CN103290372A - Method for preparing copper indium gallium rotary target material for thin-film solar cells - Google Patents
Method for preparing copper indium gallium rotary target material for thin-film solar cells Download PDFInfo
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- CN103290372A CN103290372A CN2013101724896A CN201310172489A CN103290372A CN 103290372 A CN103290372 A CN 103290372A CN 2013101724896 A CN2013101724896 A CN 2013101724896A CN 201310172489 A CN201310172489 A CN 201310172489A CN 103290372 A CN103290372 A CN 103290372A
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- copper indium
- stainless steel
- copper
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- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 title claims abstract description 98
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 37
- 239000013077 target material Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000010409 thin film Substances 0.000 title claims description 17
- 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
- CDZGJSREWGPJMG-UHFFFAOYSA-N copper gallium Chemical compound [Cu].[Ga] CDZGJSREWGPJMG-UHFFFAOYSA-N 0.000 claims abstract description 32
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000005507 spraying Methods 0.000 claims description 63
- 238000002360 preparation method Methods 0.000 claims description 34
- 238000004140 cleaning Methods 0.000 claims description 23
- 239000012809 cooling fluid Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 16
- 229910001120 nichrome Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910000809 Alumel Inorganic materials 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 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
- 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
- 239000012467 final product Substances 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 abstract description 21
- 239000013078 crystal Substances 0.000 abstract description 3
- 229910000838 Al alloy Inorganic materials 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 238000007751 thermal spraying Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 29
- 238000012545 processing Methods 0.000 description 13
- 239000011159 matrix material Substances 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000000956 alloy Substances 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 230000005611 electricity Effects 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
- 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
- 238000002844 melting Methods 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
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000000203 mixture Substances 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
- 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 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
- 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
- 230000008018 melting Effects 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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000003825 pressing 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
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
The invention provides a method for preparing a copper indium gallium rotary target material. The method for preparing the copper indium gallium rotary target material comprises the following steps of: preparing a stainless steel cylinder base body comprising a nickel aluminum or nicochrome layer; preparing a stainless steel cylinder base body comprising a copper indium or copper gallium alloy layer; preparing a stainless steel cylinder base body comprising a copper indium or copper gallium alloy layer. According to the method, a nickel aluminum alloy, a copper indium or copper gallium alloy and copper indium gallium are sequentially cured on the stainless steel cylinder base bodies layer by layer by adopting a low-pressure plasma thermal spraying method so as to form the copper indium gallium rotary target material; defects of a binding working procedure in the prior art are overcome; the technology is simple; the operation is convenient; the cost is low; the produced target material is high in density, low in porosity, uniform in component, fine in crystal particle, high in yield and good in quality.
Description
Technical field
The invention belongs to the 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 enlarges rapidly.2011, the rate of increase of U.S.'s solar energy industry is up to 109%, and was leading in technical field of new energies.Copper-indium-galliun-selenium film solar cell in solar panel field development rapidly, it is provided with molybdenum layer, CIGS thin-film absorption layer, Cadmium Sulfide buffer layer, intrinsic zinc oxide, aluminium-zinc oxide Window layer and surperficial contact layer usually successively on the glass film plates of one deck rigidity or flexible stainless steel plate.According to the research report of LuxResearch, CIGS thin-film solar market production capacity reached 1.2GW in 2011, and will reach 2.3GW in 2015; Other solar cell research institutions all predict copper-indium-galliun-selenium film solar cell the market share will by 2010 3% rise to 2015 6%, and will reach 33% at the year two thousand twenty.This shows that fully the copper-indium-galliun-selenium film solar cell technology will lead following solar cell market, and has huge business potential.As being classified as the most promising thin film solar cell technologies by the well-known solar cell of USDOE and other research institution, the copper-indium-galliun-selenium film solar cell technology just by feat of its widely advantage attracting increasing researchist and investor.Up to now, the efficient of copper-indium-galliun-selenium film solar cell has broken through 20.3% in the laboratory.Simultaneously, increasing company, mechanism are being devoted to realize the commercialization of this technology.
