CN101667610B - Preparation method of critical material for absorbing layer of thin film solar cell - Google Patents
Preparation method of critical material for absorbing layer of thin film solar cell Download PDFInfo
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- CN101667610B CN101667610B CN2009103067977A CN200910306797A CN101667610B CN 101667610 B CN101667610 B CN 101667610B CN 2009103067977 A CN2009103067977 A CN 2009103067977A CN 200910306797 A CN200910306797 A CN 200910306797A CN 101667610 B CN101667610 B CN 101667610B
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Abstract
The invention relates to a preparation method of critical material for an absorbing layer of a thin film solar cell. The critical material is CuM(1-2x)R2(1+x), wherein M is selected from one of Al and In, or selected from two of Al, In and Ga, R is selected from S or Se, and the value of x is -0.2 to 0.1; the state of material is powder or block target material. The preparation method of the materials is as follows: synthesizing the blocks of the materials in a vacuum closed container or in a closed container charged with argon, nitrogen or helium gas having the pressure lower than atmosphere pressure; crushing the blocks to obtain the required powder; and finally synthesizing the required block target material in a hot-pressing furnace. The method is a pure element method liquid phase synthesis technique, has wide applicability, accurate proportioning, low cost, high quality of prepared target materials, compactness of powder material reaching more than 99.9%, and compactness of block target material reaching more than 98.9%.
Description
Technical field
The present invention relates to a kind of preparation method of critical material for absorbing layer of thin film solar cell, particularly absorbing layer of thin film solar cell is with following sulfide or selenides: CuAl
(1-2x)S
2(1+x), CuAl
(1-2x)Se
2(1+x), CuIn
(1-2x)S
2(1+x), CuIn
(1-2x)Se
2(1+x), Cu (InGa)
(1-2x)Se
2(1+x), Cu (InGa)
(1-2x)S
2(1+x), Cu (AlGa)
(1-2x)S
2(1+x), Cu (AlGa)
(1-2x)Se
2(1+x), Cu (InAl)
(1-2x)S
2(1+x)And Cu (InAl)
(1-2x)Se
2(1+x)The preparation method, the value of x is-0.2～0.1, the materials behavior of preparation is powder or block target.
Background technology
CuAlS
2, CuAlSe
2, CuInS
2, CuInSe
2, Cu (InGa) Se
2, Cu (InGa) S
2, Cu (AlGa) S
2, Cu (AlGa) Se
2, Cu (InAl) S
2, Cu (InAl) Se
2Deng being the thin-film solar cells light absorption layer material, it is strong to have capability of resistance to radiation, advantages such as stable work in work, the present mature methods of its preparation method generally adopts selenizing after the first sputter (or sulfuration) technology, this method can not guarantee the uniformity of thin film composition and thickness, and selenizing technology relates to hypertoxic selenides (or sulfide), and is higher to equipment requirements in preparation process, needs the development that more economical technology advances thin-film solar cells badly.
In order to simplify technology, American scholar is utilized the CuInGaSe target, method by a step sputter has prepared CIGS light absorbing zone (C.Suryanarayanaa, E.Ivanovb, R.Nou, M.A.Contrerasc, J.J.Moore Synthesis and processing of a Cu-In-Ga-Se sputtering target, Thin Solid Films, 1998 v332. 340-344), this technology has been simplified preparation flow greatly, can accurately control thin film composition and thickness, makes selenizing work simplification even cancellation.Become the critical material of hull cell preparation for the corresponding target of this arts demand.
CuAlS
2, CuAlSe
2, CuInS
2, CuInSe
2, Cu (InGa) Se
2, Cu (InGa) S
2, Cu (AlGa) S
2, Cu (AlGa) Se
2, Cu (InAl) S
2, Cu (InAl) Se
2As light absorbing zone, have the characteristics of radioresistance, stable performance, can be prepared into non-maintaining solar film battery, be fit to civilianly, therefore exploitation solar cell more at a low price has great economic implications.The Japan scholar utilizes the circuit printing technology with CuInSe
2Powder is printed on and makes thin-film solar cells (T.Arita, N.Suyama, Y. Kita, S. Kitamura, T.Hibino, H.Takada, K.Omura, N.Ueno, and M.Murozono CuInSe on the various carriers
2Films Prepared by Screen-Printing and Sintering Method, 20th IEEE Photovoltaic Specialists Conference, 1,988 1650), therefore, high-quality CuAlS
2, CuAlSe
2, CuInS
2, CuInSe
2, Cu (InGa) Se
2, Cu (InGa) S
2, Cu (AlGa) S
2, Cu (AlGa) Se
2, Cu (InAl) S
2, Cu (InAl) Se
2Powder is the critical material of this kind of preparation battery equally.
