CN109763109B - Liquid metal target material and method for preparing alloy film by using same - Google Patents
Liquid metal target material and method for preparing alloy film by using same Download PDFInfo
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- CN109763109B CN109763109B CN201910161639.0A CN201910161639A CN109763109B CN 109763109 B CN109763109 B CN 109763109B CN 201910161639 A CN201910161639 A CN 201910161639A CN 109763109 B CN109763109 B CN 109763109B
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- 229910001338 liquidmetal Inorganic materials 0.000 title claims abstract description 50
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 37
- 239000000956 alloy Substances 0.000 title claims abstract description 37
- 239000013077 target material Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims description 28
- 238000004544 sputter deposition Methods 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims description 36
- 239000010949 copper Substances 0.000 claims description 29
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 27
- 229910052802 copper Inorganic materials 0.000 claims description 27
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 17
- 229910052733 gallium Inorganic materials 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000000576 coating method Methods 0.000 claims description 12
- 239000011701 zinc Substances 0.000 claims description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 11
- 229910052725 zinc Inorganic materials 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 10
- 229910052738 indium Inorganic materials 0.000 claims description 10
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 10
- 229910000846 In alloy Inorganic materials 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000005240 physical vapour deposition Methods 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 239000003929 acidic solution Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 2
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000010408 film Substances 0.000 description 27
- 239000000126 substance Substances 0.000 description 8
- 238000001755 magnetron sputter deposition Methods 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 238000010248 power generation Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910002056 binary alloy Inorganic materials 0.000 description 2
- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910002058 ternary alloy Inorganic materials 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910000807 Ga alloy Inorganic materials 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052951 chalcopyrite Inorganic materials 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010288 cold spraying Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
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Abstract
The invention relates to the field of sputtering film preparation, in particular to a liquid metal target and an alloy film prepared by the liquid metal target. The liquid metal target material has the advantages of simple preparation process, high alloy film growth speed when the liquid metal target material is used for preparing alloy, uniform and controllable thickness, simple operation, high efficiency and convenience, realization of an alloy film with continuously controllable thickness from a nanoscale to a microscale, higher conductivity and stronger production applicability.
Description
Technical Field
The invention relates to the field of preparation of alloy films, in particular to a liquid metal target material used in a film prepared by a magnetron sputtering method and an alloy film prepared by the liquid metal target material.
Background
Energy is a common concern in the world, and solar power generation becomes an important industry for solving the energy crisis. The CIGS thin-film solar cell is a chalcopyrite crystal thin-film solar cell consisting of four elements of Cu (copper), In (indium), Ga (gallium) and Se (selenium), has the advantages of strong light absorption capacity, good power generation stability, high conversion efficiency, long power generation time In the daytime, high power generation quantity, low production cost, short energy recovery period and the like, and is gradually and widely applied. The preparation of the CIGS light absorption layer is important for the manufacturing of CIGS thin film batteries, and the preparation methods of the CIGS thin film mainly comprise a solvothermal method, a spray pyrolysis method, an ion sintering method, a chemical deposition method, a reactive sputtering method, a vacuum evaporation method and the like. The selenization of a Copper Indium Gallium (CIG) alloy layer deposited by magnetron sputtering has become a mainstream preparation technology in the industry. The magnetron sputtering method of the copper indium gallium alloy layer generally includes the following two methods: the first is to adopt a mode of co-sputtering a CuGa binary alloy target and an In target, and the second is to directly sputter a CuInGa ternary alloy target. The method of smelting CuInGa or CuGa target material has narrow component and process window; the intermediate phase is easy to form and segregation occurs, so that the utilization rate of the sprayed powder is low (generally about 40-60%) in the finally formed alloy film uneven cold spraying method, only a rotary target material can be prepared, and the method is difficult to be used for producing a planar target material. The higher melting temperature (1084 ℃ higher than the melting point of copper) of the cold-pressing particle forming method can cause the indium or gallium with low melting point to be volatilized seriously, so that the alloy composition of the final particles is not matched with the designed composition; the IGZO film is prepared by adopting an indium gallium zinc oxide target magnetron sputtering method, the target preparation process is complex, the sputtering uniformity is poor, and the quality of the film layer is further influenced.
