CN202499904U - Plasma-assisted selenizing device for preparing copper-indium-gallium-selenium (CIGS) thin films - Google Patents
Plasma-assisted selenizing device for preparing copper-indium-gallium-selenium (CIGS) thin films Download PDFInfo
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- CN202499904U CN202499904U CN2012201246240U CN201220124624U CN202499904U CN 202499904 U CN202499904 U CN 202499904U CN 2012201246240 U CN2012201246240 U CN 2012201246240U CN 201220124624 U CN201220124624 U CN 201220124624U CN 202499904 U CN202499904 U CN 202499904U
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Abstract
The utility model provides a plasma-assisted selenizing device for preparing copper-indium-gallium-selenium (CIGS) thin films. The plasma-assisted selenizing device comprises an air inlet system, a thermal evaporation furnace, a plasma generator, a selenizing furnace and an air outlet system, wherein a first quartz tube is installed in a cavity of the thermal evaporation furnace; a second quartz tube is installed in a cavity of the plasma generator; a third quartz tube is installed in a cavity of the selenizing furnace; and the air inlet system, the first quartz tube, the second quartz tube, the third quartz tube and the air outlet system are communicated in order. The plasma-assisted selenizing device has the following beneficial effects: the device can accurately control the parameters of the plasma air source and selenizing respectively, realizes low-temperature growth of high-quality CIGS thin film materials, and has the advantages of simple structural design, easiness in washing, safety and good uniformity of the finally obtained CIGS thin films. Thus, the plasma-assisted selenizing device is suitable for large-scale industrial production of CIGS thin film solar cells.
Description
Technical field
The utility model belongs to the solar energy generation technology field, is specifically related to a kind of plasma body for preparing CIGS thin-film and assists the selenizing device.
Background technology
The CIGS thin-film solar cells is the yellow copper ore crystalline membrane solar cell that is made up of optimum proportion copper, indium, gallium, four kinds of elements of selenium, is the gordian technique of forming cell panel.Light absorpting ability is strong, power generation stabilization property is good, transformation efficiency is high because this product has, long, the many advantages such as generated energy is high, production cost is low and the energy recovery cycle is short of generating dutation on daytime, and the CIGS thin-film solar cells has broad application prospects.
The CIGS thin-film solar cells is to be one type of hull cell of light absorbing zone with the CIGS film.In the preparation method and device of CIGS film, mainly comprise following several types: coevaporation processing procedure, sputter process, antivacuum coating process or electroplating process.The defective of uniformity of film difference when wherein, the coevaporation processing procedure has the big area industrialization; And sputter process, antivacuum coating process or electroplating process all need pass through the selenizing processing, therefore, and these three types of defectives that device has complex structure and is difficult to large-scale industrial production.
Industry member comparatively popular is that plasma body is assisted the selenizing device, and this device can effectively improve the reactant gases activity, reduces temperature of reaction and effectively shorten reaction times, for example document Journal of Electronic materials; Vol.37 No.5; 2008,755-759 and Journal of Electrochemical Society, 150 (10); 2003; Adopt PECVD (Plasma Enhanced Chemical Vapor Deposition, plasma enhanced chemical vapor deposition method) technology all to realize the low-temperature epitaxy of high-quality ZnO and AZO film among the C693-C689, temperature is about 200 ℃.Because the fusing point of CIGS block materials is near 1000 ℃; The general best selenizing temperature of CIGS thin-film material is all more than 550 ℃; The softening temperature of the common soda-lime glass that uses as substrate material is but about 500 ℃; Thereby in the actual production on a lot of enterprises line cell panel the glass warpage all takes place, and then cause good article rate on the low side.And through adopting the PECVD technology, can effectively address the above problem.
A kind of PECVD selenizing technology and device of CIGS thin-film material are disclosed among the patent CN102051603A; But propose in this patent a kind of with precursor thin-film as heated cathode; Be equipped with the anode that can heat and contain vesicular structure simultaneously; Through applying the alternation high pressure and then producing plasma body, carry out the original position selenylation reaction that plasma body is assisted through feeding selenium steam, obtain the CIGS film.This patent selenizing apparatus structure complex design; In the original position selenizing process, best build-up of luminance air pressure and the control of selenizing air pressure are difficult to reach unanimity, and the single accurate control of sample temperature and uniformity of film also are difficult to be guaranteed; Deposit at low temperature anode and other inner selenium that produces unavoidably after the selenizing; Be difficult to disassembly, cleaning, the plasma body that alternating voltage produces also can produce damage to the CIGS film quality, thereby is difficult to be applicable to the large-scale industrial production of CIGS hull cell.