Sputter-deposition technology is widely used in aspects such as solar cell, flat-panel screens, CD, microstructure circuit; Particularly, along with the emergence of in recent years copper indium gallium selenium solar hull cell, sputtering technology has been made huge contribution for 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 targets is arisen at the historic moment, as: high-temperature vacuum hot pressing sintering method, isostatic cool pressing method, hot isostatic pressing method, vacuum melting method.Yet existing method all needs follow-up binding technology, and binding technology itself is the process of a complexity, and the bound device costliness.In order to make the target that makes that thermal diffusivity, electroconductibility preferably and work-ing life and the service efficiency that improves target be arranged, yet existing method all needs follow-up target binding technology, being about to target is tied to by brazing mode with backboard (normally metal copper plate), binding technology itself is the process of a complexity, and the bound device costliness; Simultaneously, in case the binding weak effect can make the rapid intensification of target so and cause problems such as target sealing-off, target fusing, apparatus overheat, sputtering equipment can be out of order or scrap when serious.
Hot-spraying techniques is to utilize certain thermal source, as electric arc, plasma arc, combustion flame etc. dusty material is heated to fusion or semi-melting state, make fusion or the atomizing of semi-melting powdered material by the power of flame stream itself or the high velocity air that adds then, and be ejected into through pretreated substrate material surface a kind of technology of being combined with body material with certain speed.The low-voltage plasma heat spraying method is a kind of of hot-spraying techniques, utilize this method to prepare many novel materials, new unit, and be applied to as light, magnetic recording, flat-panel screens, solar energy materials, high-technology fields such as high temperature resistant, wear-resisting aerospace, rocket engine are present one of energy-conservation and effective technologies of economizing on resources.
Summary of the invention
Goal of the invention: the purpose of this invention is to provide a kind of technology copper indium gallium rotary target material preparation method who is used for thin-film solar cells simple, with low cost.
Technical scheme: the preparation method of a kind of copper indium gallium rotary target material provided by the invention may further comprise the steps:
(1) in vacuum or the shielding gas, adopts the low-voltage plasma heat spraying method with the stainless steel cylindrical base member surface spraying alumel layer of cleaning, cool off, must comprise the stainless steel cylindrical base member of nickel aluminium or nichrome layer;
(2) in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will comprise stainless steel cylindrical base member surface spraying copper indium or the copper gallium alloy layer of nickel aluminium or nichrome layer, cool off, must comprise the stainless steel cylindrical base member of copper indium or copper gallium alloy layer;
(3) in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will comprise the stainless steel cylindrical base member surface spraying copper indium gallium alloy layer of copper indium or copper gallium alloy layer, cool off simultaneously, namely.
Wherein, stainless steel cylindrical base member top is provided with water inlet and water outlet; Method of cooling is: cooling fluid is fed in the stainless steel cylindrical base member get final product.Make stainless steel cylindrical base member outside wall temperature be lower than the solidification value of alloy after the cooling, thereby make the alloy fast deposition of molten state arrive the outside surface of cylinder and curing rapidly.
Wherein, in the step (1), described stainless steel cylindrical base member is the stainless steel cylindrical base member through preheating, and preheating temperature is 60-120 ℃.Preheating procedure can be eliminated moisture and the moisture on stainless steel cylindrical base member surface, thus the interface temperature the when alloy particle that improves spraying contacts with the stainless steel cylindrical base member, with raising coating and high base strength; Can reduce simultaneously the alloy layer that stress that the thermal dilation difference because of base material and coated material causes causes ftractures; Preheating temperature depends on size, shape and the material of stainless steel cylindrical base member, and factors such as stainless steel cylindrical base member and coating alloy material coefficient of thermal expansion coefficient.
Wherein, in the step (1), the cleaning method of described stainless steel cylindrical base member is: the surface of stainless steel cylinder base material is cleaned and got final product through suds cleaning, ultrasonic cleaning, deionized water successively.
Wherein, in the step (1), the thickness of alumel layer is 50-200nm.
Wherein, in the step (2), the thickness of copper indium or copper gallium alloy layer is 50-100nm.
Wherein, in the step (3), the thickness of copper indium gallium alloy layer is 3-20mm.
Wherein, in the step (3), the particle diameter of described copper indium gallium alloy powder is the 2200-2600 order, is preferably 2400 orders, and the mol ratio of copper, indium, gallium is 1:(0.7-0.5 in the copper indium gallium alloy): (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 the 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 the stainless steel cylindrical base member, overcome the defective of the binding operation in the existing method, technology is simple, easy to operate, with low cost, and the target density height of producing, porosity is low, composition is even, crystal grain is tiny, productive rate is high, quality is good.
