged layer on the surface of the substrate is removed by utilizing the mild treatment effect of the super atomic beam, so that a suspension chemical bond is generated on the surface of the substrate, the adhesive force of the subsequent coating is improved, and the conductivity of the metal interconnection is also improved. In the surface modification treatment, the substrate is rotated and/or heated, wherein the rotation speed is 0.1-200 rpm, and the heating temperature is room temperature-500 ℃. The included angle between the rotation normal line of the substrate and the incident super-atomic beam is 0-90 degrees. The super atomic beam comprises fluorine-based gas atoms, and the number of fluorine atoms in the fluorine-based gas atoms is 5% -60%.
In another embodiment, the invention provides a low-resistance tungsten film, which is prepared by adopting the preparation method of the low-resistance tungsten film in one embodiment, and has the characteristics of low resistivity and high compactness. The low-resistance tungsten film is used for filling contact holes, through holes or grooves of the semiconductor chip, so that interconnection among multiple layers or different metal structures in the chip is realized, RC delay time of the semiconductor chip is effectively reduced, and power consumption is greatly reduced.
In another embodiment, the invention provides a super-atomic beam auxiliary coating device, which is used for the preparation method of the low-resistance tungsten film in one embodiment, and comprises the following steps:
the chamber is provided with a target material and a substrate at relatively intervals, and can be a vacuum chamber.
And the sputtering source is arranged on the wall of the cavity and is used for emitting ion beams to the target so as to form sputtering atoms on the surface of the target, and the substrate can receive the sputtering atoms so as to enable the sputtering atoms to be deposited on the surface of the substrate to obtain a beta-phase tungsten deposition layer.
And the super-atomic beam source is arranged on the cavity wall of the cavity and is used for emitting super-atomic beams to the substrate.
In addition, the super atomic beam auxiliary coating device also comprises an electric field scanning device, a supporting component of a target material and a substrate, a heating device, a neutralizer and the like which are necessary for realizing the coating function, the specific structure and the arrangement mode of the super atomic beam auxiliary coating device are not particularly limited, and the super atomic beam auxiliary coating device can be adjusted according to actual operation conditions by a person skilled in the art, and other devices required by coating are additionally arranged on the super atomic beam auxiliary coating device.
Example 1
The embodiment provides a preparation method of a low-resistance tungsten film, which specifically comprises the following steps:
S1, providing a base wafer with the diameter of 8 inches.
S2, fixing the substrate wafer on a wafer chuck for rotation and heating, and performing ion beam sputtering on a tungsten target material to form sputtered atoms so as to form a beta-phase tungsten deposition layer on the surface of the substrate wafer, wherein the flow of the adopted ion beam is 600mA, the energy is 1200eV, the deposition rate is 10nm/min, the rotation rate of the substrate wafer is 50rpm, and the heating temperature is 300 ℃.
S3, bombarding the beta-phase tungsten deposition layer by using a super-atom beam to perform local thermal annealing to obtain an alpha-phase tungsten film layer with the thickness of 70nm, wherein the ratio of super-atoms in the super-atom beam is more than 90%, the number of basic particles in single super-atoms is more than or equal to 50, the flow rate of the super-atom beam is 50 mu A, the energy is 35keV, the super-atom beam adopts mixed gas atoms of Ar and NF 3, and the included angle between the injected super-atom beam and the rotation normal line of a substrate wafer is 30 degrees.
Example 2
The embodiment provides a preparation method of a low-resistance tungsten film, which specifically comprises the following steps:
S1, providing a substrate wafer with a diameter of 6 inches.
S2, fixing the substrate wafer on a wafer chuck for rotation and heating, and performing ion beam sputtering on a tungsten target material to form sputtered atoms so as to form a beta-phase tungsten deposition layer on the surface of the substrate wafer, wherein the flow of the adopted ion beam is 200mA, the energy is 800eV, the deposition rate is 1nm/min, the rotation rate of the substrate wafer is 150rpm, and the heating temperature is 400 ℃.
