CN114250444A - Method for plasma-assisted chemical vapor deposition of high-purity tungsten sputtering target material - Google Patents
Method for plasma-assisted chemical vapor deposition of high-purity tungsten sputtering target material Download PDFInfo
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- CN114250444A CN114250444A CN202111449598.9A CN202111449598A CN114250444A CN 114250444 A CN114250444 A CN 114250444A CN 202111449598 A CN202111449598 A CN 202111449598A CN 114250444 A CN114250444 A CN 114250444A
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
- C23C16/08—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metal halides
- C23C16/14—Deposition of only one other metal element
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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
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
Abstract
The invention provides a method for plasma-assisted chemical vapor deposition of a high-purity tungsten sputtering target material, which comprises the following steps: s1, forming a stress slow release layer on the matrix to obtain a modified matrix; s2, placing the modified substrate in a PECVD vacuum furnace, taking tungsten hexafluoride and hydrogen as reaction gases, taking argon as protective carrier gas, and depositing pure tungsten on the surface of the modified substrate until a tungsten layer with the required thickness is obtained; and S3, annealing the obtained tungsten plate blank in a hydrogen atmosphere, and rolling to obtain the high-purity tungsten target. The method can be used for preparing the tungsten target material with large thickness and large area, the damage to the matrix is greatly reduced, and the prepared tungsten target material has the advantages of high purity, clean surface, high density and the like.
Description
Technical Field
The invention relates to the field of target sputtering, in particular to a preparation method of a high-purity tungsten sputtering target.
Background
Tungsten is a refractory (3410 ℃) and high-hardness metal, and has excellent conductive performance and relatively stable chemical performance. The method has wide application prospect in the industries of integrated circuit (mainly memory chip and radio frequency chip) preparation and the like. At present, tungsten sputtering target material blanks mainly adopt a powder metallurgy technology, and tungsten powder is loaded in a special die and then is sintered and formed by hot isostatic pressing or SPS discharge plasma, and the tungsten sputtering target material blanks can also be placed in a vacuum hot pressing furnace for hot pressing and forming. The mold and the vacuum hot pressing or hot isostatic pressing sintering furnace need to be designed according to the size of the target material. The processing of large-size high-purity tungsten targets is limited by the size of the die and the size and temperature of the hot pressing and hot isostatic pressing furnace. And then, carrying out hot rolling and cold rolling on the large-size tungsten target blank by using rolling processes such as cogging, rolling and the like so as to meet the requirements of the qualified tungsten target on size and physical properties. And the oxidation speed of tungsten metal such as exposed in the atmosphere is high during hot rolling, which easily causes surface contamination of high-purity tungsten. The tungsten target prepared by the method has the advantages of relatively complicated process flow, high energy consumption, existence of gaps in the product and relatively low purity.
Chemical Vapor Deposition (CVD) is a process for generating solid-phase deposits on the surface of a heated solid through vapor-phase chemical reaction, has the advantages of high deposition rate, stable and simple process and the like, and can deposit large-sized special-shaped products with compact tissues and complex shapes. When tungsten is produced by a common CVD method, H is generally used2Reduction of WF6Or WCl6The prepared coating has the thickness of less than 40mm, has large thermal stress with the substrate, and has large damage to the substrate. Aiming at the problems, the invention provides a preparation method of a high-purity tungsten target material with large thickness, so as to overcome the defects of the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for plasma-assisted chemical vapor deposition of a high-purity tungsten sputtering target material, which aims to solve the problems that the thickness of the existing tungsten target material blank is limited, the damage to a substrate is large, the surface is easy to oxidize and pollute, the purity of the tungsten target material is low and the like.
The applicant can solve the problem of the mismatch of the thermal expansion coefficients between the tungsten and copper substrates by connecting a stress slow release layer on the substrate before the chemical vapor deposition. However, the method still has the technical problems that a coating with the thickness of more than 40mm cannot be deposited, so that a target with enough thickness cannot be obtained, the preparation method has high cost, and the damage to the substrate is large. In view of the above technical problems, the applicant has found that when the coating is deposited by chemical vapor deposition in a PECVD vacuum furnace, a coating with a thickness of 50mm or even more can be obtained, and finally a target with sufficient thickness can be obtained, and the damage to the substrate is greatly reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for plasma-assisted chemical vapor deposition of a high-purity tungsten sputtering target material comprises the following steps:
s1, forming a stress slow release layer on the substrate to obtain a modified substrate;
s2, placing the modified substrate in a PECVD vacuum furnace, taking tungsten hexafluoride and hydrogen as reaction gases, taking argon as protective carrier gas, and depositing pure tungsten on the surface of the modified substrate until a tungsten layer with the required thickness is obtained;
and S3, annealing the obtained tungsten plate blank in a hydrogen atmosphere, and rolling to obtain the high-purity tungsten target.