Particularly, the present invention has following outstanding advantage with respect to prior art:
(1) technology is simple, productive rate is high, with low cost: this method does not need follow-up binding operation, and technology 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 the low-voltage plasma heat spraying method, and wherein plasma jet can arrive that 2000m/s, velocity of particle can reach 300m/s, substrate temperature can reach 650 ℃, and coating stress is less, thickness is high, compact structure; Simultaneously, under the low pressure flame passes chap elongated, powder is heated evenly, the low-voltage plasma heat spraying method can adopt transferred arc electricity cleaning matrix surface, improves the matrix surface activity, has improved the bonding force of coating and matrix; The present invention make copper indium gallium rotary target material have density height (＞95%), porosity low (＜0.5%), composition is even, crystal grain is tiny characteristics such as (particle diameter are less than 100 μ m), do not have defectives such as isolating of macroscopic view;
(3) constant product quality: this method employing vacuum or shielding gas atmosphere such as argon gas or nitrogen can effectively be avoided the metal or metal alloy oxidation, thereby effectively avoid oxidized metal or alloy can destroy the joint tightness degree of each alloy layer, the performance of reduction target.
Description of drawings
Fig. 1 is used for the copper indium gallium rotary target material preparation technology schema of thin-film solar cells for the present invention.
Embodiment
According to following embodiment, the present invention may be better understood.Yet, those skilled in the art will readily understand that the described concrete material proportion of embodiment, processing condition and result thereof only are used for explanation the present invention, and should also can not limit the present invention described in detail in claims.
Embodiment 1
The preparation method of copper indium gallium rotary target material sees Fig. 1, may further comprise the 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 with the mol ratio of copper, indium, gallium, and after grinding with planetary ball mill, sieve that getting particle diameter is 2400 purpose copper indium gallium alloy powder;
(2) cleaning surfaces 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: the stainless steel cylindrical base member is preheated to 90 ℃;
(4) comprise the preparation of the stainless steel cylindrical base member of nickel aluminium or nichrome layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method with the alumel layer of the stainless steel cylindrical base member surface spraying 125nm thickness of cleaning, simultaneously cooling fluid being fed in the stainless steel cylindrical base member makes it be cooled to room temperature, recording the temperature that flows out cooling fluid is between 120-160 ℃, must comprise the stainless steel cylindrical base member of nickel aluminium or nichrome layer; Particularly, the basic craft course of low-voltage plasma heat spraying method comprises: reaction system is vacuumized and charges into shielding gas, the surperficial preheating of the steel cylindrical base member that will become rusty also utilizes the cleaning of surperficial transferred arc electricity, spraying and cooling; Wherein, low-voltage plasma heat spraying method processing parameter is: argon gas (rise/minute) 10-30; Powder feeding gas (rise/minute) 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 when transferred arc is handled; For further protection matrix, avoid matrix oxidized, can also feed hydrogen (rise/minute): 0.5-1.5;
(5) comprise the preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will comprise copper indium or the copper gallium alloy layer of the stainless steel cylindrical base member surface spraying 75nm thickness of nickel aluminium or nichrome layer, simultaneously cooling fluid being fed in the stainless steel cylindrical base member makes it be cooled to room temperature, recording the temperature that flows out cooling fluid is between 120-160 ℃, the stainless steel cylindrical base member that must comprise copper indium or copper gallium alloy layer, low-voltage plasma heat spraying method processing parameter are same step (4);
(6) comprise the preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will 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, simultaneously cooling fluid being fed in the stainless steel cylindrical base member makes it be cooled to room temperature, recording the temperature that flows out cooling fluid is between 120-160 ℃, 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 deposit the stainless steel cylindrical base member cool to room temperature of copper indium gallium alloy, and target be carried out mechanical workout make it meet dimension precision requirement and surfaceness, namely.
Embodiment 2
The preparation method of copper indium gallium rotary target material sees Fig. 1, may further comprise the 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 with the mol ratio of copper, indium, gallium, and after grinding with planetary ball mill, sieve that getting particle diameter is 2600 purpose copper indium gallium alloy powder;
(2) cleaning surfaces 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: the stainless steel cylindrical base member is preheated to 120 ℃;
(4) comprise the preparation of the stainless steel cylindrical base member of nickel aluminium or nichrome layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method with the alumel layer of the stainless steel cylindrical base member surface spraying 50nm thickness of cleaning, be cooled to room temperature, must comprise the stainless steel cylindrical base member of nickel aluminium or nichrome layer; Particularly, the basic craft course of low-voltage plasma heat spraying method comprises: reaction system is vacuumized and charges into shielding gas, the surperficial preheating of the steel cylindrical base member that will become rusty also utilizes the cleaning of surperficial transferred arc electricity, spraying and cooling; Wherein, low-voltage plasma heat spraying method processing parameter is: argon gas (rise/minute) 10-30; Powder feeding gas (rise/minute) 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 when transferred arc is handled; For further protection matrix, avoid matrix oxidized, can also feed hydrogen (rise/minute): 0.5-1.5;
(5) comprise the preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will comprise copper indium or the copper gallium alloy layer of the stainless steel cylindrical base member surface spraying 50nm thickness of nickel aluminium or nichrome layer, simultaneously cooling fluid being fed in the stainless steel cylindrical base member makes it be cooled to room temperature, recording the temperature that flows out cooling fluid is between 120-160 ℃, the stainless steel cylindrical base member that must comprise copper indium or copper gallium alloy layer, low-voltage plasma heat spraying method processing parameter are same step (4);
(6) comprise the preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will 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, simultaneously cooling fluid being fed in the stainless steel cylindrical base member makes it be cooled to room temperature, recording the temperature that flows out cooling fluid is between 120-160 ℃, 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 deposit the stainless steel cylindrical base member cool to room temperature of copper indium gallium alloy, and target be carried out mechanical workout make it meet dimension precision requirement and surfaceness, namely.
