CN101916794A - Equipment for continuously preparing CIGSeS solar cell absorption layer - Google Patents
Equipment for continuously preparing CIGSeS solar cell absorption layer Download PDFInfo
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- CN101916794A CN101916794A CN2010102169463A CN201010216946A CN101916794A CN 101916794 A CN101916794 A CN 101916794A CN 2010102169463 A CN2010102169463 A CN 2010102169463A CN 201010216946 A CN201010216946 A CN 201010216946A CN 101916794 A CN101916794 A CN 101916794A
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- 238000010521 absorption reaction Methods 0.000 title abstract description 11
- 230000007704 transition Effects 0.000 claims abstract description 39
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims description 25
- 239000011669 selenium Substances 0.000 claims description 15
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 12
- 239000005864 Sulphur Substances 0.000 claims description 12
- 229910052711 selenium Inorganic materials 0.000 claims description 12
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000033001 locomotion Effects 0.000 claims description 7
- 238000005070 sampling Methods 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 4
- 230000007423 decrease Effects 0.000 claims description 3
- 210000000245 forearm Anatomy 0.000 claims description 3
- 239000012774 insulation material Substances 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000001228 spectrum Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract description 2
- 238000004073 vulcanization Methods 0.000 abstract 3
- 230000031700 light absorption Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 23
- 238000000034 method Methods 0.000 description 22
- 238000005987 sulfurization reaction Methods 0.000 description 21
- 239000012528 membrane Substances 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 239000012159 carrier gas Substances 0.000 description 6
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 5
- 229910052733 gallium Inorganic materials 0.000 description 5
- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 3
- 229910052951 chalcopyrite Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000004876 x-ray fluorescence Methods 0.000 description 3
- 229910052774 Proactinium Inorganic materials 0.000 description 2
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Photovoltaic Devices (AREA)
Abstract
The invention discloses equipment for continuously preparing a CIGSeS solar cell absorption layer, which belongs to the technical field of equipment for preparing photovoltaic new energy materials. The equipment is a continuous five-chamber selenylation and vulcanization furnace; a preheating chamber, a selenylation chamber, a transition chamber, a vulcanization chamber and a cooling chamber are connected in turn; and a CIGSeS/CIGSe composite absorption layer with S component gradient distribution can be prepared by adopting the continuous five-chamber selenylation and vulcanization furnace, wherein the absorption layer not only improves the band gap based on CISe, but also forms a band gap gradient along the thickness direction to increase absorption of light energy in solar spectrum and improve the photoelectric conversion efficiency of a CISe series solar cell. According to the equipment, a manufacturing process for the CISe series thin-film solar cell is simple, has low manufacturing cost, good operation stability and high production efficiency, and provides convenience and equipment guarantee for preparing the CISe series solar cell with high photoelectric conversion efficiency and large area.
Description
Technical field
The invention belongs to preparation photovoltaic new energy materials device therefor technical field, particularly a kind of equipment of continuous preparation CIGSSe solar cell absorbing layer.
Background technology
Copper indium diselenide (CuInSe
2, be called for short CISe) and be that solar cell is considered to the most potential thin-film solar cells of new generation, have high-photoelectric transformation efficiency, low cost, strong, the stable advantages of higher of capability of resistance to radiation.CISe be the basic structure of solar cell be (descending) substrate the Mo back electrode CISe be absorbed layer resilient coating Window layer transparent electrode layer metal gates (on).
Basis material CISe is the direct gap semiconductor material, energy gap 1.04eV, and the absorption coefficient of light reaches 10
5Cm
-1Magnitude.Absorbed layer as solar cell, the ideal range of energy gap is 1.4eV～1.6eV, prepare the energy gap that CIGSe, CIGS, CIGSeS can effectively improve absorbed layer by doped gallium in CISe (Ga), sulphur (S) element, improve the conversion efficiency of CISe solar cell.At present, CIGSeS film main preparation methods has coevaporation method and prefabricated membrane selenizing sulfuration method.Coevaporation method can prepare the high-quality CIGSeS film of small size, but is difficult to prepare the uniform CIGSeS film of large tracts of land.Prefabricated membrane selenizing sulfuration method is owing to the process that has adopted the magnetron sputtering technique that is suitable for the even plated film of large tracts of land to be considered to most possibly to realize large tracts of land uniform preparation CIGSeS film.