In step S1, a stress-relieving layer may be attached to the substrate by hot isostatic pressing, thermal diffusion welding, or brazing.
Preferably, in step S2, the vacuum degree of the deposition is 100-500Pa, the deposition temperature is 250-600 ℃, and the deposition rate is 0.2-1 mm/h.
Preferably, in step S2, the molar ratio of tungsten hexafluoride to hydrogen in the reaction gas is 1-3: 4.
Preferably, in step S3, the annealing temperature is 1000-1600 ℃.
Preferably, in step S2, after the deposition of pure tungsten is completed, the heating is stopped, the introduction of tungsten hexafluoride is stopped, and hydrogen and argon are introduced during the cooling process.
Preferably, the purity of tungsten hexafluoride, hydrogen, and argon is greater than or equal to 99.999%.
Preferably, the stress slow release layer is made of tungsten-copper gradient material, nickel or titanium; the thickness of the stress slow release layer is 2-5 mm.
Preferably, in step S2, before placing the modified substrate in the PECVD vacuum furnace, a step of pretreating the modified substrate is further included; the pretreatment comprises the following steps: polishing and grinding the connected matrix, cleaning oil stain with acetone, cleaning with absolute ethyl alcohol, and dehydrating and drying.
Preferably, the substrate is a red copper substrate, and the diameter of the substrate is 100-500 mm.
Preferably, the purity of the obtained high-purity tungsten target material is more than or equal to 6N, and the density is 19.1-19.2g/cm3。
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, a stress slow release layer is deposited on the substrate, then plasma-assisted chemical vapor deposition is carried out in a PECVD (plasma enhanced chemical vapor deposition) vacuum furnace by taking hydrogen and tungsten hexafluoride as raw materials and argon as carrier gas, so that high-purity tungsten targets with different thicknesses and shapes can be obtained, different requirements on the tungsten targets are met, the obtained tungsten targets also have the advantages of high purity, high density, clean surface, few defects and the like, the material performance can more easily meet the requirements of application to integrated circuits, and the damage to the substrate is small.
2. The invention obtains high density (19.10-19.2 g/cm) by optimizing process parameters3) And tungsten targets up to 50mm in thickness.
3. The preparation method has the advantages of simple process, no pollution to the target material, high deposition rate, low deposition temperature, high production efficiency and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Example 1:
a method for plasma-assisted chemical vapor deposition of a high-purity tungsten sputtering target, the process flow diagram of which is shown in FIG. 1, comprises:
a layer of 2mm nickel is brazed on a flat red copper substrate with the diameter of 400mm and the thickness of 10mm by thermal diffusion welding. Polishing and grinding the connected matrix, cleaning oil stain with acetone, cleaning with absolute ethyl alcohol, and dehydrating and drying. The substrate was placed in a PECVD vacuum furnace. High-purity tungsten hexafluoride and high-purity hydrogen (the purity is more than or equal to 99.999%) are used as reaction gases, high-purity argon (the purity is more than or equal to 99.999%) is used as protective carrier gas, and deposition is carried out on a red copper matrix under the conditions of vacuum degree of 200Pa and deposition temperature of 350 ℃. Molar ratio of reaction gas WF6:H2=1:2.5, after the reaction is completed, heating is stopped, and then WF is turned off6Continuing to introduce H2And Ar is cooled to room temperature. The obtained product has the diameter of 400mm, the thickness of 25mm, the purity of more than or equal to 6N and the density of 19.16g/cm3A tungsten slab. Annealing the tungsten plate blank at 1400 ℃ in a hydrogen atmosphere, and then rolling to obtain the high-purity tungsten target material.
Example 2:
a layer of 2mm nickel is brazed on a flat red copper substrate with the diameter of 400mm and the thickness of 10mm by thermal diffusion welding. Polishing and grinding the connected matrix, cleaning oil stain with acetone, cleaning with absolute ethyl alcohol, and dehydrating and drying. The substrate was placed in a PECVD vacuum furnace. High-purity tungsten hexafluoride and high-purity hydrogen (the purity is more than or equal to 99.999%) are used as reaction gases, high-purity argon (the purity is more than or equal to 99.999%) is used as protective carrier gas, and deposition is carried out on a red copper matrix under the conditions that the vacuum degree is 200Pa and the deposition temperature is 450 ℃. Molar ratio of reaction gas WF6:H2=1:2.5, after the reaction is completed, heating is stopped, and then WF is turned off6Continuing to introduce H2Cooling with Ar to room temperature to obtain a product with diameter of 400mm, thickness of 40mm, purity of 6N or more, and density of 19.18g/cm3A tungsten slab. Annealing the tungsten plate blank at 1400 ℃ in a hydrogen atmosphere, and then rolling to obtain the high-purity tungsten target material.