Embodiment 3
The preparation method of copper indium gallium rotary target material sees Fig. 1, may further comprise the 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 with the mol ratio of copper, indium, gallium, and after grinding with planetary ball mill, sieve that getting particle diameter is 2200 purpose copper indium gallium alloy powder;
(2) cleaning surfaces 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: the stainless steel cylindrical base member is preheated to 60 ℃;
(4) comprise the preparation of the stainless steel cylindrical base member of nickel aluminium or nichrome layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method with the alumel layer of the stainless steel cylindrical base member surface spraying 200nm thickness of cleaning, be cooled to room temperature, must comprise the stainless steel cylindrical base member of nickel aluminium or nichrome layer; Particularly, the basic craft course of low-voltage plasma heat spraying method comprises: reaction system is vacuumized and charges into shielding gas, the surperficial preheating of the steel cylindrical base member that will become rusty also utilizes the cleaning of surperficial transferred arc electricity, spraying and cooling; Wherein, low-voltage plasma heat spraying method processing parameter is: argon gas (rise/minute) 10-30; Powder feeding gas (rise/minute) 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 when transferred arc is handled; For further protection matrix, avoid matrix oxidized, can also feed hydrogen (rise/minute): 0.5-1.5;
(5) comprise the preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will comprise copper indium or the copper gallium alloy layer of the stainless steel cylindrical base member surface spraying 100nm thickness of nickel aluminium or nichrome layer, simultaneously cooling fluid being fed in the stainless steel cylindrical base member makes it be cooled to room temperature, recording the temperature that flows out cooling fluid is between 120-160 ℃, the stainless steel cylindrical base member that must comprise copper indium or copper gallium alloy layer, low-voltage plasma heat spraying method processing parameter are same step (4);
(6) comprise the preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will 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, simultaneously cooling fluid being fed in the stainless steel cylindrical base member makes it be cooled to room temperature, recording the temperature that flows out cooling fluid is between 120-160 ℃, 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 deposit the stainless steel cylindrical base member cool to room temperature of copper indium gallium alloy, and target be carried out mechanical workout make it meet dimension precision requirement and surfaceness, namely.
Embodiment 4
The preparation method of copper indium gallium rotary target material sees Fig. 1, may further comprise the 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 with the mol ratio of copper, indium, gallium, and after grinding with planetary ball mill, sieve that getting particle diameter is 2500 purpose copper indium gallium alloy powder;
(2) cleaning surfaces 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: the stainless steel cylindrical base member is preheated to 80 ℃;
(4) comprise the preparation of the stainless steel cylindrical base member of nickel aluminium or nichrome layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method with the alumel layer of the stainless steel cylindrical base member surface spraying 150nm thickness of cleaning, be cooled to room temperature, must comprise the stainless steel cylindrical base member of nickel aluminium or nichrome layer; Particularly, the basic craft course of low-voltage plasma heat spraying method comprises: reaction system is vacuumized and charges into shielding gas, the surperficial preheating of the steel cylindrical base member that will become rusty also utilizes the cleaning of surperficial transferred arc electricity, spraying and cooling; Wherein, low-voltage plasma heat spraying method processing parameter is: argon gas (rise/minute) 10-30; Powder feeding gas (rise/minute) 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 when transferred arc is handled; For further protection matrix, avoid matrix oxidized, can also feed hydrogen (rise/minute): 0.5-1.5;
(5) comprise the preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will comprise copper indium or the copper gallium alloy layer of the stainless steel cylindrical base member surface spraying 60nm thickness of nickel aluminium or nichrome layer, simultaneously cooling fluid being fed in the stainless steel cylindrical base member makes it be cooled to room temperature, recording the temperature that flows out cooling fluid is between 120-160 ℃, the stainless steel cylindrical base member that must comprise copper indium or copper gallium alloy layer, low-voltage plasma heat spraying method processing parameter are same step (4);
(6) comprise the preparation of the stainless steel cylindrical base member of copper indium or copper gallium alloy layer: in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will 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, simultaneously cooling fluid being fed in the stainless steel cylindrical base member makes it be cooled to room temperature, recording the temperature that flows out cooling fluid is between 120-160 ℃, 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 deposit the stainless steel cylindrical base member cool to room temperature of copper indium gallium alloy, and target be carried out mechanical workout make it meet dimension precision requirement and surfaceness, namely.