But the CIGSeS film all prepares through sulfuration on the basis of CIGSe film at present.In operating process, the CIGSe film can be exposed to a period of time in the external environment (air) before sulfuration, make oxygen in the environment, solid particle polluter etc. destroy the surface state of CIGSe film, reduced the quality of CIGSeS film, battery performance is caused negative influence.
Therefore, the present invention has designed a kind of equipment---the continous way five Room selenizing vulcanizing ovens that can realize preparing continuously the CIGSeS/CIGSe composite absorption floor with the distribution of S component gradient, make CIGSeS/CIGSe absorbed layer film not only on the CISe material foundation, improve energy gap, and make it to form band gap gradient along the absorber thickness direction, increase is to the absorption of luminous energy in the solar spectrum, and having improved CISe is the photoelectric conversion efficiency of solar cell.
Summary of the invention
The equipment that the purpose of this invention is to provide a kind of continuous preparation CIGSSe solar cell absorbing layer (CIGSeS/CIGSe composite absorption layer), it is characterized in that: this equipment is mainly by preheating chamber, the selenizing chamber, transition chamber, five operating rooms of vulcanizing chamber and cooling chamber form, wherein, preheating chamber, the selenizing chamber, transition chamber, vulcanizing chamber links to each other in turn with cooling chamber, and between two adjacent operating rooms gate valve is set, each operating room's outer wall resistance heater of evenly arranging, make the indoor temperature of respectively working even, covering insulation material outside heater, guarantee that the equipment outside wall temperature is no more than 40 ℃, at preheating chamber, be respectively equipped with the sample presentation manipulator in transition chamber and the cooling chamber, transition manipulator and sampling manipulator, in selenizing chamber and vulcanizing chamber, be respectively equipped with selenizing chamber sample support platform and vulcanizing chamber specimen holder support platform, be respectively equipped with selenium source heating tank and sulphur source heating tank in the bottom of selenizing chamber and vulcanizing chamber, this equipment vacuum system is a mechanical pump, lobe pump, three grades of pumped vacuum systems of molecular pump.
In the said equipment, selenizing chamber sample support platform and vulcanizing chamber specimen holder support platform are liftable specimen holder support platform.
Selenizing chamber sample support platform and vulcanizing chamber specimen holder support platform drive its rising or decline by cylinder.
In the said equipment, sample presentation manipulator, transition manipulator and sampling manipulator are four link robot manipulator, and the transition manipulator can whole Rotate 180 °.
Described four link robot manipulator comprise mechanical arm, mechanical arm rolling bearing, gear train, synchromesh gear group and specimen holder saddle, described four link robot manipulator provide power by stepping motor, stepping motor drives the reciprocating motion of specimen holder saddle by gear drive, realize the stretching, extension and the retraction of manipulator, the synchromesh gear group guarantees that specimen holder saddle movement locus is a straight line.
Described mechanical arm is made up of forearm (near specimen holder saddle one side), postbrachium (near gear train one side) two parts, and forward and backward arm connects by described mechanical rotation bearing shaft realizes stretching, contracting of mechanical arm; Described gear train, described synchromesh gear group realize the fixing of the forward and backward arm of described mechanical arm respectively by screw thread-screw rod connection; Described specimen holder saddle and described synchromesh gear group are connected and fixed by screw thread-screw rod.
This equipment base vacuum can reach 1.0 * 10
-3Pa.