S3, bombarding the beta-phase tungsten deposition layer by utilizing a super-atom beam to perform local thermal annealing to obtain an alpha-phase tungsten film layer with the thickness of 10nm, wherein the ratio of super-atoms in the super-atom beam is more than 90%, the number of basic particles in single super-atoms is more than or equal to 50, the flow rate of the super-atom beam is 20 mu A, the energy is 25keV, and the included angle between the injected super-atom beam and the rotation normal of a substrate wafer is 60 degrees.
Example 3
The embodiment provides a preparation method of a low-resistance tungsten film, which specifically comprises the following steps:
S1, providing a substrate wafer with a diameter of 12 inches.
S2, fixing the substrate wafer on a wafer chuck for rotation and heating, and performing ion beam sputtering on a tungsten target material to form sputtered atoms so as to form a beta-phase tungsten deposition layer on the surface of the substrate wafer, wherein the flow of the adopted ion beam is 800mA, the energy is 500eV, the deposition rate is 15nm/min, the rotation rate of the substrate wafer is 180rpm, and the heating temperature is 150 ℃.
S3, bombarding the beta-phase tungsten deposition layer by using a super-atom beam to perform local thermal annealing to obtain an alpha-phase tungsten film layer with the thickness of 25nm, wherein the ratio of super-atoms in the super-atom beam is more than 90%, the number of basic particles in single super-atoms is more than or equal to 50, the flow rate of the super-atom beam is 10 mu A, the energy is 15keV, the super-atom beam adopts mixed gas atoms of Ar and NF 3, and the included angle between the injected super-atom beam and the rotation normal line of a substrate wafer is 30 degrees.
Example 4
The embodiment provides a preparation method of a low-resistance tungsten film, which specifically comprises the following steps:
S1, providing a base wafer with a diameter of 4 inches.
S2, fixing the substrate wafer on a wafer chuck for rotation and heating, and performing ion beam sputtering on a tungsten target material to form sputtered atoms so as to form a beta-phase tungsten deposition layer on the surface of the substrate wafer, wherein the flow of the adopted ion beam is 100mA, the energy is 1600eV, the deposition rate is 10nm/min, the rotation rate of the substrate wafer is 50rpm, and the heating temperature is 500 ℃.
S3, bombarding the beta-phase tungsten deposition layer by using a super-atom beam to perform local thermal annealing to obtain an alpha-phase tungsten film layer with the thickness of 40nm, wherein the ratio of super-atoms in the super-atom beam is more than 90%, the number of basic particles in single super-atoms is more than or equal to 50, the flow rate of the super-atom beam is 65 mu A, the energy is 60keV, the super-atom beam adopts mixed gas atoms of Ar and NF 3, and the included angle between the injected super-atom beam and the rotation normal line of a substrate wafer is 87 degrees.
Example 5
The embodiment provides a preparation method of a low-resistance tungsten film, which specifically comprises the following steps:
S1, providing a base wafer with the diameter of 10 inches.
S2, fixing the substrate wafer on a wafer chuck for rotation and heating, and performing ion beam sputtering on a tungsten target material to form sputtered atoms so as to form a beta-phase tungsten deposition layer on the surface of the substrate wafer, wherein the flow of the adopted ion beam is 200mA, the energy is 2000eV, the deposition rate is 20nm/min, the rotation rate of the substrate wafer is 1rpm, and the heating temperature is 60 ℃.
S3, bombarding the beta-phase tungsten deposition layer by using a super-atom beam to perform local thermal annealing to obtain an alpha-phase tungsten film layer with the thickness of 30nm, wherein the ratio of super-atoms in the super-atom beam is more than 90%, the number of basic particles in a single super-atom beam is more than or equal to 50, the flow rate of the super-atom beam is 80 mu A, the energy is 15keV, the super-atom beam adopts mixed gas atoms of Ar and NF 3, and the included angle between the injected super-atom beam and the rotation normal line of a substrate wafer is 45 degrees.
