CN103296139B - A kind of preparation method of copper-indium-galliun-selenium film solar cell absorbed layer - Google Patents
A kind of preparation method of copper-indium-galliun-selenium film solar cell absorbed layer Download PDFInfo
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Abstract
The preparation method that the invention discloses a kind of copper-indium-galliun-selenium film solar cell absorbed layer, it be the method adopting magnetically controlled DC sputtering at soda-lime deposition on glass double-level-metal Mo electrode, then by the method for rf magnetron sputtering by sputtering CIGS quaternary alloy list target (CuIn0.7Ga0.3Se2) on Mo electrode, deposit CIGS thin film.Sputter procedure keeps certain base reservoir temperature and sputtering power, sputters obtained CIGS thin film and there is yellow copper structure, be suitable as the absorbed layer of solaode, method of the present invention not only cost is low, technique is simple, and eliminates selenized annealing, is more beneficial for environmental protection.
Description
Technical field
The invention belongs to technical field of solar batteries, the preparation method being specifically related to a kind of copper-indium-galliun-selenium film solar cell absorbed layer.
Background technology
Copper-indium-galliun-selenium film solar cell is considered as the solaode of future generation of most potentiality, has the life-span long, stable performance, and production cost is low, and radiation resistance is strong, the advantage such as excellent low light level individual features and higher electricity conversion.Its structure of current copper-indium-galliun-selenium film solar cell is generally by soda-lime glass, metal Mo electrode, absorbed layer CIGS (CIGS) thin film, cushion cadmium sulfide (CdS), and zinc oxide (ZnO), mix the zinc oxide (AZO) of aluminum, the upper electrode composition of Al/Ag；Wherein Mo electrode prepares mainly by the method for magnetically controlled DC sputtering, and absorbed layer CIGS (CIGS) thin film is mainly obtained by the method sputtered by three stage Co-evaporation or two steps.For the CIGS thin film solaode of extensive, large area manufacture, the method for three stage Co-evaporation is complex, it is difficult to composition and deposition process are accurately controlled, and improves the repeatability of property of thin film；And the method for two step sputterings also has weak point, in the process of sputtering preformed layer, the preformed layer of rich In and rich Ga is easily caused CIGS thin film rough surface, and selenizing also can to environment.Preparation technology and device architecture yet with relative complex, the industrialization of copper-indium-galliun-selenium film solar cell is faced with very big difficulty, therefore, further developmental research low cost and the copper-indium-galliun-selenium film solar cell produced of easily looking unfamiliar greatly are significant.
Summary of the invention
The preparation method that the invention provides a kind of copper-indium-galliun-selenium film solar cell absorbed layer, it is characterised in that undertaken by the steps:
1) adopting the method for magnetically controlled DC sputtering at soda-lime deposition on glass double-level-metal Mo electrode, sputtering power is 100w；Described deposition double-level-metal Mo electrode refers to first under operating air pressure 1.4Pa, and sputtering Mo metal targets deposit thickness is the Mo thin film of 100nm, then sputters the thick Mo thin film of Mo metal targets deposition 900nm again under operating air pressure 0.2Pa；
2) adopt the method for rf magnetron sputtering by sputtering CIGS quaternary alloy list target (CuIn0.7Ga0.3Se2) on Mo electrode, deposit CIGS thin film；In sputter procedure, base reservoir temperature controls at 550 DEG C-630 DEG C, and power controls between 100w-200w, and operating air pressure controls between 0.4P-2.0Pa.
The more detailed preparation method of the present invention is as follows:
1) adopt the method for magnetically controlled DC sputtering at soda-lime deposition on glass double-level-metal Mo electrode；
2) adopt the method for rf magnetron sputtering by sputtering CIGS quaternary alloy list target (CuIn0.7Ga0.3Se2) on Mo electrode, deposit CIGS thin film；
Above-mentioned steps 1) in sputtering power be 100W, first under operating air pressure 1.4Pa, sputtering Mo metal targets deposit thickness is the Mo thin film of 100nm, then sputters the thick Mo thin film of Mo metal targets deposition 900nm again under operating air pressure 0.2Pa.