Present CuAlS
2, CuAlSe
2, CuInS
2, CuInSe
2, Cu (InGa) Se
2, Cu (InGa) S
2, Cu (AlGa) S
2, Cu (AlGa) Se
2, Cu (InAl) S
2, Cu (InAl) Se
2Material all adopts compound to synthesize method, promptly adopts Cu
2Se compound and In
2Se
3Compound solid phase synthesis CuInSe
2Material, the material of solid phase synthesis is because intergranular contact area is less, diffusion coefficient when each element solid-state diffusion coefficient is far smaller than liquid phase, cause the component difference between the material granule (crystal grain) of solid phase synthesis process preparation bigger, cause the concentration of element skewness, film quality is low when sputter, can't satisfy the actual fabrication needs to the absorbing layer of thin film solar cell of composition proportion sensitivity.
Summary of the invention
The technical problem to be solved in the present invention is: the preparation method that a kind of critical material for absorbing layer of thin film solar cell is provided, this method is a kind of pure element method liquid phase synthesis process, it is wide to have applicability, proportion speed, cost is low, the target quality height of preparation, the density of dusty material reaches more than 99.9%, and block target density reaches the advantage more than 98.9%.
The technical scheme that solves its above-mentioned technical problem is: a kind of preparation method of critical material for absorbing layer of thin film solar cell, described critical material is CuM
(1-2x)R
2(1+x), wherein M for or be selected from a kind of element among Al, the In, or be selected from two kinds of elements among Al, In, the Ga, R is selected from a kind of element among S or the Se, the value of x is-0.2～0.1, the preparation of above-mentioned material may further comprise the steps:
A. required element material is put into container after by material composition requirement proportioning, be lower than 10
-2Under the Pa vacuum degree condition closed container or under the condition that charges into the argon gas, nitrogen or the helium that are lower than atmospheric pressure closed container;
B. airtight vessel temp is adjusted under the condition that is higher than material melting point and be incubated 0.1 hour～10 hours, make its slow cool to room temperature in 8 hours, the block for preparing is taken out the back ball milling in container,, obtain powder-product powder sieving; The described condition that is higher than material melting point is meant 1000 ℃～1200 ℃ of temperature;
C. the powder of preparing is put into hot pressing furnace mould on demand dimensioned after 600 ℃～920 ℃, 30MPa～300MPa compacting and promptly obtained required block target.
Further technical scheme of the present invention is: when needed product is powder, and can cancellation step C.
Even in order to satisfy the thin-film solar cells industry to composition, the requirement of the solar battery obsorbing layer of proportion speed, the preparation method of the present invention's critical material for absorbing layer of thin film solar cell, what adopt is a kind of pure element method liquid phase synthesis process, it is even to be used for prepared composition, proportion speed, the solar battery obsorbing layer material that purity is high, beneficial effect of the present invention is as follows:
1, applicability is wide: the CuAl that can prepare the heterogeneity proportioning
(1-2x)S
2(1+x), CuAl
(1-2x)Se
2(1+x), CuIn
(1-2x)S
2(1+x), CuIn
(1-2x)Se
2(1+x), Cu (InGa)
(1-2x)Se
2(1+x), Cu (InGa)
(1-2x)S
2(1+x), Cu (AlGa)
(1-2x)S
2(1+x), Cu (AlGa)
(1-2x)Se
2(1+x), Cu (InAl)
(1-2x)S
2(1+x)And Cu (InAl)
(1-2x)Se
2(1+x)The preparation method, the value of x is-0.2～0.1; The material property of preparing is stable, and the materials behavior of preparation is powder or block target, and powder can be used for coating, and the block target can be used for sputter coating.
2, proportion speed: the material of acquisition is difficult for introducing impurity, composition is even, element ratio is easy to control, proportion speed.
3, cost is low: this technology can prepare large-area target, and can make in batches.
4, target quality height: owing to adopt vacuum tightness synthetic, hot pressed sintering, the target even compact that obtains, the density of dusty material reaches more than 99.9%, and block target density reaches more than 98.9%, the film even film layer that obtains, smooth, strong adhesion.
Below, the technical characterictic to the preparation method of the present invention's critical material for absorbing layer of thin film solar cell is further described in conjunction with the accompanying drawings and embodiments.