Embodiment 5
Detect the copper indium gallium rotary target material that embodiment 1 to 4 makes.
X-ray scanning instrument, electronic scanning Electronic Speculum, penetron, porosity measurement instrument, ICP mass-spectrometer measurement instrument, supersonic reflectoscope etc. are adopted in the measurement of target.That measures the results are shown in Table 1.
The copper indium gallium rotary target material parameter that table 1 makes for embodiment 1 to 4
Claims (8)
1. copper indium gallium rotary target material preparation method who is used for thin-film solar cells is characterized in that: may further comprise the steps:
(1) in vacuum or the shielding gas, adopts the low-voltage plasma heat spraying method with the stainless steel cylindrical base member surface spraying alumel layer of cleaning, cool off simultaneously, must comprise the stainless steel cylindrical base member of nickel aluminium or nichrome layer;
(2) in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will comprise stainless steel cylindrical base member surface spraying copper indium or the copper gallium alloy layer of nickel aluminium or nichrome layer, cool off simultaneously, must comprise the stainless steel cylindrical base member of copper indium or copper gallium alloy layer;
(3) in vacuum or the shielding gas, adopt the low-voltage plasma heat spraying method will comprise the stainless steel cylindrical base member surface spraying copper indium gallium alloy layer of copper indium or copper gallium alloy layer, cool off simultaneously, namely.
2. 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: stainless steel cylindrical base member top is provided with water inlet and water outlet; Method of cooling is: cooling fluid is fed in the stainless steel cylindrical base member get final product.
3. a kind of copper indium gallium rotary target material preparation method for thin-film solar cells according to claim 1 is characterized in that: in the step (1), described stainless steel cylindrical base member is the stainless steel cylindrical base member through preheating, and preheating temperature is 60-120 ℃.
4. 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 the step (1), the cleaning method of described stainless steel cylindrical base member is: the surface of stainless steel cylinder base material is cleaned and got final product through suds cleaning, ultrasonic cleaning, deionized water successively.
5. 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 the step (1), the thickness of alumel layer is 50-200nm.
6. 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 the step (2), the thickness of copper indium or copper gallium alloy layer is 50-100nm.
7. 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 the step (3), the thickness of copper indium gallium alloy layer is 3-20mm.
8. 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 the step (3), the particle diameter of described copper indium gallium alloy powder is the 2200-2600 order, be preferably 2400 orders, the mol ratio of copper, indium, gallium is 1:(0.7-0.5 in the copper indium gallium alloy): (0.3-0.5).
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| CN104451563A (en) * | 2013-09-12 | 2015-03-25 | 汉能新材料科技有限公司 | Copper indium gallium selenium target material preparation and application method |
| 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 |
| 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 |
| CN108907512A (en) * | 2018-08-30 | 2018-11-30 | 河南理工大学 | Enhancing aluminum-base composite material by silicon carbide particles gallium base solder preparation and application |
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| CN103045995A (en) * | 2012-12-19 | 2013-04-17 | 西北稀有金属材料研究院 | Rotary niobium oxide target material and preparation method thereof |
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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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451563A (en) * | 2013-09-12 | 2015-03-25 | 汉能新材料科技有限公司 | Copper indium gallium selenium target material preparation and application method |
| 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 |
| 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 |
| 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 |
| 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 |
| WO2019024421A1 (en) * | 2017-08-04 | 2019-02-07 | 米亚索乐装备集成（福建）有限公司 | Method for preparing target material and target material |
| CN108907512A (en) * | 2018-08-30 | 2018-11-30 | 河南理工大学 | Enhancing aluminum-base composite material by silicon carbide particles gallium base solder preparation and application |
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