CN103290372B - A kind of copper indium gallium rotary target material preparation method for thin-film solar cells - Google Patents
A kind of copper indium gallium rotary target material preparation method for thin-film solar cells Download PDFInfo
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- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 31
- 239000013077 target material Substances 0.000 title claims abstract description 20
- 239000010409 thin film Substances 0.000 title claims description 12
- 239000010935 stainless steel Substances 0.000 claims abstract description 94
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 94
- 229910000807 Ga alloy Inorganic materials 0.000 claims abstract description 64
- 238000005507 spraying Methods 0.000 claims abstract description 64
- CDZGJSREWGPJMG-UHFFFAOYSA-N copper gallium Chemical compound [Cu].[Ga] CDZGJSREWGPJMG-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 32
- 229910000809 Alumel Inorganic materials 0.000 claims abstract description 12
- 239000012809 cooling fluid Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 19
- 238000004140 cleaning Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- 229910052738 indium Inorganic materials 0.000 claims description 6
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 239000000956 alloy Substances 0.000 abstract description 22
- 229910045601 alloy Inorganic materials 0.000 abstract description 21
- YYCNOHYMCOXPPJ-UHFFFAOYSA-N alumane;nickel Chemical compound [AlH3].[Ni] YYCNOHYMCOXPPJ-UHFFFAOYSA-N 0.000 abstract description 15
- 239000013078 crystal Substances 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 29
- 238000005516 engineering process Methods 0.000 description 14
- 238000012545 processing Methods 0.000 description 13
- 239000011159 matrix material Substances 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000010408 film Substances 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 230000005611 electricity Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 229910052711 selenium Inorganic materials 0.000 description 5
- 239000011669 selenium Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- QNWMNMIVDYETIG-UHFFFAOYSA-N gallium(ii) selenide Chemical compound [Se]=[Ga] QNWMNMIVDYETIG-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 206010023230 Joint stiffness Diseases 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000010339 dilation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Abstract
The invention provides a kind of preparation method of copper indium gallium rotary target material, comprise the preparation of the stainless steel cylindrical base member of bag nickel-and aluminum-containing or nickel-chrome alloy layer, comprise the preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer, comprise the steps such as the preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer.The method adopts low-voltage plasma heat spraying method successively alumel, copper indium or copper gallium alloy, copper indium gallium to be solidified successively and form copper indium gallium rotary target material on stainless steel cylindrical base member, overcome the defect of the binding operation in existing method, technique is simple, easy to operate, with low cost, and the target density produced is high, porosity is low, uniform composition, crystal grain are tiny, productive rate is high, quality is good.
Description
Technical field
The invention belongs to Application of Solar Energy apparatus field, particularly a kind of copper indium gallium rotary target material preparation method for thin-film solar cells.
Background technology
In the past few decades, the production scale of solar panel expands rapidly.2011, the rate of increase of U.S.'s solar energy industry was up to 109%, leading in technical field of new energies.In the development of solar panel field rapidly, it is provided with molybdenum layer, CIGS thin-film absorption layer, Cadmium Sulfide buffer layer, native oxide zinc, aluminium-zinc oxide Window layer and surface contact layer successively to copper-indium-galliun-selenium film solar cell usually on the glass film plates of one deck rigidity or the stainless steel plate of flexibility.According to the research report of LuxResearch, within 2011, CIGS thin-film solar market production capacity reaches 1.2GW, and will reach 2.3GW in 2015; Other solar cell research institutions all predict the market share of copper-indium-galliun-selenium film solar cell by by 2010 3% rise to 2015 6%, and 33% will be reached at the year two thousand twenty.This fully shows that copper-indium-galliun-selenium film solar cell technology is by the solar cell market of the Fashion of Future, and has huge business potential.Be classified as the most promising thin film solar cell technologies as by USDOE and other well-known solar cell research institutions, copper-indium-galliun-selenium film solar cell technology just by feat of its widely advantage attract increasing researchist and investor.Up to now, the efficiency of copper-indium-galliun-selenium film solar cell breaches 20.3% in the lab.Meanwhile, increasing company, mechanism are being devoted to the commercialization realizing this technology.