Each operating room's operating temperature range of the said equipment is: 25 ℃～500 ℃ of preheating chambers, 25 ℃～600 ℃ of selenizing chambers, 25 ℃～400 ℃ of transition chambers, 25 ℃～500 ℃ of vulcanizing chambers, 25 ℃～400 ℃ of cooling chambers.
Beneficial effect of the present invention is: adopt continous way five Room selenizing vulcanizing ovens to prepare and have the CIGSeS/CIGSe composite absorption floor that the S component gradient distributes, make this absorbed layer not only on the CISe basis, improve band gap, and make it to form band gap gradient along the absorber thickness direction, increase is to the absorption of luminous energy in the solar spectrum, and having improved CISe is the photoelectric conversion efficiency of solar cell.
The present invention can be so that copper indium diselenide (CuInSe
2, being called for short CISe) and the manufacturing process of series film solar battery is simple, low cost of manufacture, operational stability is good, and the production efficiency height is for preparation high-photoelectric transformation efficiency, large tracts of land CISe are that solar cell provides convenient and equipment guarantees.
Description of drawings
Fig. 1 is five Room selenizing vulcanizing oven schematic diagrames;
Fig. 2 is a manipulator initial position schematic diagram;
Fig. 3 is that manipulator stretches the back position view;
Fig. 4 is a specimen holder transmittance process schematic diagram;
Number in the figure:
The 1-preheating chamber, 2-selenizing chamber, 3-transition chamber, 4-vulcanizing chamber, 5-cooling chamber, the 6-manipulator of taking a sample, the 7-gate valve, 8-vulcanizing chamber specimen holder support platform, 9-sulphur source heating tank, 10-transition manipulator, 11-selenizing chamber sample support platform, 12-selenium source heating tank, 13-sample presentation manipulator, the 21-mechanical arm, 22-gear train, 23-mechanical arm rolling bearing, 24-specimen holder saddle, 25-synchromesh gear group, 26-specimen holder.
Embodiment
The invention provides a kind of equipment that can prepare CIGSeS/CIGSe composite absorption layer continuously, the present invention further described below in conjunction with embodiment:
Embodiment 1
A kind of equipment of continuous preparation CIGSSe solar cell absorbing layer, as shown in Figure 1, this equipment is mainly by preheating chamber 1, selenizing chamber 2, transition chamber 3,5 five operating rooms of vulcanizing chamber 4 and cooling chamber form, wherein, preheating chamber 1, selenizing chamber 2, transition chamber 3, vulcanizing chamber 4 links to each other in turn with cooling chamber 5, and between two adjacent operating rooms gate valve 7 is set, each operating room's outer wall resistance heater of evenly arranging, make the indoor temperature of respectively working even, covering insulation material outside heater, guarantee that the equipment outside wall temperature is no more than 40 ℃, at preheating chamber 1, be respectively equipped with sample presentation manipulator 13 in transition chamber 3 and the cooling chamber 5, transition manipulator 10 and sampling manipulator 6, in selenizing chamber 2 and vulcanizing chamber 4, be respectively equipped with selenizing chamber sample support platform 11 and vulcanizing chamber specimen holder support platform 8, be respectively equipped with selenium source heating tank 12 and sulphur source heating tank 9 in the bottom of selenizing chamber 2 and vulcanizing chamber 4, selenium source is solid-state simple substance selenium, the sulphur source is solid-state elemental sulfur, this equipment vacuum system is a mechanical pump, lobe pump, three grades of pumped vacuum systems of molecular pump, this equipment base vacuum can reach 1.0 * 10
-3Pa.
In the said equipment, selenizing chamber sample support platform 11 and vulcanizing chamber specimen holder support platform 8 are liftable specimen holder support platform.
Selenizing chamber sample support platform 11 and vulcanizing chamber specimen holder support platform 8 drive its rising or decline by cylinder.