The utility model content
Defective to the prior art existence; The utility model provides a kind of plasma body for preparing CIGS thin-film to assist the selenizing device; Can distinguish the parameter of accurate control plasma body source of the gas and selenizing; Realize the low-temperature epitaxy of high quality CIGS thin-film material, also had selenizing apparatus structure simplicity of design, be prone to clean, the advantage of the good uniformity of safety and the CIGS film that finally obtains, therefore be applicable to the large-scale industrialization production of CIGS thin-film solar cells.
The technical scheme that the utility model adopts is following:
The utility model provides a kind of plasma body for preparing CIGS thin-film to assist the selenizing device, comprising: inlet system, thermal evaporation stove, plasma producing apparatus, selenizing stove and the system of giving vent to anger; The cavity of said thermal evaporation stove is equipped with first silica tube; The cavity of said plasma producing apparatus is equipped with second silica tube; The cavity of said selenizing stove is equipped with the 3rd silica tube, and said inlet system, said first silica tube, said second silica tube, said the 3rd silica tube and the said system of giving vent to anger are communicated with in order.
Preferably, said inlet system is the stainless steel inlet pipe; The said system of giving vent to anger is the stainless steel escape pipe.
Preferably, said inlet system also comprises: first valve; Said first valve is installed in the air inlet mouth of pipe place of said stainless steel inlet pipe.
Preferably, in the pipe of said first silica tube, be placed with plumbago crucible.
Preferably, between said second silica tube and said the 3rd silica tube, the heated filament pipe is installed also; The entrance end of said heated filament pipe is communicated with said second silica tube, and the exit end of said heated filament pipe is communicated with said the 3rd silica tube.
Preferably, in the joint of said second silica tube and said the 3rd silica tube second valve is installed also.
Preferably, in the pipe of said the 3rd silica tube, slot is installed.
Preferably, the exit end at said the 3rd silica tube is equipped with tensimeter.
Preferably, the exit end at said the 3rd silica tube also is communicated with cold-trap.
Preferably, said cold-trap comprises: interior pipe and outer tube; Pipe is built in the inside of said outer tube in said; Said outer tube is communicated with water-in and water outlet; The inlet pipe mouth of pipe is communicated with the exit end of said the 3rd silica tube in said, the outlet spout and the said system connectivity of giving vent to anger of said interior pipe.
The beneficial effect of the utility model is following:
The plasma body of the preparation CIGS thin-film that the utility model provides assists the selenizing device to have the following advantages:
(1) will evaporate independently plasma body source of the gas of selenium binding plasma generating unit conduct, thereby the plasma body air supply system will be separated with the selenizing device, carry out the isoparametric accurate control of temperature and air pressure respectively;
(2) selenizing temperature is starkly lower than traditional selenizing temperature, has realized the low temperature selenizing to the copper-indium-galliun-selenium precursor thin-film, and cooperates the selenizing technical matters of syllogic in the selenizing stove, can guarantee the homogeneity of CIGS film.
(3) cool off through the residual gas of cold-trap after, avoided the pollution of environment to external world of high poisonous gas on the one hand selenizing; On the other hand, can also reclaim the starting material that the cold-trap internal cooling obtains, thus can recycling selenium steam, have the advantage of practicing thrift cost.
(4) entire equipment has with low cost, making processes and advantage simple to operate.
Description of drawings
The plasma body of the preparation CIGS thin-film that Fig. 1 provides for the utility model is assisted the structural representation of selenizing device;
The plasma body of the preparation CIGS thin-film that Fig. 2 provides for the utility model is assisted the structural representation of slot in the selenizing device;
The plasma body of the preparation CIGS thin-film that Fig. 3 provides for the utility model is assisted the structural representation of cold-trap in the selenizing device.
Embodiment
Below in conjunction with accompanying drawing the utility model is elaborated:
As shown in Figure 1, the plasma body of the preparation CIGS thin-film that the utility model provides is assisted the selenizing device, comprising: inlet system 1, thermal evaporation stove 2, plasma producing apparatus 3 and selenizing stove 4 and the system 5 of giving vent to anger; The cavity of thermal evaporation stove 2 is equipped with first silica tube 21; The cavity of plasma producing apparatus 3 is equipped with second silica tube 31; The cavity of selenizing stove 4 is equipped with the 3rd silica tube 41, and inlet system 1, first silica tube 21, second silica tube 31 and the 3rd silica tube 41 and the system 5 of giving vent to anger are communicated with in order.