Example 6
The embodiment provides a preparation method of a low-resistance tungsten film, which is different from embodiment 1 in that a super-atom beam radiation substrate is adopted for surface modification treatment before ion beam sputtering, the time is 120s, the proportion of super-atoms in the adopted super-atom beam is more than 90%, the number of basic particles in single super-atom is more than or equal to 50, the flow rate of the super-atom beam is 10 mu A, the energy is 45keV, the super-atom beam is a mixed gas atom of Ar and SF 4, the number proportion of fluorine atoms is 12%, and the rest steps and process parameters are the same as those of embodiment 1.
Example 7
The embodiment provides a preparation method of a low-resistance tungsten film, which is different from embodiment 1 in that a super-atom beam radiation substrate is adopted for surface modification treatment before ion beam sputtering, the time is 120s, the proportion of super-atoms in the adopted super-atom beam is more than 90%, the number of basic particles in single super-atom is more than or equal to 50, the flow rate of the super-atom beam is 60 mu A, the energy is 30keV, the super-atom beam is a mixed gas atom of Ar and SF 4, the number proportion of fluorine atoms is 20%, and the rest steps and process parameters are the same as those of embodiment 1.
Example 8
The present example provides a method for preparing a low-resistance tungsten film, which is different from example 6 in that the substrate wafer provided is placed in a vacuum chamber, and is evacuated to 0.01Pa, then the vacuum chamber is inflated to 500Pa, and the substrate is heated to 300 ℃ at the same time, and is subjected to a heat-preserving treatment for 30 seconds, and the remaining steps and process parameters are the same as those of example 6.
Comparative example 1
This comparative example provides a method for preparing a tungsten film, which is different from example 1 in that the super-atomic beam is not used for local thermal annealing, and the rest of the steps and process parameters are the same as those of example 1.
The surface resistivity of the alpha-phase tungsten film prepared in examples 1-8 was detected by a standard four-probe method, and the results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the films prepared by the super-atomic beam bombardment-assisted thermal annealing in examples 1 to 8 of the present invention all have lower resistivity. Compared with example 1, examples 6 to 7 have lower resistivity, which is mainly due to the fact that the pretreatment process of super atomic beam radiation is added before film deposition, the adhesion of the film is improved, the film quality is improved, and the resistivity is reduced. In the embodiment 8, the degassing treatment procedure of the wafer is added, so that the pollution to the film is avoided, and the film coating effect is improved. Comparative example 1 had a resistivity of 78.0. Mu. Ω. Cm.
The tungsten films obtained in example 1, example 8 and comparative example 1 were subjected to X-ray diffraction phase analysis, and the results are shown in fig. 1, 2 and 3.
It is not difficult to see that example 8 was subjected to degassing treatment and surface modification treatment before film deposition, respectively, which improved the deposition quality of the film and the uniformity of the crystal phase of the crystal grains, so that the peak value of alpha phase tungsten was significantly increased, almost all of it was the alpha phase, while the content of the alpha phase was very low in comparative example 1.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (10)
1. The preparation method of the low-resistance tungsten film is characterized by comprising the following steps of:
providing a substrate, forming a beta-phase tungsten deposition layer on the surface of the substrate by ion beam sputtering, and bombarding the beta-phase tungsten deposition layer by using a super-atomic beam to perform local thermal annealing to obtain an alpha-phase tungsten film layer.
2. The method for manufacturing a low-resistance tungsten film according to claim 1, wherein the thickness of the α -phase tungsten film layer is 5 to 300nm;
And/or the resistivity of the alpha-phase tungsten film layer is 7-20 mu omega cm;
And/or the diameter of the substrate is 4-12 inches;
And/or, rotating the substrate during the ion beam sputtering and local thermal annealing;
and/or the rotating speed is 0.1-200 rpm;
And/or the included angle between the rotation normal of the substrate and the injected super-atomic beam is 0-90 degrees;
And/or heating the substrate during the ion beam sputtering and local thermal annealing;
And/or the heating temperature is room temperature to 500 ℃.