In addition, indium gallium zinc oxide IGZO is a novel semiconductor material having higher electron mobility than amorphous silicon (α -Si). IGZO is used in a new generation of high performance Thin Film Transistors (TFTs) as a channel material, thereby improving display panel resolution. The high-performance thin film transistor can be used on a display screen and can also replace a traditional monocrystalline silicon-based electronic chip. The preparation process has similar problems with magnetron sputtering CuInGa film.
Disclosure of Invention
Aiming at the problems in the prior art in preparing alloy targets and magnetron sputtering alloy films, the invention firstly provides a liquid metal target which comprises a target substrate and a liquid metal target layer coated on the surface of the target substrate, wherein the liquid metal is gallium-based alloy or gallium, and the target substrate is copper or iron.
Compared with the traditional CuGa or CuGaIn target material, the liquid metal is uniformly distributed on the surface of the target material substrate in a liquid state, no intermediate phase is formed in the preparation process, the uniformity of the alloy film formed after final sputtering can be ensured, and the alloy component of the final particles is ensured to be matched with the designed component.
Preferably, the thickness of the liquid metal target material layer is 0.1-1.0 mm. The thickness can achieve uniform coverage of the liquid metal layer to the surface and ensure adhesion of the liquid metal to the target substrate surface.
Preferably, the gallium-based alloy is a gallium-indium alloy.
More preferably, the molar percentage of gallium in the gallium-indium alloy is 20 to 100%, and more preferably 40 to 60%.
Preferably, the content of impurities in the elementary indium and the elementary gallium is not more than 0.01 percent
Preferably, the liquid metal target material is prepared by the following method: and (3) placing the liquid metal and the target substrate in an acid solution for treatment, so that the liquid metal covers the surface of the target substrate.
Preferably, the pH value of the acidic solution is less than 2, and the acidic solution is treated for 1-10 min at the temperature of 20-100 ℃;
preferably, the pH value of the acid solution is 0-1, and the acid solution is treated for 1-5 min at the temperature of 40-80 ℃.
The invention also aims to protect the method for preparing the alloy film by utilizing the liquid metal target material, and the main improvement point is that the alloy film is prepared by taking the liquid metal target material and copper or zinc as raw materials through a co-sputtering method.
Preferably, the copper content in the copper target is more than 99.99%, and the zinc content in the zinc target is more than 99.99%.
Preferably, the method comprises the following steps: and (3) placing the liquid metal target and the copper target or placing the liquid metal target and the zinc target in physical vapor deposition coating equipment for coating by a co-sputtering method.
Preferably, the plating conditions of the liquid metal target are as follows: argon flow is 10-30 sccm, oxygen flow is 0 or 10-30 sccm, target base distance is 18-40mm, substrate temperature is 15-25 ℃, and sputtering power is 40-100W.
The plating conditions of the copper or zinc target are as follows: argon gas flow is 10-30 sccm, the target base distance is 18-40mm, the substrate temperature is 15-25 ℃, and the sputtering power is 40-100W.
Preferably, the solid substrate includes but is not limited to one or more of silicon wafer, glass, copper, molybdenum, PDMS;
further preferred is a silicon wafer, molybdenum or glass.
Preferably, the preparation method of the alloy film comprises the following steps:
1) coating a gallium-based liquid metal target material layer on the surface of copper or iron of the target material substrate to obtain a liquid metal target material;
2) and preparing an alloy film by using the liquid metal target material and the copper target material or the zinc target material as raw materials through a co-sputtering method.
The invention also protects the alloy film prepared by the method; a GaInZn film or a CuGaIn film is preferred.
Preferably, the GaInZn alloy film is sputtered in an oxygen atmosphere and is subjected to oxidation treatment, preferably at the temperature of 300-800 ℃, for 2-12 hours, so as to obtain the IGZO film.