Sputter-deposition technology is widely used in the aspects such as solar cell, flat-panel screens, CD, microstructure circuit; Particularly, along with the emergence of copper indium gallium selenium solar hull cell in recent years, sputtering technology is for huge contribution has been made in the commercialization of copper indium gallium selenium solar cell.Demand as the critical material copper indium gallium target market of copper indium gallium selenium solar cell is increasing.The technology of various production of copper indium gallium target is arisen at the historic moment, as: high-temperature vacuum hot pressing sintering method, cold isostatic pressing process, hot isostatic pressing method, vacuum melting method.But existing method all needs follow-up binding technique, binding technology itself is a complicated process, and bound device is expensive.There are good thermal diffusivity, electroconductibility to make the target obtained and improve work-ing life and the service efficiency of target, but existing method all needs follow-up target binding technique, be bound together by brazing mode by target and backboard (normally metal copper plate), binding technology itself is a complicated process, and bound device is expensive; Meanwhile, once binding weak effect, so can make target rapid temperature increases and cause the problems such as the fusing of target sealing-off, target, apparatus overheat, time serious, sputtering equipment can be out of order or scrap.
Hot-spraying techniques utilizes certain thermal source, as dusty material is heated to melting or semi-melting state by electric arc, plasma arc, combustion flame etc., then melting or the atomization of semi-melting powdered material is made by the power of flame stream itself or additional high velocity air, and be ejected into through pretreated substrate material surface with certain speed, a kind of technology be combined with body material.Low-voltage plasma heat spraying method is the one of hot-spraying techniques, utilized the method to prepare many novel materials, new unit, and be applied to as light, magnetic recording, flat-panel screens, solar energy materials, the high-technology fields such as high temperature resistant, wear-resisting aerospace, rocket engine are one of energy-conservation and effective technologies of economizing on resources at present.
Summary of the invention
Goal of the invention: the object of this invention is to provide the copper indium gallium rotary target material preparation method for thin-film solar cells that a kind of technique is simple, with low cost.
Technical scheme: the preparation method of a kind of copper indium gallium rotary target material provided by the invention, comprises the following steps:
(1), in vacuum or shielding gas, adopt the stainless steel cylindrical base member surface spraying alumel layer that low-voltage plasma heat spraying method will be clean, cooling, obtains the stainless steel cylindrical base member of bag nickel-and aluminum-containing or nickel-chrome alloy layer;
(2), in vacuum or shielding gas, adopt low-voltage plasma heat spraying method by the stainless steel cylindrical base member surface spraying copper indium of bag nickel-and aluminum-containing or nickel-chrome alloy layer or copper gallium alloy layer, cooling, must comprise the stainless steel cylindrical base member of copper indium or copper gallium alloy layer;
(3), in vacuum or shielding gas, adopt low-voltage plasma heat spraying method to comprise the stainless steel cylindrical base member surface spraying copper indium gallium alloy layer of copper indium or copper gallium alloy layer, cool simultaneously, to obtain final product.
Wherein, stainless steel cylindrical base member top is provided with water inlet and water outlet; Method of cooling is: cooling fluid passed in stainless steel cylindrical base member.Make stainless steel cylindrical base member outside wall temperature lower than the solidification value of alloy after cooling, thus make the alloy fast deposition of molten state to the outside surface of cylinder and rapid solidification.
Wherein, in step (1), described stainless steel cylindrical base member is the stainless steel cylindrical base member through preheating, and preheating temperature is 60-120 DEG C.Preheating procedure can eliminate moisture and the moisture on stainless steel cylindrical base member surface, thus the interface temperature when alloy particle improving spraying contacts with stainless steel cylindrical base member, to improve the bonding strength of coating and matrix; Stress that the thermal dilation difference because of base material and coated material causes can be reduced and the alloy layer that causes ftractures simultaneously; Preheating temperature depends on the size of stainless steel cylindrical base member, shape and material, and the factor such as the thermal expansivity of stainless steel cylindrical base member and coating alloy material.