Example 3:
a layer of 2mm tungsten-copper gradient material is brazed on a flat red copper substrate with the diameter of 400mm and the thickness of 10mm through thermal diffusion welding. The tungsten-copper gradient material is prepared by adopting an infiltration-welding method. The tungsten content in the tungsten-copper gradient material is 50 wt.%. Polishing and grinding the connected matrix, cleaning oil stain with acetone, cleaning with absolute ethyl alcohol, and dehydrating and drying. The substrate was placed in a PECVD vacuum furnace. High-purity tungsten hexafluoride and high-purity hydrogen (the purity is more than or equal to 99.999%) are used as reaction gases, and high-purity argon is used as protective carrier gas, and deposition is carried out on a red copper matrix under the conditions that the vacuum degree is 200Pa and the deposition temperature is 450 ℃. Molar ratio of reaction gas WF6:H2=1:2.5, after the reaction is completed, heating is stopped, and then WF is turned off6Continuing to introduce H2And Ar is cooled to room temperature. The obtained product has a diameter of 400mm, a thickness of 50mm, a purity of more than or equal to 6N, and a density of 19.2g/cm3A tungsten slab. Annealing the tungsten plate blank at 1400 ℃ in a hydrogen atmosphere, and then rolling to obtain the high-purity tungsten target material.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for plasma-assisted chemical vapor deposition of a high-purity tungsten sputtering target material is characterized by comprising the following steps:
s1, forming a stress slow release layer on the matrix to obtain a modified matrix;
s2, placing the modified substrate in a PECVD vacuum furnace, taking tungsten hexafluoride and hydrogen as reaction gases, taking argon as protective carrier gas, and depositing pure tungsten on the surface of the modified substrate until a tungsten layer with the required thickness is obtained;
and S3, annealing the obtained tungsten plate blank in a hydrogen atmosphere, and rolling to obtain the high-purity tungsten target.
2. The method as claimed in claim 1, wherein in step S2, the deposition vacuum is 100-500Pa, the deposition temperature is 250-600 ℃, and the deposition rate is 0.2-1 mm/h.
3. The method according to claim 1, wherein in step S2, the molar ratio of tungsten hexafluoride to hydrogen in the reactive gas is 1-3: 4.
4. The method as claimed in claim 1, wherein the annealing temperature is 1000-1600 ℃ in step S3.
5. The method according to any of claims 1 to 4, wherein in step S2, after the deposition of pure tungsten is completed, the heating is stopped, the introduction of tungsten hexafluoride is stopped, and hydrogen and argon are introduced during the cooling process.
6. The method according to any of claims 1-4, wherein the stress-relaxation layer is made of a tungsten-copper gradient material, nickel or titanium; the thickness of the stress slow release layer is 2-5 mm.
7. The method according to any of claims 1 to 4, further comprising a step of pre-treating the modified substrate before placing the modified substrate in the PECVD vacuum furnace in step S2; the pretreatment comprises the following steps: polishing and grinding the connected matrix, cleaning oil stain with acetone, cleaning with absolute ethyl alcohol, and dehydrating and drying.
8. The method according to any of claims 1-4, wherein the substrate is a red copper substrate with a diameter of 100-500 mm.
9. The method for plasma-assisted chemical vapor deposition of a high-purity tungsten sputtering target according to any one of claims 1 to 4, wherein the purity of the obtained high-purity tungsten target is not less than 6N, and the density is 19.10 to 19.2g/cm3。
10. The method according to any of claims 1-4, wherein the purity of the tungsten hexafluoride, hydrogen and argon is greater than or equal to 99.999%.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115354308A (en) * | 2022-08-10 | 2022-11-18 | 安徽光智科技有限公司 | Deposition equipment and thin film resistor uniformity debugging method |
EP4350030A1 (en) * | 2022-09-26 | 2024-04-10 | Kokusai Electric Corporation | Method of processing substrate, method of manufacturing semiconductor device, substrate processing apparatus, and program |
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CN115354308A (en) * | 2022-08-10 | 2022-11-18 | 安徽光智科技有限公司 | Deposition equipment and thin film resistor uniformity debugging method |
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EP4350030A1 (en) * | 2022-09-26 | 2024-04-10 | Kokusai Electric Corporation | Method of processing substrate, method of manufacturing semiconductor device, substrate processing apparatus, and program |
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