In the said equipment, sample presentation manipulator 13, transition manipulator 10 and sampling manipulator 6 are four link robot manipulator, and transition manipulator 10 can whole Rotate 180 °.
Described four link robot manipulator comprise mechanical arm 21, mechanical arm rolling bearing 23, gear train 22, synchromesh gear group 25 and specimen holder saddle 24, described four link robot manipulator provide power by stepping motor, stepping motor drives 24 reciprocating motions of specimen holder saddle by gear drive, realize the stretching, extension and the retraction of manipulator, the synchromesh gear group guarantees that specimen holder saddle movement locus is a straight line.
Described mechanical arm 21 is made up of forearm (near specimen holder saddle 24 1 sides), postbrachium (near gear train 22 1 sides) two parts, and forward and backward arm connects by 23 on described mechanical rotation bearing realizes stretching, contracting of mechanical arm; Described gear train 22, described synchromesh gear group 25 realize the fixing of described mechanical arm 21 forward and backward arms respectively by screw thread-screw rod connection; Described specimen holder saddle 24 and described synchromesh gear group 25 are connected and fixed by screw thread-screw rod.
Manipulator initial position schematic diagram is shown in 2, and manipulator stretches the back position view as shown in Figure 3.
Each operating room's operating temperature range of the said equipment is: 25 ℃～500 ℃ of preheating chambers, 25 ℃～600 ℃ of selenizing chambers, 25 ℃～400 ℃ of transition chambers, 25 ℃～500 ℃ of vulcanizing chambers, 25 ℃～400 ℃ of cooling chambers.
In the preparation CIGSeS/CIGSe laminated film process, interoperation by manipulator and specimen holder support platform is realized the transmission of sample between each operating room, with manipulator sample presentation process is the transport process of example (sequence of movement of sampling process in contrast) interpret sample, as shown in Figure 4.When sample presentation manipulator 13 stretches (shown in Fig. 4-a), until specimen holder 26 is transported to specimen holder support platform 11 directly over when (shown in Fig. 4-b), specimen holder support platform 11 rises, specimen holder 26 is held up until the specimen holder saddle (24) (shown in Fig. 4-c) that leaves manipulator, manipulator retraction (shown in Fig. 4-d) then, be back to original position, finish the sample presentation process.
The equipment work process is as follows:
During preparation CIGSeS/CIGSe laminated film, be sample, sample is placed on the special titanium alloy specimen holder, put into equipment of the present invention (five Room selenizing vulcanizing ovens) again and carry out the selenizing sulfuration with copper indium gallium (CuInGa) alloy prefabricated membrane.Wherein, the substrate of CuInGa alloy prefabricated membrane is a soda-lime glass, first sputter one deck Mo back electrode in substrate, adopt the method for midfrequent AC magnetron sputtering to prepare CuInGa alloy prefabricated membrane again on the metal molybdenum back electrode, CuInGa alloy prefabricated membrane can adopt CuIn, CuGa dual-target sputtering prepared or adopt the single target sputtering technology preparation of CuInGa.