Wherein, in step (1), the cleaning method of described stainless steel cylindrical base member is: cleaned through suds cleaning, ultrasonic cleaning, deionized water successively on the surface of stainless steel cylinder base material.
Wherein, in step (1), the thickness of alumel layer is 50-200nm.
Wherein, in step (2), the thickness of copper indium or copper gallium alloy layer is 50-100nm.
Wherein, in step (3), the thickness of copper indium gallium alloy layer is 3-20mm.
Wherein, in step (3), the particle diameter of described copper indium gallium alloy powder is 2200-2600 order, and be preferably 2400 orders, in copper indium gallium alloy, the mol ratio of copper, indium, gallium is 1:(0.7-0.5): (0.3-0.5).
Beneficial effect: the copper indium gallium rotary target material preparation method for thin-film solar cells provided by the invention adopts low-voltage plasma heat spraying method successively alumel, copper indium or copper gallium alloy, copper indium gallium to be solidified successively and form copper indium gallium copper indium gallium rotary target material on stainless steel cylindrical base member, overcome the defect of the binding operation in existing method, technique is simple, easy to operate, with low cost, and the target density produced is high, porosity is low, uniform composition, crystal grain are tiny, productive rate is high, quality is good.
Specifically, the present invention has following outstanding advantage relative to prior art:
(1) technique is simple, productive rate is high, with low cost: the method does not need follow-up binding operation, and technique is simple, easy to operate, with low cost, does not need complicated molding, has good economic benefit ratio;
(2) good product quality: the present invention adopts low-voltage plasma heat spraying method, wherein plasma jet can arrive 2000m/s, velocity of particle can reach 300m/s, substrate temperature can reach 650 DEG C, and coating stress is less, thickness is high, compact structure; Meanwhile, under low pressure, flame passes is thicker elongated, and powder can be made to be heated evenly, and low-voltage plasma heat spraying method can adopt transferred arc electricity cleaning matrix surface, improves matrix surface active, improves the bonding force of coating and matrix; What the present invention obtained copper indium gallium rotary target material has the features such as density high (> 95%), porosity low (<0.5%), uniform composition, crystal grain tiny (particle diameter is less than 100 μm), does not have the defect such as to isolate of macroscopic view;
(3) constant product quality: the method adopts vacuum or shielding gas atmosphere such as argon gas or nitrogen effectively to avoid metal or metal alloy to be oxidized, thus effectively avoid oxidized metal or alloy can destroy the joint tightness degree of each alloy layer, reduce the performance of target.
Accompanying drawing explanation
Fig. 1 is the copper indium gallium rotary target material preparation technology schema of the present invention for thin-film solar cells.