Above-mentioned steps 2) the middle method sputtering CIGS quaternary alloy list target (CuIn adopting rf magnetron sputtering0.7Ga0.3Se2) deposition CIGS thin film, in sputter procedure, base reservoir temperature controls between 550 DEG C-630 DEG C, and power controls between 100W-200W.
One preferred preparation method of the present invention is as follows:
(1) the 99.99% high-purity CIGS (CuIn of sputtering target material respectively diameter 50.9mm, 99.99% high purity metal molybdenum (Mo) target of thickness 3mm and diameter 50.9mm, thickness 3mm0.7Ga0.3Se2) quaternary alloy target, using the length of side be 2.5cm, thickness be 1mm square Soda-lime glass as substrate；
(2) before putting soda-lime glass into chamber, first with acetone ultrasonic cleaning 20min, then with ethanol ultrasonic cleaning 5min, and dried up standby；
(3) base vacuum tested is 4.0 × 10-4Pa, before deposition Mo thin film, carries out bias and cleans 15min substrate, and air pressure during cleaning is 2.0Pa, biases as-400V；
(4) deposit in the process of thin film, substrate constantly rotates to improve the uniformity of thin film, under room temperature, the method utilizing magnetically controlled DC sputtering deposits the Mo back electrode that 900nm is thick on the glass substrate, the method adopting bilayer sputtering, under the noble gas argon of 1.2Pa, first sputter 4min, 36min is sputtered again under the air pressure of 0.4Pa, afterwards again by the method for rf magnetron sputtering, it is being coated with the deposition on glass CIGS thin film of Mo back electrode by sputtering CIGS quaternary alloy target under the air pressure of 0.8Pa, in sputter procedure, power is 100w, and base reservoir temperature is 550 DEG C.
Presently preferred preparation method is as follows:
(1) the 99.99% high-purity CIGS (CuIn of sputtering target material respectively diameter 50.9mm, 99.99% high purity metal molybdenum (Mo) target of thickness 3mm and diameter 50.9mm, thickness 3mm0.7Ga0.3Se2) quaternary alloy target, using the length of side be 2.5cm, thickness be 1mm square Soda-lime glass as substrate；
(2) before putting soda-lime glass into chamber, first with acetone ultrasonic cleaning 20min, then with ethanol ultrasonic cleaning 5min, and dried up standby；
(3) base vacuum tested is 4.0 × 10-4Pa, before deposition Mo thin film, carries out bias and cleans 15min substrate, and air pressure during cleaning is 2.0Pa, biases as-400V；
(4) deposit in the process of thin film, substrate constantly rotates to improve the uniformity of thin film, under room temperature, the method utilizing magnetically controlled DC sputtering deposits the Mo back electrode that 900nm is thick on the glass substrate, the method adopting bilayer sputtering, under the noble gas argon of 1.2Pa, first sputter 4min, 36min is sputtered again under the air pressure of 0.4Pa, afterwards again by the method for rf magnetron sputtering, it is being coated with the deposition on glass CIGS thin film of Mo back electrode by sputtering CIGS quaternary alloy target under the air pressure of 0.8Pa, in sputter procedure, power is 100w, and base reservoir temperature is 630 DEG C.
What the preparation method of copper-indium-galliun-selenium film solar cell absorbed layer provided by the invention had compared with prior art has the active effect that
(1) present invention is by directly sputtering high-purity CIGS (CuIn by the method for rf magnetron sputtering0.7Ga0.3Se2) quaternary alloy target, by changing, technological parameter in inquiry experiment process finds that base reservoir temperature controls between 550 DEG C-620 DEG C, the CIGS thin film that power prepares when controlling between 100w-200w has yellow copper structure, is suitable as the absorbed layer of solaode, and compares with two original step sputtering methods, eliminate this step of selenizing, decreasing the pollution to environment, compare technique with the method for three stage Co-evaporation simple many, the repeatability cutting thin film is higher.
(2) sputter obtained CIGS thin film and there is yellow copper structure (by X-ray diffraction (XRD) test discovery, (112) of corresponding Chalkopyrite, (220)/(204), (116)/(312) peak all occurs in that, and show CIGS well-crystallized by scanning electron microscope (SEM) test), it is suitable as the absorbed layer of solaode.