[description of drawings]
Fig. 1: preparation method's flow chart of the present invention's critical material for absorbing layer of thin film solar cell.
[embodiment]
Embodiment 1
With Cu powder, In piece, the Se piece of purity 99.98%, behind the Cu:In:Se=l:1:2 proportioning 500g, put into the autoclave of liner aluminium oxide ceramics, in molar ratio 7 * 10
-3Seal autoclave under the Pa vacuum degree condition.
With the insulation 2 hours down of the temperature conditions of the adjustment to 1050 of autoclave ℃, make its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in autoclave, powder sieving is become-400 purpose grades, obtain CuInSe
2Powder, powder purity is greater than 99.9%.
The powder of preparing is put into diameter 76mm mould at the target that is processed into diameter 70mm under 850 ℃, 150MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 99.1%.
Embodiment 2
With Cu powder, In piece, the S piece of purity 99.995%, behind the Cu:In:S=l:1:2 proportioning 400g, put into the retort of liner zirconia ceramics, in molar ratio 8 * 10
-3Seal retort under the Pa vacuum degree condition.
The temperature conditions that the retort of sealing under the vacuum is adjusted to 1010 ℃ descends insulation 8 hours, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in retort, powder sieving is become-200 purpose grades, obtain CuInS
2Powder, powder purity is greater than 99.99%.
The powder of preparing is put into diameter 70mm mould at the target that is processed into diameter 60mm under 860 ℃, 110MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 99.2%.
Embodiment 3
With Cu powder, Al powder, the Se piece of purity 99.98%, behind the Cu:Al:Se=l:1:2 proportioning 700g, put into the reactor of liner aluminium oxide ceramics in molar ratio, charge into the argon gas capping still that is lower than atmospheric pressure.
The temperature conditions that the reactor that charges into argon gas is adjusted to 1100 ℃ descends insulation 2.5 hours, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in reactor, powder sieving is become-300 purpose grades, obtain CuAlSe
2Powder, powder purity is greater than 99.9%.
The powder of preparing is put into diameter 320mm mould at the target that is processed into diameter 300mm under 870 ℃, 70MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 98.9%.
Embodiment 4
With Cu powder, Al powder, the S powder of purity 99.995%, behind the Cu:Al:S=l:1:2 proportioning 500g, put into the reactor of liner aluminium oxide ceramics in molar ratio, charge into the nitrogen closing reactor that is lower than atmospheric pressure.
The temperature conditions that the reactor that charges into nitrogen is adjusted to 1080 ℃ descends insulation 4 hours, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in reactor, powder sieving is become-400 purpose grades, obtain CuAlS
2Powder, powder purity is greater than 99.99%.
The powder of preparing is put into diameter 160mm mould at the target that is processed into diameter 150mm under 900 ℃, 180MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 99.5%.
Embodiment 5
With Cu powder, In piece, Ga piece, the Se piece of purity 99.98%, behind the Cu:In:Ga:Se=l:0.7:0.3:2 proportioning 500g, put into the autoclave of liner aluminium oxide ceramics, in molar ratio 6.2 * 10
-3Seal autoclave under the Pa vacuum degree condition.
The temperature conditions that the autoclave that seals under the vacuum is adjusted to 1200 ℃ descends insulation 9 hours, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in autoclave, powder sieving is become-200 purpose grades, obtain Cu(In
0.7Ga
0.3) Se
2Powder, powder purity is greater than 99.9%.
The powder of preparing is put into diameter 120mm mould at the target that is processed into diameter 100mm under 880 ℃, 160MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 99.3%.
Embodiment 6
With Cu powder, In piece, Ga piece, the S piece of purity 99.995%, behind the Cu:In:Ga:S=l:0.8:0.2:2 proportioning 100g, put into the autoclave of liner zirconia ceramics, in molar ratio 5 * 10
-3Seal autoclave under the Pa vacuum degree condition.
The temperature conditions that the autoclave that seals under the vacuum is adjusted to 1080 ℃ descends insulation 10 hours, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in autoclave, powder sieving is become-400 purpose grades, obtain Cu(In
0.8Ga
0.2) S
2Powder, powder purity is greater than 99.99%.
The powder of preparing is put into diameter 60mm mould at the target that is processed into diameter 58mm under 900 ℃, 280MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 99.9%.
Embodiment 7
With Cu powder, Al powder, Ga piece, the S piece of purity 99.98%, behind the Cu:Al:Ga:S=l:0.8:0.2:2 proportioning 900g, put into the reactor of liner aluminium oxide ceramics, in molar ratio 4 * 10
-3Seal reactor under the Pa vacuum degree condition.