Embodiment
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, concrete material proportion, processing condition and result thereof described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Embodiment 1
The preparation method of copper indium gallium rotary target material, is shown in Fig. 1, comprises the following steps:
(1) preparation of copper indium gallium alloy powder: be that the copper indium gallium alloy of 1:0.6:0.4 carries out Mechanical Crushing by the mol ratio of copper, indium, gallium, and after grinding with planetary ball mill, sieve, obtaining particle diameter is 2400 object copper indium gallium alloy powder;
(2) surface cleaning of stainless steel cylindrical base member: the surface of stainless steel cylinder base material is cleaned through suds cleaning, ultrasonic cleaning, deionized water successively;
(3) preheating: stainless steel cylindrical base member is preheated to 90 DEG C;
(4) preparation of the stainless steel cylindrical base member of bag nickel-and aluminum-containing or nickel-chrome alloy layer: in vacuum or shielding gas, adopt low-voltage plasma heat spraying method by the alumel layer of clean stainless steel cylindrical base member surface spraying 125nm thickness, cooling fluid passed in stainless steel cylindrical base member makes it be cooled to room temperature simultaneously, recording the temperature flowing out cooling fluid is between 120-160 DEG C, obtains the stainless steel cylindrical base member of bag nickel-and aluminum-containing or nickel-chrome alloy layer; Specifically, the basic craft course of low-voltage plasma heat spraying method comprises: reaction system vacuumized and be filled with shielding gas, by rust steel cylindrical base member surface preheating and utilize surperficial transferred arc electricity cleaning, spraying and cooling; Wherein, low-voltage plasma heat spraying method processing parameter is: argon gas (liter/min) 10-30; Powder feeding gas (liter/min) 0.2-1; Powder feeding rate (gram/minute); 10-60; Electric current (ampere): 450-600; Voltage (volt) 36-72; Spray is apart from (millimeter): 100-500; Vacuum pressure (Pa) 300-5000 during transferred arc process; In order to protect matrix further, avoiding matrix oxidized, hydrogen (liter/min) can also be passed into: 0.5-1.5;
(5) preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer is comprised: in vacuum or shielding gas, adopt low-voltage plasma heat spraying method by the copper indium of the stainless steel cylindrical base member surface spraying 75nm thickness of bag nickel-and aluminum-containing or nickel-chrome alloy layer or copper gallium alloy layer, cooling fluid passed in stainless steel cylindrical base member makes it be cooled to room temperature simultaneously, recording the temperature flowing out cooling fluid is between 120-160 DEG C, must comprise the stainless steel cylindrical base member of copper indium or copper gallium alloy layer, low-voltage plasma heat spraying method processing parameter is same step (4);
(6) preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer is comprised: in vacuum or shielding gas, low-voltage plasma heat spraying method is adopted to comprise the copper indium gallium alloy layer of the stainless steel cylindrical base member surface spraying 12mm thickness of copper indium or copper gallium alloy layer, cooling fluid passed in stainless steel cylindrical base member makes it be cooled to room temperature simultaneously, recording the temperature flowing out cooling fluid is between 120-160 DEG C, must comprise the stainless steel cylindrical base member of copper indium gallium alloy layer; Low-voltage plasma heat spraying method processing parameter is same step (4);
(7) will the stainless steel cylindrical base member cool to room temperature of copper indium gallium alloy be deposited, and mechanical workout be carried out to target and makes it meet dimension precision requirement and surfaceness, to obtain final product.
Embodiment 2
The preparation method of copper indium gallium rotary target material, is shown in Fig. 1, comprises the following steps:
(1) preparation of copper indium gallium alloy powder: be that the copper indium gallium alloy of 1:0.7:0.5 carries out Mechanical Crushing by the mol ratio of copper, indium, gallium, and after grinding with planetary ball mill, sieve, obtaining particle diameter is 2600 object copper indium gallium alloy powder;
(2) surface cleaning of stainless steel cylindrical base member: the surface of stainless steel cylinder base material is cleaned through suds cleaning, ultrasonic cleaning, deionized water successively;
(3) preheating: stainless steel cylindrical base member is preheated to 120 DEG C;
(4) preparation of the stainless steel cylindrical base member of bag nickel-and aluminum-containing or nickel-chrome alloy layer: in vacuum or shielding gas, adopt low-voltage plasma heat spraying method by the alumel layer of clean stainless steel cylindrical base member surface spraying 50nm thickness, be cooled to room temperature, obtain the stainless steel cylindrical base member of bag nickel-and aluminum-containing or nickel-chrome alloy layer; Specifically, the basic craft course of low-voltage plasma heat spraying method comprises: reaction system vacuumized and be filled with shielding gas, by rust steel cylindrical base member surface preheating and utilize surperficial transferred arc electricity cleaning, spraying and cooling; Wherein, low-voltage plasma heat spraying method processing parameter is: argon gas (liter/min) 10-30; Powder feeding gas (liter/min) 0.2-1; Powder feeding rate (gram/minute); 10-60; Electric current (ampere): 450-600; Voltage (volt) 36-72; Spray is apart from (millimeter): 100-500; Vacuum pressure (Pa) 300-5000 during transferred arc process; In order to protect matrix further, avoiding matrix oxidized, hydrogen (liter/min) can also be passed into: 0.5-1.5;