At first, utilize three grades of pumped vacuum systems that equipment is vacuumized, treat that each operating room's vacuum degree reaches 1.0 * 10
-3Behind the Pa, in each operating room, charge into carrier gas, heat each operating room to proper temperature.After treating that each operating room reaches design temperature, open preheating chamber 1, specimen holder is placed on the specimen holder saddle of sample presentation manipulator 13 in the preheating chamber 1, close preheating chamber 1, the beginning preheating.Need preheating chamber 1 is vacuumized after putting into sample, treat that vacuum degree reaches 1.0 * 10
-3Behind the Pa, in preheating chamber 1, charge into carrier gas with selenizing chamber 2 balances.Behind the samples pre-heated certain hour, open the gate valve of 2 of preheating chamber 1 and selenizing chambers, specimen holder is sent to selenizing chamber 2 by sample presentation manipulator 13.Under the drive of cylinder, selenizing chamber specimen holder support platform 11 rises the saddle of specimen holder band from sample presentation manipulator 13, and sample presentation manipulator 13 is back to preheating chamber 1 then, closes the gate valve of 2 of preheating chamber 1 and selenizing chambers, and selenizing begins.After selenizing finishes, open the gate valve of 3 of selenizing chamber 2 and transition chambers, transition manipulator 10 extends in the selenizing chamber 2, under the drive of cylinder, specimen holder support platform 11 times general who has surrendered's specimen holders in selenizing chamber play back on the saddle of transition manipulator 10, transition manipulator 10 is back to transition chamber 3 then, closes the gate valve of 2 of transition chamber 3 and selenizing chambers, and selenizing finishes.In transition chamber 3, transition manipulator 10 whole Rotate 180s °, open the gate valve of 4 of transition chamber 3 and vulcanizing chambers then, by transition manipulator 10 specimen holder is transported to vulcanizing chamber 4, under the drive of cylinder, vulcanizing chamber specimen holder support platform 8 rises the saddle of specimen holder band from transition manipulator 10, and transition manipulator 10 is back to transition chamber then, close the gate valve of 4 of transition chamber 3 and vulcanizing chambers, the sulfuration beginning.Behind the sulfuration certain hour, open the gate valve of 4 of cooling chamber 5 and vulcanizing chambers, cooling manipulator 6 extends in the vulcanizing chamber, and under the drive of cylinder, the playback of 8 times general who has surrendered's specimen holders of vulcanizing chamber specimen holder support platform is on the saddle of cooling manipulator 6, cool off manipulator 6 then and be back to cooling chamber, close the gate valve of 4 of cooling chamber 5 and vulcanizing chambers, sulfuration finishes, treat that sample is cooled to proper temperature after, take out sample, finish continuous selenizing sulfuration process.
Embodiment 2
With copper indium gallium (CuInGa) alloy prefabricated membrane is sample, adopts the equipment of embodiment 1 to carry out the selenizing sulfuration, the preparation CIGSSe solar cell absorbing layer.
Select 200 ℃ of preheat temperatures for use, 450 ℃ of selenizing temperature, selenizing time 10min, 550 ℃ of selenium source temperature, 400 ℃ of curing temperatures, cure time 5min, the technological parameter that the sulphur source temperature is 400 ℃ prepares the CIGSeS/CIGSe laminated film, and the work carrier gas is a high-purity N
2Operating process is as follows:
1), adopt three grades of pumped vacuum systems, take out each operating room's vacuum to 1.0 * 10
-3Pa.
2), charge into work carrier gas high-purity N to each operating room
2
3), heat each operating room to preset temperature: 200 ℃ of preheating chambers, 450 ℃ of selenizing chambers, 400 ℃ of vulcanizing chambers, 550 ℃ of selenium source temperature, 400 ℃ of sulphur source temperatures.
4), open preheating chamber, put into the specimen holder of placing sample.
5), behind the preheating 10min, specimen holder is sent to the selenizing chamber, the beginning selenizing.
6), behind the selenizing 10min, the sample in the selenizing chamber is sent to vulcanizing chamber via transition chamber, begin sulfuration.
7), the sulfuration 5min after, sample is sent to cooling chamber, finish the selenizing sulfuration process.
The CIGSeS/CIGSe laminated film for preparing is carried out X-ray diffraction analysis (XRD), X-ray fluorescence spectra analysis (XRF), scanning electron microscopy (SEM) observation analysis, finding to adopt continous way five Room selenizing vulcanizing ovens successfully to prepare structure is that chalcopyrite phase, component ratio are Cu/ (In+Ga)=0.95, the CIGSeS/CIGSe laminated film of S/ (S+Se)=0.2, the grain size desirable suitable preparation solar cell about 1 μ m.
Embodiment 3
With copper indium gallium (CuInGa) alloy prefabricated membrane is sample, adopts the equipment of embodiment 1 to carry out the selenizing sulfuration, the preparation CIGSSe solar cell absorbing layer.