3. The method of manufacturing a low-resistance tungsten film according to claim 1, wherein a flux of 10 to 800ma of ion beam is used in the ion beam sputtering process;
and/or the energy of the adopted ion beam is 200-2000 eV;
and/or the deposition rate of the beta-phase tungsten deposition layer is 0.1-20 nm/min.
4. The method of producing a low-resistance tungsten film according to claim 1, wherein the proportion of super atoms in the super-atom beam is >90%;
And/or, the single super atom is formed by gathering basic particles, the number of the basic particles is more than or equal to 50, and the basic particles are single atoms or molecules;
and/or the flow rate of the super-atomic beam is 1-200 mu A;
and/or the energy of the super-atomic beam is 1-60 keV;
and/or the super-atomic beam comprises any one atom or at least two mixed gas atoms of Ar, SF 6、NF3 or N 2.
5. The method of manufacturing a low-resistance tungsten film according to claim 1, further comprising performing a surface modification treatment with a super-atomic beam radiation substrate before the ion beam sputtering;
And/or the surface modification treatment time is 10-180 s;
and/or the flux of the super-atomic beam adopted by the surface modification treatment is 1-200 mu A;
And/or the energy of the super-atomic beam adopted by the surface modification treatment is 1-60 keV;
And/or, the super-atomic beam comprises fluorine-based gas atoms;
And/or the number of fluorine atoms in the fluorine-based gas atoms is 5% -60%.
6. The method of manufacturing a low-resistance tungsten film according to claim 1, further comprising degassing the provided substrate;
And/or the degassing treatment mode comprises the steps of placing the substrate in a vacuum chamber, vacuumizing to a first pressure, then inflating the vacuum chamber to a second pressure, heating the substrate, then performing heat preservation treatment, and then recovering the pressure in the vacuum chamber to the first pressure.
7. The method of manufacturing a low-resistance tungsten film according to claim 6, wherein the first pressure is 1 x 10 -6 to 0.1Pa;
And/or the second pressure is 50-5000 Pa;
and/or heating the substrate to 60-400 ℃;
And/or the heat preservation treatment time is 5-300 s.
8. A low-resistance tungsten film, wherein the low-resistance tungsten film is produced by the method for producing a low-resistance tungsten film according to any one of claims 1 to 7.
9. The low resistance tungsten film according to claim 8, wherein the α -phase in the tungsten film is greater than 90%.
10. The super-atomic beam auxiliary coating device is used for the preparation method of the low-resistance tungsten film according to any one of claims 1 to 7, and comprises the following components:
The chamber is provided with a target and a substrate at relatively intervals;
the sputtering source is arranged on the wall of the cavity and is used for emitting ion beams to the target material to form sputtering atoms and enabling the sputtering atoms to be deposited on the surface of the substrate to obtain a beta-phase tungsten deposition layer;
And the super-atomic beam source is arranged on the cavity wall of the cavity and is used for emitting super-atomic beams to the substrate.
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| CN202510965016.4A CN120776252A (en) | 2025-07-14 | 2025-07-14 | Coating method and coating system |
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| CN202511512438.2A Pending CN121250301A (en) | 2025-07-14 | 2025-10-22 | A low resistivity thin film, its preparation method, and a superatom beam assisted coating device |
| CN202511512440.XA Pending CN121250302A (en) | 2025-07-14 | 2025-10-22 | A method for coating in high aspect ratio holes and a superatom beam assisted coating device |
| CN202511514069.0A Pending CN121250303A (en) | 2025-07-14 | 2025-10-22 | A low-resistivity tungsten film, its preparation method, and a superatom beam assisted coating device |
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| CN202511512438.2A Pending CN121250301A (en) | 2025-07-14 | 2025-10-22 | A low resistivity thin film, its preparation method, and a superatom beam assisted coating device |
| CN202511512440.XA Pending CN121250302A (en) | 2025-07-14 | 2025-10-22 | A method for coating in high aspect ratio holes and a superatom beam assisted coating device |
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