(5) preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer is comprised: in vacuum or shielding gas, adopt low-voltage plasma heat spraying method by the copper indium of the stainless steel cylindrical base member surface spraying 50nm thickness of bag nickel-and aluminum-containing or nickel-chrome alloy layer or copper gallium alloy layer, cooling fluid passed in stainless steel cylindrical base member makes it be cooled to room temperature simultaneously, recording the temperature flowing out cooling fluid is between 120-160 DEG C, must comprise the stainless steel cylindrical base member of copper indium or copper gallium alloy layer, low-voltage plasma heat spraying method processing parameter is same step (4);
(6) preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer is comprised: in vacuum or shielding gas, low-voltage plasma heat spraying method is adopted to comprise the copper indium gallium alloy layer of the stainless steel cylindrical base member surface spraying 3mm thickness of copper indium or copper gallium alloy layer, cooling fluid passed in stainless steel cylindrical base member makes it be cooled to room temperature simultaneously, recording the temperature flowing out cooling fluid is between 120-160 DEG C, must comprise the stainless steel cylindrical base member of copper indium gallium alloy layer; Low-voltage plasma heat spraying method processing parameter is same step (4);
(7) will the stainless steel cylindrical base member cool to room temperature of copper indium gallium alloy be deposited, and mechanical workout be carried out to target and makes it meet dimension precision requirement and surfaceness, to obtain final product.
Embodiment 3
The preparation method of copper indium gallium rotary target material, is shown in Fig. 1, comprises the following steps:
(1) preparation of copper indium gallium alloy powder: be that the copper indium gallium alloy of 1:0.5:0.3 carries out Mechanical Crushing by the mol ratio of copper, indium, gallium, and after grinding with planetary ball mill, sieve, obtaining particle diameter is 2200 object copper indium gallium alloy powder;
(2) surface cleaning of stainless steel cylindrical base member: the surface of stainless steel cylinder base material is cleaned through suds cleaning, ultrasonic cleaning, deionized water successively;
(3) preheating: stainless steel cylindrical base member is preheated to 60 DEG C;
(4) preparation of the stainless steel cylindrical base member of bag nickel-and aluminum-containing or nickel-chrome alloy layer: in vacuum or shielding gas, adopt low-voltage plasma heat spraying method by the alumel layer of clean stainless steel cylindrical base member surface spraying 200nm thickness, be cooled to room temperature, obtain the stainless steel cylindrical base member of bag nickel-and aluminum-containing or nickel-chrome alloy layer; Specifically, the basic craft course of low-voltage plasma heat spraying method comprises: reaction system vacuumized and be filled with shielding gas, by rust steel cylindrical base member surface preheating and utilize surperficial transferred arc electricity cleaning, spraying and cooling; Wherein, low-voltage plasma heat spraying method processing parameter is: argon gas (liter/min) 10-30; Powder feeding gas (liter/min) 0.2-1; Powder feeding rate (gram/minute); 10-60; Electric current (ampere): 450-600; Voltage (volt) 36-72; Spray is apart from (millimeter): 100-500; Vacuum pressure (Pa) 300-5000 during transferred arc process; In order to protect matrix further, avoiding matrix oxidized, hydrogen (liter/min) can also be passed into: 0.5-1.5;
(5) preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer is comprised: in vacuum or shielding gas, adopt low-voltage plasma heat spraying method by the copper indium of the stainless steel cylindrical base member surface spraying 100nm thickness of bag nickel-and aluminum-containing or nickel-chrome alloy layer or copper gallium alloy layer, cooling fluid passed in stainless steel cylindrical base member makes it be cooled to room temperature simultaneously, recording the temperature flowing out cooling fluid is between 120-160 DEG C, must comprise the stainless steel cylindrical base member of copper indium or copper gallium alloy layer, low-voltage plasma heat spraying method processing parameter is same step (4);
(6) preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer is comprised: in vacuum or shielding gas, low-voltage plasma heat spraying method is adopted to comprise the copper indium gallium alloy layer of the stainless steel cylindrical base member surface spraying 20mm thickness of copper indium or copper gallium alloy layer, cooling fluid passed in stainless steel cylindrical base member makes it be cooled to room temperature simultaneously, recording the temperature flowing out cooling fluid is between 120-160 DEG C, must comprise the stainless steel cylindrical base member of copper indium gallium alloy layer; Low-voltage plasma heat spraying method processing parameter is same step (4);
(7) will the stainless steel cylindrical base member cool to room temperature of copper indium gallium alloy be deposited, and mechanical workout be carried out to target and makes it meet dimension precision requirement and surfaceness, to obtain final product.