Select 300 ℃ of preheat temperatures for use, 550 ℃ of selenizing temperature, selenizing time 20min, 550 ℃ of selenium source temperature, 500 ℃ of curing temperatures, cure time 10min, the technological parameter that the sulphur source temperature is 450 ℃ prepares the CIGSeS/CIGSe laminated film.Operating process is as follows:
1), adopt three grades of pumped vacuum systems, take out each operating room's vacuum to 1.0 * 10
-3Pa.
2), charge into work carrier gas high-purity N to each operating room
2
3), heat each operating room to preset temperature: 300 ℃ of preheating chambers, 550 ℃ of selenizing chambers, 500 ℃ of vulcanizing chambers, 550 ℃ of selenium source temperature, 450 ℃ of sulphur source temperatures.
4), open the preheating chamber door, put into the specimen holder of placing sample.
5), behind the preheating 10min, specimen holder is sent to the selenizing chamber, the beginning selenizing.
6), behind the selenizing 20min, the sample in the selenizing chamber is sent to vulcanizing chamber via transition chamber, begin sulfuration.
7), the sulfuration 10min after, sample is sent to cooling chamber, finish the selenizing sulfuration process.
The CIGSeS/CIGSe laminated film for preparing is carried out X-ray diffraction analysis (XRD), X-ray fluorescence spectra analysis (XRF), scanning electron microscopy (SEM) observation analysis, finding to adopt continous way five Room selenizing vulcanizing ovens successfully to prepare structure is that chalcopyrite phase, component ratio are Cu/ (In+Ga)=0.96, the CIGSeS/CIGSe laminated film of S/ (S+Se)=0.25, the grain size desirable suitable preparation solar cell about 1.2 μ m.
Embodiment 4
With copper indium gallium (CuInGa) alloy prefabricated membrane is sample, adopts the equipment of embodiment 1 to carry out the selenizing sulfuration, the preparation CIGSSe solar cell absorbing layer.
Select 400 ℃ of preheat temperatures for use, 500 ℃ of selenizing temperature, selenizing time 10min, 550 ℃ of selenium source temperature, 500 ℃ of curing temperatures, cure time 10min, the technological parameter that the sulphur source temperature is 500 ℃ prepares the CIGSeS/CIGSe laminated film.Operating process is as follows:
1), adopt three grades of pumped vacuum systems, take out each operating room's vacuum to 1.0 * 10
-3Pa.
2), charge into work carrier gas high-purity N to each operating room
2
3), heat each operating room to preset temperature: 400 ℃ of preheating chambers, 500 ℃ of selenizing chambers, 500 ℃ of vulcanizing chambers, 550 ℃ of selenium source temperature, 500 ℃ of sulphur source temperatures.
4), open the preheating chamber door, put into the specimen holder of placing sample.
5), behind the preheating 10min, specimen holder is sent to the selenizing chamber, the beginning selenizing.
6), behind the selenizing 10min, the sample in the selenizing chamber by being sent to vulcanizing chamber by transition chamber, is begun sulfuration.
7), the sulfuration 1min after, sample is sent to cooling chamber, finish the selenizing sulfuration process.
The CIGSeS/CIGSe laminated film for preparing is carried out X-ray diffraction analysis (XRD), X-ray fluorescence spectra analysis (XRF), scanning electron microscopy (SEM) observation analysis, finding to adopt continous way five Room selenizing vulcanizing ovens successfully to prepare structure is that chalcopyrite phase, component ratio are Cu/ (In+Ga)=0.95, the CIGSeS/CIGSe laminated film of S/ (S+Se)=0.34, the grain size desirable suitable preparation solar cell about 1.5 μ m.