A final object of the invention is to protect the use of said liquid metal alloy film in the preparation of solar cells;
preferably in the production of light-absorbing layers for solar cells.
The invention has the following beneficial effects:
1) compared with the prior art that the CuGa binary alloy target and the In target are co-sputtered or the CuInGa ternary alloy target is directly sputtered, the method disclosed by the invention has the advantages that the liquid metal is coated on the copper or iron target substrate, the liquid metal can be spread and wetted on the treated copper or iron substrate, the target with uniformly distributed liquid state can be obtained, no liquid and solid intermediate phase exists, and the uniformity of a sputtered film can be further ensured.
2) The liquid metal target material has the advantages of simple preparation process, high growth speed of the alloy film prepared by the target material, uniform and controllable thickness, simple operation, high efficiency and convenience, and can realize the alloy film with the continuously controllable thickness from the nanoscale to the microscale.
Drawings
FIG. 1 is a diagram of a liquid metal target according to example 1;
FIG. 2 is an SEM picture of a CuInGa alloy film of example 1;
FIG. 3 is a SEM image of a section of a GaInZn alloy film of example 2.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
The embodiment first relates to a hydraulic metal target, which includes a target substrate and a gallium-indium alloy target layer covering the surface of the target substrate, wherein the target substrate is copper.
In the gallium-indium alloy, the molar ratio of simple substance indium to simple substance gallium is 50:50, the thickness of the target material layer is 0.8mm, and the impurity content of the simple substance indium and the simple substance gallium is not more than 0.01%;
the target material is prepared by the following method:
the copper target substrate and the liquid metal GaIn alloy are put into an acid solution with the pH value of 0, and a liquid metal GaIn alloy layer is prepared on the surface of the copper target at the temperature of 40 ℃ (see figure 1, the preparation time is 5min), and as can be seen from figure 1, the liquid metal alloy layer is uniformly covered on the copper substrate.
The invention also relates to a liquid metal film, and the preparation method comprises the following steps: and (3) taking a copper target with the copper content of more than 99.99% as a raw material, and putting the liquid metal target and the Cu target into PVD (physical vapor deposition) to carry out co-sputtering and plating of CuInGa on a silicon wafer (shown in an SEM (figure 2)). The PVD coating process comprises the following steps: the liquid metal target coating conditions are as follows: argon flow of 15sccm, oxygen flow of 0sccm, target base distance of 40mm, substrate temperature of 20 ℃ and sputtering power of 40W. The plating conditions of the copper target are as follows: argon gas flow of 30sccm, target base distance of 18mm, substrate temperature of 25 ℃ and sputtering power of 100W.
As can be seen from FIG. 2, the alloy film layer obtained by sputtering according to the method of the present invention has uniform and dense grain distribution.
Example 2
The embodiment first relates to a hydraulic metal target, which includes a target substrate and a gallium-indium alloy target layer covering the surface of the target substrate, wherein the target substrate is copper.
In the gallium-indium alloy, the molar ratio of simple substance indium to simple substance gallium is 40:60, and the thickness of the target material layer is 0.5 mm. The impurity content of the simple substance indium and the simple substance gallium is not more than 0.01 percent.
The target material is prepared by the following method:
and (3) putting the copper target substrate and the liquid metal GaIn alloy into an acid solution with the pH value of 1, and preparing a liquid metal GaIn alloy layer on the surface of the copper target at the temperature of 60 ℃ for 2 min.
The method comprises the steps of taking a material with the zinc content of more than 99.99% as a zinc target, putting a liquid metal target and a Zn target into PVD (physical vapor deposition) to carry out co-sputtering and coating of GaInZn on a silicon wafer substrate (an alloy section SEM is shown in figure 3). The PVD coating process comprises the following steps: the liquid metal target coating conditions are as follows: argon flow of 20sccm, oxygen flow of 30sccm, target base distance of 25mm, substrate temperature of 20 ℃ and sputtering power of 60W. The plating conditions of the zinc target are as follows: argon gas flow of 30sccm, oxygen gas flow of 30sccm, target base distance of 20mm, substrate temperature of 25 ℃, and sputtering power of 80W.