Embodiment 4
The preparation method of copper indium gallium rotary target material, is shown in Fig. 1, comprises the following steps:
(1) preparation of copper indium gallium alloy powder: be that the copper indium gallium alloy of 1:0.6:0.5 carries out Mechanical Crushing by the mol ratio of copper, indium, gallium, and after grinding with planetary ball mill, sieve, obtaining particle diameter is 2500 object copper indium gallium alloy powder;
(2) surface cleaning of stainless steel cylindrical base member: the surface of stainless steel cylinder base material is cleaned through suds cleaning, ultrasonic cleaning, deionized water successively;
(3) preheating: stainless steel cylindrical base member is preheated to 80 DEG C;
(4) preparation of the stainless steel cylindrical base member of bag nickel-and aluminum-containing or nickel-chrome alloy layer: in vacuum or shielding gas, adopt low-voltage plasma heat spraying method by the alumel layer of clean stainless steel cylindrical base member surface spraying 150nm thickness, be cooled to room temperature, obtain the stainless steel cylindrical base member of bag nickel-and aluminum-containing or nickel-chrome alloy layer; Specifically, the basic craft course of low-voltage plasma heat spraying method comprises: reaction system vacuumized and be filled with shielding gas, by rust steel cylindrical base member surface preheating and utilize surperficial transferred arc electricity cleaning, spraying and cooling; Wherein, low-voltage plasma heat spraying method processing parameter is: argon gas (liter/min) 10-30; Powder feeding gas (liter/min) 0.2-1; Powder feeding rate (gram/minute); 10-60; Electric current (ampere): 450-600; Voltage (volt) 36-72; Spray is apart from (millimeter): 100-500; Vacuum pressure (Pa) 300-5000 during transferred arc process; In order to protect matrix further, avoiding matrix oxidized, hydrogen (liter/min) can also be passed into: 0.5-1.5;
(5) preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer is comprised: in vacuum or shielding gas, adopt low-voltage plasma heat spraying method by the copper indium of the stainless steel cylindrical base member surface spraying 60nm thickness of bag nickel-and aluminum-containing or nickel-chrome alloy layer or copper gallium alloy layer, cooling fluid passed in stainless steel cylindrical base member makes it be cooled to room temperature simultaneously, recording the temperature flowing out cooling fluid is between 120-160 DEG C, must comprise the stainless steel cylindrical base member of copper indium or copper gallium alloy layer, low-voltage plasma heat spraying method processing parameter is same step (4);
(6) preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer is comprised: in vacuum or shielding gas, low-voltage plasma heat spraying method is adopted to comprise the copper indium gallium alloy layer of the stainless steel cylindrical base member surface spraying 8mm thickness of copper indium or copper gallium alloy layer, cooling fluid passed in stainless steel cylindrical base member makes it be cooled to room temperature simultaneously, recording the temperature flowing out cooling fluid is between 120-160 DEG C, must comprise the stainless steel cylindrical base member of copper indium gallium alloy layer; Low-voltage plasma heat spraying method processing parameter is same step (4);
(7) will the stainless steel cylindrical base member cool to room temperature of copper indium gallium alloy be deposited, and mechanical workout be carried out to target and makes it meet dimension precision requirement and surfaceness, to obtain final product.