The temperature conditions that the reactor that seals under the vacuum is adjusted to 1190 ℃ descends insulation 0.1 hour, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in reactor, powder sieving is become-300 purpose grades, obtain Cu(Al
0.8Ga
0.2) S
2Powder, powder purity is greater than 99.9%.
The powder of preparing is put into diameter 160mm mould at the target that is processed into diameter 150mm under 900 ℃, 150MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 99.3%.
Embodiment 8
With Cu powder, Al powder, Ga piece, the Se piece of purity 99.98%, behind the Cu:Al:Ga:Se=l:0.7:0.3:2 proportioning 900g, put into the autoclave of liner aluminium oxide ceramics in molar ratio, charge into the argon gas sealing autoclave that is lower than atmospheric pressure.
The temperature conditions that the autoclave that charges into argon gas is adjusted to 1100 ℃ descends insulation 3 hours, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in autoclave, powder sieving is become-400 purpose grades, obtain Cu(Al
0.7Ga
0.3) Se
2Powder, powder purity is greater than 99.99%.
The powder of preparing is put into diameter 200mm mould at the target that is processed into diameter 180mm under 850 ℃, 130MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 99.3%.
Embodiment 9
With Cu piece, In piece, Al powder, the S piece of purity 99.995%, behind the Cu:In:Al:S=l:0.6:0.4:2 proportioning 80g, put into the reactor of liner aluminium oxide ceramics, in molar ratio 4 * 10
-3Seal reactor under the Pa vacuum degree condition.
The temperature conditions that the reactor that seals under the vacuum is adjusted to 1050 ℃ descends insulation 3 hours, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in reactor, powder sieving is become-300 purpose grades, obtain Cu(In
0.6Al
0.4) S
2Powder, powder purity is greater than 99.99%.
The powder of preparing is put into diameter 35mm mould at the target that is processed into diameter 30mm under 900 ℃, 300MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 99.9%.
Embodiment 10
With Cu piece, In piece, Al powder, the Se piece of purity 99.98%, behind the Cu:In:Al:Se=l:0.7:0.3:2 proportioning 1000g, put into the reactor of liner zirconia ceramics in molar ratio, charge into the nitrogen closing reactor that is lower than atmospheric pressure,
The temperature conditions that the reactor that charges into nitrogen is adjusted to 1100 ℃ descends insulation 2 hours, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in reactor, powder sieving is become-400 purpose grades, obtain Cu(In
0.7Al
0.3) Se
2Powder, powder purity is greater than 99.9%.
The powder of preparing is put into diameter 190mm mould at the target that is processed into diameter 180mm under 890 ℃, 150MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 99.2%.
Embodiment 11
With Cu piece, In piece, Ga piece, the Se piece of purity 99.98%, behind the Cu:In:Ga:Se=l:0.9:0.5:1.6 proportioning 500g, put into the pressure pan of enamel, in molar ratio 6.0 * 10
-3Seal pressure pan under the Pa vacuum degree condition;
The pressure pan that seals under the vacuum is adjusted to 1000 ℃ down insulation 0.5 hour of temperature conditions, makes its slow cool to room temperature in 8 hours, the block of preparation is taken out the back ball milling in pressure pan, powder sieving is become-200 purpose grades, obtain Cu(Al
0.9Ga
0.5) S
1.6Powder, powder purity is greater than 99.9%.
The powder of preparing is put into diameter 120mm mould at the target that is processed into diameter 100mm under 900 ℃, 40MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 98.9%.
Embodiment 12
With Cu piece, Al piece, Ga piece, the Se piece of purity 99.99%, in molar ratio behind the Cu:Al:Ga:Se=l:0.7:0.2:2.1 proportioning 300g, put into enamel autoclave, charge into the argon gas sealing autoclave that is lower than atmospheric pressure;
The autoclave that charges into argon gas is adjusted to 1100 ℃ down insulation 1 hour of temperature conditions, makes its slow cool to room temperature in 8 hours, the block of preparation is taken out the back ball milling in autoclave, powder sieving is become-400 purpose grades, obtain Cu(Al
0.7Ga
0.2) Se
2.1Powder; Powder purity is greater than 99.9%.
The powder of preparing is put into diameter 50mm mould at the target that is processed into diameter 48mm under 650 ℃, 260MPa condition after with the hot-pressed sintering furnace compacting, and the target density can reach 99.0%.