Wherein, inlet system 1 can be the stainless steel inlet pipe; The system of giving vent to anger 5 can be the stainless steel escape pipe.In the pipe of first silica tube 21, be placed with plumbago crucible, plumbago crucible is used to place selenium powder or granules of selenium.Between second silica tube 31 and the 3rd silica tube 41, heated filament pipe 6 is installed also; The entrance end of heated filament pipe 6 is communicated with second silica tube 31, and the exit end of heated filament pipe 6 is communicated with the 3rd silica tube 41.As shown in Figure 2; Slot 7 is installed in the pipe of the 3rd silica tube 41; Slot 7 is used for fixing the copper-indium-galliun-selenium precursor thin-film; The material of slot can be graphite, Mo, W or Ta, according to actual needs and the size of the 3rd silica tube sectional area, and can disposable placement tens even hundreds of sheet copper-indium-galliun-selenium precursor thin-film.。Exit end at the 3rd silica tube 41 is equipped with tensimeter 8, and for easy to use, tensimeter can be digital display manometer.In addition, the exit end at the 3rd silica tube 41 can also be communicated with cold-trap 9.
As shown in Figure 3, cold-trap 9 comprises: interior pipe 91 and outer tube 92; Interior pipe 91 is built in the inside of outer tube 92; Outer tube 92 is communicated with water-in 93 and water outlet 94; The inlet pipe mouth of interior pipe 91 is communicated with the exit end of the 3rd silica tube 41, and the outlet spout of interior pipe 91 is communicated with the system of giving vent to anger 5.
In order accurately to control plasma body source of the gas and selenizing parameter respectively, also comprise first valve and second valve; Wherein, first valve is installed in the air inlet mouth of pipe place of stainless steel inlet pipe; Second valve is installed in the joint of second silica tube 31 and the 3rd silica tube 41.
The plasma body of the preparation CIGS thin-film that the utility model provides assists the working process of selenizing device to be:
(1) for independent accurately control plasma body source of the gas and selenizing parameter, close second valve, and open first valve, to the inlet system delivery of carrier gas, inlet system is transported to carrier gas in first silica tube again through first valve;
In this step, carrier gas can be in advance through overmulling gas tank mixing before getting into inlet system, and the flow through mass flowmeter control carrier gas.And the composition of carrier gas can be adjusted according to actual needs, can be argon gas/hydrogen mixed gas, and wherein, the hydrogen proportion can be 5%, 15% or 10% etc.
(2) in the pipe of first silica tube, place plumbago crucible in advance, plumbago crucible is placed with a certain amount of selenium powder or granules of selenium, for example: about 1 gram; After carrier gas arrives first silica tube, the heating plumbago crucible, the temperature maintenance that makes plumbago crucible is about 250 ℃; Therefore; Under this temperature, selenium powder or granules of selenium become liquid selenium, and produce a certain amount of selenium steam; Through the rolling action of carrier gas, selenium steam is imported in second silica tube in the plasma producing apparatus;
(3) plasma producing apparatus generally can be the red copper coil of high frequency; Through applying variable high-frequency voltage; And then make gas ionizing in second silica tube, and produce plasma body, make the selenium steam macromolecular mass that is written into be decomposed into highly active selenium atom; Part obtains the high reactivity selenium hydride with hydrogen reaction, and then produces the high reactivity plasma body that comprises selenium hydride, selenium atom, hydrogen and argon.Wherein, plasma producing apparatus can adopt 150W power.
(4) close first valve, and open second valve, the high reactivity plasma body that plasma producing apparatus produces is transported in the 3rd built-in silica tube of selenizing stove through the heated filament pipe.
In the utility model, adopt the purpose of heated filament pipe to be: prevent the high reactivity plasma body in pipeline internal cooling deposition, thus the forfeiture reactive behavior.
(5) the graphite slot is installed in advance in the pipe of the 3rd silica tube, the graphite slot is used for fixing the copper-indium-galliun-selenium precursor thin-film, after importing the high reactivity plasma body; Temperature in the control selenizing stove was kept in the selenizing stove 250 ℃ of temperature 10 minutes, was rapidly heated 420 ℃ then; Keep the selenium vp about 650 holders; And reacted 10 minutes, with the cooling of 25 ℃/min rate of temperature fall, obtain high-quality CIGS film at last.
In the utility model, the selenizing temperature is starkly lower than traditional selenizing temperature, thereby has realized the low temperature selenizing to the copper-indium-galliun-selenium precursor thin-film, and cooperates the selenizing technical matters of syllogic in the selenizing stove, can guarantee the homogeneity of CIGS film.
(6) after being purified through cold-trap, the residual gas after the selenizing is discharged to the external world.
The residual gas of cold-trap after to selenizing cools off, and makes toxic gas cooling such as selenium steam in cold-trap, avoided the pollution of environment to external world of high poisonous gas on the one hand; On the other hand, can also reclaim the starting material that the cold-trap internal cooling obtains, thus can recycling selenium steam, have the advantage of practicing thrift cost.