Embodiment 5
Detect the copper indium gallium rotary target material that embodiment 1 to 4 is obtained.
The measurement of target adopts X-ray scanners, electronic scanning Electronic Speculum, penetron, porosity measurement instrument, ICP mass-spectrometer measurement instrument, supersonic reflectoscope etc.That measures the results are shown in Table 1.
Table 1 is the copper indium gallium rotary target material parameter that embodiment 1 to 4 obtains
Claims (3)
1., for a copper indium gallium rotary target material preparation method for thin-film solar cells, it is characterized in that: comprise the following steps:
(1), in vacuum or shielding gas, adopt the stainless steel cylindrical base member surface spraying alumel layer that low-voltage plasma heat spraying method will be clean, cool simultaneously, the stainless steel cylindrical base member of alumel layer must be comprised; The thickness of alumel layer is 50-200nm; Described stainless steel cylindrical base member is the stainless steel cylindrical base member through preheating, and preheating temperature is 60-120 DEG C;
(2), in vacuum or shielding gas, adopt low-voltage plasma heat spraying method to comprise stainless steel cylindrical base member surface spraying copper indium or the copper gallium alloy layer of alumel layer, cool simultaneously, the stainless steel cylindrical base member of copper indium or copper gallium alloy layer must be comprised; The thickness of copper indium or copper gallium alloy layer is 50-100nm;
(3), in vacuum or shielding gas, adopt low-voltage plasma heat spraying method to comprise the stainless steel cylindrical base member surface spraying copper indium gallium alloy layer of copper indium or copper gallium alloy layer, cool simultaneously, to obtain final product; The thickness of copper indium gallium alloy layer is 3-20mm; The particle diameter of described copper indium gallium alloy powder is 2200-2600 order, and in copper indium gallium alloy, the mol ratio of copper, indium, gallium is 1:(0.7-0.5): (0.3-0.5).
2. a kind of copper indium gallium rotary target material preparation method for thin-film solar cells according to claim 1, is characterized in that: stainless steel cylindrical base member top is provided with water inlet and water outlet; Method of cooling is: cooling fluid passed in stainless steel cylindrical base member.
3. a kind of copper indium gallium rotary target material preparation method for thin-film solar cells according to claim 1, it is characterized in that: in step (1), the cleaning method of described stainless steel cylindrical base member is: cleaned through suds cleaning, ultrasonic cleaning, deionized water successively on the surface of stainless steel cylinder base material.
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| EP3456857A4 (en) * | 2017-08-04 | 2019-03-27 | Miasolé Equipment Integration (Fujian) Co., Ltd. | Method for preparing target material and target material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104451563B (en) * | 2013-09-12 | 2017-02-01 | 汉能新材料科技有限公司 | Copper indium gallium selenium target material preparation and application method |
| CN104818465B (en) * | 2015-04-17 | 2017-06-20 | 无锡舒玛天科新能源技术有限公司 | Copper and indium gallium rotary target material and the method that copper and indium gallium rotary target material is prepared using controlled atmosphere cold spraying |
| CN108907512B (en) * | 2018-08-30 | 2020-08-14 | 河南理工大学 | Preparation and use method of gallium-based brazing filler metal for silicon carbide particle reinforced aluminum-based composite material |
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| CN102286717A (en) * | 2011-09-01 | 2011-12-21 | 基迈克材料科技（苏州）有限公司 | Cylindrical large-area film coating target prepared through plasma spray coating and method |
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