Claims (8)
1. continuous equipment of preparation CIGSSe solar cell absorbing layer, it is characterized in that: this equipment is mainly by preheating chamber (1), selenizing chamber (2), transition chamber (3), (5) five operating rooms of vulcanizing chamber (4) and cooling chamber form, wherein, preheating chamber (1), selenizing chamber (2), transition chamber (3), vulcanizing chamber (4) links to each other in turn with cooling chamber (5), and between two adjacent operating rooms gate valve (7) is set, each operating room's outer wall resistance heater of evenly arranging, make the indoor temperature of respectively working even, covering insulation material outside heater, guarantee that the equipment outside wall temperature is no more than 40 ℃, in preheating chamber (1), be respectively equipped with sample presentation manipulator (13) in transition chamber (3) and the cooling chamber (5), transition manipulator (10) and sampling manipulator (6), in selenizing chamber (2) and vulcanizing chamber (4), be respectively equipped with selenizing chamber sample support platform (11) and vulcanizing chamber specimen holder support platform (8), be respectively equipped with selenium source heating tank (12) and sulphur source heating tank (9) in the bottom of selenizing chamber (2) and vulcanizing chamber (4), this equipment vacuum system is a mechanical pump, lobe pump, three grades of pumped vacuum systems of molecular pump.
2. the equipment of a kind of continuous preparation CIGSSe solar cell absorbing layer according to claim 1 is characterized in that: described selenizing chamber sample support platform (11) and vulcanizing chamber specimen holder support platform (8) are liftable specimen holder support platform.
3. the equipment of a kind of continuous preparation CIGSSe solar cell absorbing layer according to claim 1 and 2 is characterized in that: described selenizing chamber sample support platform (11) and vulcanizing chamber specimen holder support platform (8) drive its rising or decline by cylinder.
4. the equipment of a kind of continuous preparation CIGSSe solar cell absorbing layer according to claim 1, it is characterized in that: described sample presentation manipulator (13), transition manipulator (10) and sampling manipulator (6) are four link robot manipulator, and transition manipulator (10) can whole Rotate 180 °.
5. the equipment of a kind of continuous preparation CIGSSe solar cell absorbing layer according to claim 4, it is characterized in that: described four link robot manipulator comprise mechanical arm (21), mechanical arm rolling bearing (23), gear train (22), synchromesh gear group (25) and specimen holder saddle (24), described four link robot manipulator provide power by stepping motor, stepping motor drives specimen holder saddle (24) reciprocating motion by gear drive, realize the stretching, extension and the retraction of manipulator, the synchromesh gear group guarantees that specimen holder saddle movement locus is a straight line.
6. the equipment of a kind of continuous preparation CIGSSe solar cell absorbing layer according to claim 5, it is characterized in that: described mechanical arm (21) is made up of forearm, postbrachium two parts, and forward and backward arm connects by described mechanical rotation bearing (23) axle realizes stretching, contracting of mechanical arm; Described gear train (22), described synchromesh gear group (25) realize the fixing of the forward and backward arm of described mechanical arm (21) respectively by screw thread-screw rod connection; Described specimen holder saddle (24) and described synchromesh gear group (25) are connected and fixed by screw thread-screw rod.
7. the equipment of a kind of continuous preparation CIGSSe solar cell absorbing layer according to claim 1 is characterized in that: described equipment base vacuum can reach 1.0 * 10
-3Pa.
8. the equipment of a kind of continuous preparation CIGSSe solar cell absorbing layer according to claim 1, it is characterized in that: each operating room's operating temperature range of described equipment is: 25 ℃～500 ℃ of preheating chambers, 25 ℃～600 ℃ of selenizing chambers, 25 ℃～400 ℃ of transition chambers, 25 ℃～500 ℃ of vulcanizing chambers, 25 ℃～400 ℃ of cooling chambers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102169463A CN101916794A (en) | 2010-06-25 | 2010-06-25 | Equipment for continuously preparing CIGSeS solar cell absorption layer |
Applications Claiming Priority (1)
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