In sum, the plasma body of the preparation CIGS thin-film that the utility model provides is assisted the selenizing device, has the following advantages:
(1) will evaporate independently plasma body source of the gas of selenium binding plasma generating unit conduct, thereby the plasma body air supply system will be separated with the selenizing device, carry out the isoparametric accurate control of temperature and air pressure respectively;
(2) selenizing temperature is starkly lower than traditional selenizing temperature, has realized the low temperature selenizing to the copper-indium-galliun-selenium precursor thin-film, and cooperates the selenizing technical matters of syllogic in the selenizing stove, can guarantee the homogeneity of CIGS film.
(3) cool off through the residual gas of cold-trap after, avoided the pollution of environment to external world of high poisonous gas on the one hand selenizing; On the other hand, can also reclaim the starting material that the cold-trap internal cooling obtains, thus can recycling selenium steam, have the advantage of practicing thrift cost.
(4) entire equipment has with low cost, making processes and advantage simple to operate.
The above only is the preferred implementation of the utility model; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the utility model principle; Can also make some improvement and retouching, these improvement and retouching also should be looked the protection domain of the utility model.
Claims (10)
1. a plasma body for preparing CIGS thin-film is assisted the selenizing device, it is characterized in that, comprising: inlet system, thermal evaporation stove, plasma producing apparatus, selenizing stove and the system of giving vent to anger; The cavity of said thermal evaporation stove is equipped with first silica tube; The cavity of said plasma producing apparatus is equipped with second silica tube; The cavity of said selenizing stove is equipped with the 3rd silica tube, and said inlet system, said first silica tube, said second silica tube, said the 3rd silica tube and the said system of giving vent to anger are communicated with in order.
2. the plasma body of preparation CIGS thin-film according to claim 1 is assisted the selenizing device, it is characterized in that said inlet system is the stainless steel inlet pipe; The said system of giving vent to anger is the stainless steel escape pipe.
3. the plasma body of preparation CIGS thin-film according to claim 2 is assisted the selenizing device, it is characterized in that said inlet system also comprises: first valve; Said first valve is installed in the air inlet mouth of pipe place of said stainless steel inlet pipe.
4. the plasma body of preparation CIGS thin-film according to claim 1 is assisted the selenizing device, it is characterized in that, in the pipe of said first silica tube, is placed with plumbago crucible.
5. the plasma body of preparation CIGS thin-film according to claim 1 is assisted the selenizing device, it is characterized in that, between said second silica tube and said the 3rd silica tube, the heated filament pipe is installed also; The entrance end of said heated filament pipe is communicated with said second silica tube, and the exit end of said heated filament pipe is communicated with said the 3rd silica tube.
6. the plasma body of preparation CIGS thin-film according to claim 1 is assisted the selenizing device, it is characterized in that, in the joint of said second silica tube and said the 3rd silica tube second valve is installed also.
7. the plasma body of preparation CIGS thin-film according to claim 1 is assisted the selenizing device, it is characterized in that, in the pipe of said the 3rd silica tube, slot is installed.
8. the plasma body of preparation CIGS thin-film according to claim 1 is assisted the selenizing device, it is characterized in that, at the exit end of said the 3rd silica tube tensimeter is installed.
9. the plasma body of preparation CIGS thin-film according to claim 1 is assisted the selenizing device, it is characterized in that, also is communicated with cold-trap at the exit end of said the 3rd silica tube.
10. the plasma body of preparation CIGS thin-film according to claim 9 is assisted the selenizing device, it is characterized in that said cold-trap comprises: interior pipe and outer tube; Pipe is built in the inside of said outer tube in said; Said outer tube is communicated with water-in and water outlet; The inlet pipe mouth of pipe is communicated with the exit end of said the 3rd silica tube in said, the outlet spout and the said system connectivity of giving vent to anger of said interior pipe.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012201246240U CN202499904U (en) | 2012-03-29 | 2012-03-29 | Plasma-assisted selenizing device for preparing copper-indium-gallium-selenium (CIGS) thin films |
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| CN2012201246240U CN202499904U (en) | 2012-03-29 | 2012-03-29 | Plasma-assisted selenizing device for preparing copper-indium-gallium-selenium (CIGS) thin films |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965641A (en) * | 2012-12-05 | 2013-03-13 | 中国电子科技集团公司第十八研究所 | Selenizing method of CIGS (Copper Indium Gallium Selenide) layer of thin film solar cell |
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2012
- 2012-03-29 CN CN2012201246240U patent/CN202499904U/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965641A (en) * | 2012-12-05 | 2013-03-13 | 中国电子科技集团公司第十八研究所 | Selenizing method of CIGS (Copper Indium Gallium Selenide) layer of thin film solar cell |
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Granted publication date: 20121024 |
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| CX01 | Expiry of patent term |