CN113862620A - Preparation method of CIGS rotary sputtering target material - Google Patents
Preparation method of CIGS rotary sputtering target material Download PDFInfo
- Publication number
- CN113862620A CN113862620A CN202111092127.7A CN202111092127A CN113862620A CN 113862620 A CN113862620 A CN 113862620A CN 202111092127 A CN202111092127 A CN 202111092127A CN 113862620 A CN113862620 A CN 113862620A
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- target material
- cigs
- spraying
- sputtering target
- preparing
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- 239000013077 target material Substances 0.000 title claims abstract description 25
- 238000005477 sputtering target Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 32
- 238000005507 spraying Methods 0.000 claims abstract description 21
- 229910052738 indium Inorganic materials 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 7
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 7
- 238000012545 processing Methods 0.000 claims abstract description 7
- 238000005488 sandblasting Methods 0.000 claims abstract description 7
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000009689 gas atomisation Methods 0.000 claims abstract description 4
- 238000010288 cold spraying Methods 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 6
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 238000007514 turning Methods 0.000 claims description 3
- 238000012805 post-processing Methods 0.000 claims description 2
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 abstract description 10
- 239000010949 copper Substances 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 239000010409 thin film Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- -1 copper indium gallium selenide compound Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
Abstract
The invention provides a preparation method of a rotary copper indium gallium selenide sputtering target material, which comprises the following steps of 1, mixing Cu, In, Ga and Se as raw materials In proportion, and preparing spherical powder by adopting vacuum gas atomization; step 2, carrying out sand blasting coarsening on the back pipe; step 3, assembling the back tube on a spraying device, selecting a spraying process, and spraying spherical powder on the back tube to form a target material; and 4, carrying out post-treatment processing on the target. The preparation and processing of the copper indium gallium selenide target material are carried out by adopting the flow processes of copper indium gallium selenide powder preparation, back tube sand blasting, spraying and post-treatment, the obtained target material is not less than 98 percent, the yield is high, the powder utilization rate is high, and the large-scale production is easy.
Description
Technical Field
The invention relates to the field of target processing and production, in particular to a preparation method of a copper indium gallium selenide rotary sputtering target.
Background
The CIGS thin-film solar cell has the remarkable characteristics of low production cost, small pollution, no recession, good low-light performance and the like, the photoelectric conversion efficiency is the first of various thin-film solar cells, is close to that of crystalline silicon solar cells, is only one third of the cost, is called as a novel thin-film solar cell with very promising next generation, and is a hotspot for research and development in recent years. In addition, the battery has a soft and uniform black appearance, and is an ideal choice for places with higher requirements on appearance. The CIGS rotary sputtering target is a novel sputtering target, is a core material for manufacturing a module of a CIGS thin-film solar cell, and is mainly used for preparing a photoelectric conversion layer material of the CIGS thin-film solar cell by a sputtering selenization process.
Patent No. CN102199751B discloses a method for manufacturing a copper indium gallium selenide target, which comprises the steps of crushing and mixing a copper indium gallium selenide raw material to obtain a copper indium gallium selenide compound powder, pressing the copper indium gallium selenide compound powder into a blank by a forming machine, and sintering the blank at a high temperature to form a target, thereby forming the copper indium gallium selenide target, wherein the process effectively shortens the reaction time and improves the production efficiency, but the process adopts a hot-pressing sintering mode, and requires high-temperature equipment, so that the manufacturing cost is high; the requirement for manufacturing large-size targets cannot be met due to equipment limitation; the target material manufactured is a planar target material. Sputtering is less efficient and more costly, and it is therefore important to address this problem.
Disclosure of Invention
The invention aims to provide a preparation method of a CIGS rotary sputtering target, which solves the problems of high cost, large size and high utilization rate in the manufacturing of the CIGS sputtering target in the background technology by preparing CIGS into powder for mixing and spraying the powder on a back tube through spraying equipment.
The invention provides a preparation method of a rotary copper indium gallium selenide sputtering target material, which comprises the following steps of 1, mixing Cu, In, Ga and Se as raw materials In proportion, and preparing spherical powder by adopting vacuum gas atomization; step 2, carrying out sand blasting coarsening on the back pipe; step 3, assembling the back tube on a spraying device, selecting a spraying process, and spraying spherical powder on the back tube to form a target material; and 4, carrying out post-treatment processing on the target.