As can be seen from FIG. 3, the GaInZn coating prepared by the method of the invention is compact and has uniform thickness.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (5)
1. A preparation method of a GaInZn alloy film or a CuGaIn alloy film is characterized by comprising the following steps: placing a metal target and a copper target or placing a liquid metal target and a zinc target in physical vapor deposition coating equipment for coating by a co-sputtering method;
the coating conditions of the liquid metal target material are as follows: argon gas flow is 10-30 sccm, oxygen flow is 0 or 10-30 sccm, target base distance is 18-40mm, substrate temperature is 15-25 ℃, and sputtering power is 40-100W;
the plating conditions of the copper or zinc target material are as follows: argon gas flow is 10-30 sccm, oxygen flow is 0 or 10-30 sccm, target base distance is 18-40mm, substrate temperature is 15-25 ℃, and sputtering power is 40-100W;
the liquid metal target comprises a target substrate and a liquid metal target layer covering the surface of the target substrate, the liquid metal is gallium-indium alloy, the molar percentage of gallium in the gallium-indium alloy is 40-60%, and the target substrate is copper or iron;
the liquid metal target is prepared by the following method: placing liquid metal and a target substrate in an acid solution for treatment, so that the liquid metal covers the surface of the target substrate;
the pH value of the acidic solution is 0-1, and the acidic solution is treated for 1-5 min at the temperature of 40-80 ℃.
2. The method according to claim 1, wherein the thickness of the liquid metal target layer is 0.1 to 1 mm.
3. The method according to claim 1, wherein the content of impurities in the elemental indium and gallium is not more than 0.01%.
4. The method of claim 1, wherein the substrate comprises one or more of but not limited to silicon wafer, glass, copper, molybdenum, PDMS.
5. The method according to claim 4, wherein the substrate is a silicon wafer, molybdenum, or glass.
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| CN112062147B (en) * | 2020-09-21 | 2021-11-09 | 山东大学 | Low-cost and high-efficiency preparation method of lutetium oxide film |
| CN115504845B (en) * | 2021-06-22 | 2023-10-13 | 中国科学院理化技术研究所 | Liquid metal working medium belt for laser micro-propulsion and preparation method thereof |
| CN115747744B (en) * | 2023-01-06 | 2023-04-21 | 中国科学院理化技术研究所 | Gallium indium oxide film and preparation method thereof |
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| US5211824A (en) * | 1991-10-31 | 1993-05-18 | Siemens Solar Industries L.P. | Method and apparatus for sputtering of a liquid |
| KR20030071926A (en) * | 2002-03-02 | 2003-09-13 | 엘지.필립스 엘시디 주식회사 | Sputtering target assembly and sputtering apparatus using the same |
| JP4982259B2 (en) * | 2007-06-14 | 2012-07-25 | 昭和電工株式会社 | Method for manufacturing group III nitride compound semiconductor light emitting device |
| EP2742539B1 (en) * | 2011-08-11 | 2016-03-02 | Nuvosun, Inc. | Sputtering systems for liquid target materials |
| JP5672252B2 (en) * | 2012-01-31 | 2015-02-18 | 新日鐵住金株式会社 | Cu-Ga sputtering target and manufacturing method thereof |
| CN107557718B (en) * | 2016-06-24 | 2019-07-19 | 中国科学院理化技术研究所 | Method for preparing inorganic nano material layer on surface of flexible material |
| CN106319469B (en) * | 2016-10-28 | 2018-08-24 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of copper and indium gallium alloy target |
| CN106498348B (en) * | 2016-12-12 | 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 apparatus preparing flexible electronic route using liquid metal |
| CN110218981A (en) * | 2019-06-28 | 2019-09-10 | 先导薄膜材料（广东）有限公司 | A kind of copper gallium target and preparation method thereof |
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