As a kind of conversion of various embodiments of the present invention, when needed product was powder, cancellation hot-pressed sintering furnace pressing step got final product.
As a kind of conversion of the embodiment of the invention 3, embodiment 4, embodiment 8, embodiment 10 and embodiment 12, the described gas that charges in the closed container can also be helium.
As a kind of conversion of various embodiments of the present invention, described hot pressing furnace can also adopt the high temperature insostatic pressing (HIP) stove.
Above-described embodiment is preferable embodiments more of the present invention, and those skilled in the art can make various modifications within the scope of the appended claims.
Claims (6)
1. the preparation method of a critical material for absorbing layer of thin film solar cell, described critical material is CuM
(1-2x)R
2(1+x), wherein M for or be selected from a kind of element among Al, the In, or be selected from two kinds of elements among Al, In, the Ga, R is selected from a kind of element among S or the Se, the value of x is-0.2～0.1, it is characterized in that: the preparation of above-mentioned material may further comprise the steps:
A. required element material is put into container after by material composition requirement proportioning, be lower than 10
-2Under the Pa vacuum degree condition closed container or under the condition that charges into the argon gas, nitrogen or the helium that are lower than atmospheric pressure closed container;
B. airtight vessel temp is adjusted under the condition that is higher than material melting point and be incubated 0.1 hour～10 hours, make its slow cool to room temperature in 8 hours, the block for preparing is taken out the back ball milling in container,, obtain powder-product powder sieving; The described condition that is higher than material melting point is meant 1000 ℃～1200 ℃ of temperature;
C. the powder of preparing is put into hot pressing furnace mould on demand dimensioned after 600 ℃～920 ℃, 30MPa～300MPa compacting and promptly obtained required block target.
2. the preparation method of critical material for absorbing layer of thin film solar cell according to claim 1, it is characterized in that: required element material Cu, M described in the steps A and the mol ratio of R are: Cu: M: R=1: 1(1-2x): 2(1+x), the value of x is-0.2～0.1.
3. the preparation method of critical material for absorbing layer of thin film solar cell according to claim 2, it is characterized in that: described M is two kinds of elements that are selected among Al, In, the Ga, and the value of x is-0.05～0.05.
4. according to the preparation method of claim 1,2 or 3 described critical material for absorbing layer of thin film solar cell, it is characterized in that: when needed product is powder, cancellation step C.
5. according to the preparation method of claim 1,2 or 3 described critical material for absorbing layer of thin film solar cell, it is characterized in that: the container described in the steps A is autoclave, pressure pan, reactor or the retort of liner aluminium oxide ceramics, zirconia ceramics or enamel.
6. according to the preparation method of claim 1,2 or 3 described critical material for absorbing layer of thin film solar cell, it is characterized in that: the hot pressing furnace described in the step C is high temperature insostatic pressing (HIP) stove or hot-pressed sintering furnace.
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| KR101293330B1 (en) | 2010-09-27 | 2013-08-06 | 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 | Cu-in-ga-se quaternary alloy sputtering target |
| CN103255367B (en) * | 2013-04-28 | 2015-07-29 | 柳州百韧特先进材料有限公司 | The preparation method of solar cell CIGS absorption layer target material |
| CN103236472B (en) * | 2013-04-28 | 2015-09-30 | 柳州百韧特先进材料有限公司 | The preparation method of CIGS thin film solar cell selenides |
| CN104143579A (en) * | 2013-05-07 | 2014-11-12 | 华中科技大学 | Antimony-base compound thin film solar cell and manufacturing method thereof |
| CN103633165B (en) * | 2013-11-27 | 2016-02-10 | 中国科学院上海硅酸盐研究所 | Yellow copper structure Intermediate Gray solar battery obsorbing layer material and preparation method thereof |
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| CN1885566A (en) * | 2006-05-26 | 2006-12-27 | 华东师范大学 | Compound semiconductor layer making method and solar battery using the semiconductor layer and its making method |
| CN101307397A (en) * | 2008-04-15 | 2008-11-19 | 成都先锋材料有限公司 | Vacuum smelting method and apparatus for copper-indium-gallium-selenium photovoltaic material |
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| CN1885566A (en) * | 2006-05-26 | 2006-12-27 | 华东师范大学 | Compound semiconductor layer making method and solar battery using the semiconductor layer and its making method |
| CN101307397A (en) * | 2008-04-15 | 2008-11-19 | 成都先锋材料有限公司 | Vacuum smelting method and apparatus for copper-indium-gallium-selenium photovoltaic material |
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