The further improvement lies in that: the atomic ratio of Cu, In, Ga and Se is 0.9-1.3: 0.6-0.9:0.2-0.5:1.5-2.5, the granularity of the spherical powder is 5-500 meshes, and the purity is more than or equal to 3N.
The further improvement lies in that: the spraying process adopts a cold spraying process.
The further improvement lies in that: the cold spraying process parameters are that the cooling water temperature is 0-80 ℃; the pressure of the cavity is 1-10Mpa, the gas temperature is 300-1500 ℃, the spray gun is PCS-300-PCS-800, the gun distance is 10-100mm, the moving speed of the spray gun is 1-100mm/s, the rotating speed of the back pipe is 100-500rpm, the powder feeding flow is 5-200SLM, and multiple paths of powder feeding are adopted, wherein the powder feeding amount of each path is 10-100 g/min.
The further improvement lies in that: the thickness of the single-side spraying is 1-30 mm.
The further improvement lies in that: the post-processing comprises processing the surface of the target by a turning tool; and (5) carrying out product inspection and packaging on the machined target material.
The invention has the beneficial effects that: the method has the advantages that the steps of forming the target at high temperature are reduced and the production cost is reduced by adopting the preparation of the copper indium gallium selenide powder, sand blasting of the back tube, bottoming of the back tube, cold spraying, machining and inspection;
the powder is sprayed out by high-speed airflow at the temperature far lower than the melting point of the material by cold spraying, and powder particles finally impact on a substrate at a high speed of more than 600m/s to generate plastic deformation deposition to form a coating, and the coating has the advantages of compact structure, low porosity, uniform components and the like; through high-speed spraying, the particles impact the substrate at high speed to fully deform to form a coating, the coating has compact structure, the relative density of the target material is more than or equal to 98 percent, the oxygen content is less than or equal to 3000ppm, the nitrogen content is less than or equal to 1000ppm, the grain structure is uniformly refined, the yield is high, the powder utilization rate is high, and the large-scale production is easy;
by adopting the cold spraying process, the rotary sputtering target material with the length of 100-8000mm can be prepared, the length can be adjusted according to the requirements of users, the unilateral thickness of the coating is 1-30mm, the utilization rate of the target material is improved, the thickness can be adjusted according to the requirements of the users, the production cost is effectively reduced, and the coating requirement of large-size products of the users is met.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the present invention.
The embodiment provides a preparation method of a rotary copper indium gallium selenide sputtering target, which comprises the following steps of 1, mixing Cu, In, Ga and Se serving as raw materials In proportion, wherein the atomic ratio of Cu, In, Ga and Se is 1: 0.7:0.3: 2, preparing spherical powder by vacuum gas atomization, wherein the granularity of the powder is 5-500 meshes, and the purity is more than or equal to 3N;
step 2, performing sand blasting coarsening on the surface of the back pipe by using a sand blasting machine;
step 3, assembling the back pipe on spraying equipment, and setting plasma spraying process parameters by adopting a cold spraying process, wherein the process parameters are that the cooling water temperature is 0-80 ℃; the pressure of the cavity is 1-10Mpa, the gas temperature is 300-1500 ℃, the spray gun is PCS-300-PCS-800, the gun distance is 10-100mm, the moving speed of the spray gun is 1-100mm/s, the rotating speed of the back pipe is 100-500rpm, the powder feeding flow is 5-200SLM, and multiple paths of powder feeding can be adopted during spraying, wherein the powder feeding amount of each path is 10-100 g/min;
the thickness of the single-side spraying is 20 mm.
Step 5, machining the surface of the target by using a turning tool;
and 6, inspecting and packaging the product.
The target material prepared by the embodiment is integrated, splicing and binding are not needed, expensive metal indium is saved, the cost of the target material is reduced, the CIGS is prepared into powder and mixed to prepare spherical powder, the powder is sprayed on the surface of the back tube to form a coating by adopting a cold spraying mode through spraying equipment, and the density of the coating is increased.
The method has the advantages of simple process and low cost, can prepare large-size target materials meeting the requirements of customers, has the relative density of more than or equal to 98 percent and uniform components, and can meet the requirements of the current market.
Claims (6)
1. A preparation method of a CIGS rotary sputtering target material is characterized by comprising the following steps of 1, mixing Cu, In, Ga and Se serving as raw materials In proportion, and preparing spherical powder by adopting vacuum gas atomization; step 2, carrying out sand blasting coarsening on the back pipe; step 3, assembling the back tube on a spraying device, selecting a spraying process, and spraying spherical powder on the back tube to form a target material; and 4, carrying out post-treatment processing on the target.
2. The method for preparing the CIGS rotary sputtering target material according to claim 1, wherein the method comprises the following steps: the atomic ratio of Cu, In, Ga and Se is 0.9-1.3: 0.6-0.9:0.2-0.5:1.5-2.5, the granularity of the spherical powder is 5-500 meshes, and the purity is more than or equal to 3N.
3. The method for preparing the CIGS rotary sputtering target material according to claim 1, wherein the method comprises the following steps: the spraying process adopts a cold spraying process.
4. The method for preparing the CIGS rotary sputtering target material according to claim 3, wherein the method comprises the following steps: adopting a cold spraying process, wherein the process parameters are that the temperature of cooling water is 0-80 ℃; the pressure of the cavity is 1-10Mpa, the gas temperature is 300-1500 ℃, the spray gun is PCS-300-PCS-800, the gun distance is 10-100mm, the moving speed of the spray gun is 1-100mm/s, the rotating speed of the back pipe is 100-500rpm, the powder feeding flow is 5-200SLM, and multiple paths of powder feeding are adopted, wherein the powder feeding amount of each path is 10-100 g/min.
5. The method for preparing the CIGS rotary sputtering target material according to claim 1, wherein the method comprises the following steps: the thickness of the single-side spraying is 1-30 mm.
6. The method for preparing the CIGS rotary sputtering target material according to claim 1, wherein the method comprises the following steps: the post-processing comprises processing the surface of the target by a turning tool; and (5) carrying out product inspection and packaging on the machined target material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111092127.7A CN113862620A (en) | 2021-09-17 | 2021-09-17 | Preparation method of CIGS rotary sputtering target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111092127.7A CN113862620A (en) | 2021-09-17 | 2021-09-17 | Preparation method of CIGS rotary sputtering target material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113862620A true CN113862620A (en) | 2021-12-31 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111092127.7A Pending CN113862620A (en) | 2021-09-17 | 2021-09-17 | Preparation method of CIGS rotary sputtering target material |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818465A (en) * | 2015-04-17 | 2015-08-05 | 无锡舒玛天科新能源技术有限公司 | Copper/indium/gallium rotating target and method for preparing copper/indium/gallium rotating target by controllable atmosphere cold spraying |
| CN106825592A (en) * | 2016-12-22 | 2017-06-13 | 广州市尤特新材料有限公司 | A kind of preparation method of the alloy powder for cold spraying |
| CN107557737A (en) * | 2017-08-04 | 2018-01-09 | 米亚索乐装备集成（福建）有限公司 | A kind of method for preparing tubular target |
| CN107904565A (en) * | 2017-10-27 | 2018-04-13 | 包头稀土研究院 | The preparation method of Cu In Ga Se compound rotary target materials |
| CN109295428A (en) * | 2018-11-02 | 2019-02-01 | 中国科学院宁波材料技术与工程研究所 | A kind of method and products thereof using cold spray process preparation copper and indium gallium rotary target material |
| CN111826625A (en) * | 2020-07-22 | 2020-10-27 | 厦门佰事兴新材料科技有限公司 | Preparation method of alloy target material and alloy target material prepared by using method |
-
2021
- 2021-09-17 CN CN202111092127.7A patent/CN113862620A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818465A (en) * | 2015-04-17 | 2015-08-05 | 无锡舒玛天科新能源技术有限公司 | Copper/indium/gallium rotating target and method for preparing copper/indium/gallium rotating target by controllable atmosphere cold spraying |
| CN106825592A (en) * | 2016-12-22 | 2017-06-13 | 广州市尤特新材料有限公司 | A kind of preparation method of the alloy powder for cold spraying |
| CN107557737A (en) * | 2017-08-04 | 2018-01-09 | 米亚索乐装备集成（福建）有限公司 | A kind of method for preparing tubular target |
| CN107904565A (en) * | 2017-10-27 | 2018-04-13 | 包头稀土研究院 | The preparation method of Cu In Ga Se compound rotary target materials |
| CN109295428A (en) * | 2018-11-02 | 2019-02-01 | 中国科学院宁波材料技术与工程研究所 | A kind of method and products thereof using cold spray process preparation copper and indium gallium rotary target material |
| CN111826625A (en) * | 2020-07-22 | 2020-10-27 | 厦门佰事兴新材料科技有限公司 | Preparation method of alloy target material and alloy target material prepared by using method |
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Application publication date: 20211231 |