(3) method of the present invention not only cost is low, and technique is simple, and (original two step sputtering methods refer to that the method first with sputtering prepares CIG preformed layer, carry out selenization subsequently and produce CIGS thin film in selenizing stove to eliminate selenized annealing.Three stage Co-evaporation method refers to, the first step, at underlayer temperature is 300-400 DEG C, and coevaporation In, Ga, Se, form (In0.7Ga0.3)2Se3Preformed layer, second step 500-600 DEG C that underlayer temperature is raised, coevaporation Cu and Se and preformed layer (In0.7Ga0.3)2Se3Reaction forms the CIGS thin film of slightly rich Cu, the 3rd step, and underlayer temperature remains unchanged, In, Ga, the Se that re-evaporation is a small amount of, forms the thin layer of rich In at film surface, and finally gives the CIGS thin film close to stoichiometric proportion), it is more beneficial for environmental protection.
Example figure explanation
Fig. 1 is copper-indium-galliun-selenium film solar cell absorbed layer schematic diagram.1st layer is soda-lime glass, and the 2nd layer is metal Mo electrode, and the 3rd layer is CIGS (CIGS) thin film；
Fig. 2 is by the scanning electron microscopy picture (SEM) on embodiment 1 gained CIGS surface；
Fig. 3 is by the X-ray diffractogram (XRD) on embodiment 1 gained CIGS surface；
Fig. 4 is the X-ray diffractogram (XRD) on embodiment 2 gained CIGS surface；
Fig. 5 is the Raman spectrogram of the CIGS of embodiment 1 gained；
Fig. 6 is the Raman spectrogram of the CIGS of embodiment 2 gained；
Fig. 7 is JGP-450 type magnetron sputtering deposition system；
Wherein 1. substrate, 2 molecular pumps, 3 gas accesses, 4 direct current targets, 5 radio frequency targets.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is further described, rather than the range of application of the restriction present invention.Material used in the present invention is commercially available.
Embodiment 1
Film sample adopts the preparation method of magnetically controlled DC sputtering and rf magnetron sputtering to obtain in JGP-450 type magnetron sputtering deposition system, high-purity (99.99%) CIGS (CuIn of sputtering target material respectively diameter 50.9mm, high-purity (99.99%) metal molybdenum (Mo) target of thickness 3mm and diameter 50.9mm, thick 3mm0.7Ga0.3Se2) quaternary alloy target, using the length of side be 2.5cm, thickness be 1mm square Soda-lime glass as substrate, before putting soda-lime glass into chamber, first with acetone ultrasonic cleaning 20min, then with ethanol ultrasonic cleaning 5min, and dried up.The base vacuum of experiment is 4.0 × 10-4Pa, before deposition Mo thin film, carries out bias and cleans 15min substrate, and air pressure during cleaning is 2.0Pa, biases as-400V.In the process of deposition thin film, substrate constantly rotates to improve the uniformity of thin film.Under room temperature, the method utilizing magnetically controlled DC sputtering deposits the Mo back electrode that about 900nm is thick on the glass substrate, the method adopting bilayer sputtering, under the noble gas argon of 1.2Pa, first sputter 4min, under the air pressure of 0.4Pa, sputter 36min again, afterwards again by the method for rf magnetron sputtering, under the air pressure of 0.8Pa, be coated with the deposition on glass CIGS thin film of Mo back electrode by sputtering CIGS quaternary alloy target, in sputter procedure, power is 100w, and base reservoir temperature is 550 DEG C.
Utilizing D/MAX-2500 type X-ray diffractometer (XRD) that sample carries out thing phase and crystal structure analysis, sweep limits 10 ° ~ 100 °, step-length is 0.02 °, and tube voltage is 40kV, and tube current is 100mA.Adopt the surface topography of scanning electron microscope (SEM) viewing film.
Embodiment 2
Film sample adopts the preparation method of magnetically controlled DC sputtering and rf magnetron sputtering to obtain in JGP-450 type magnetron sputtering deposition system, high-purity (99.99%) CIGS (CuIn of sputtering target material respectively diameter 50.9mm, high-purity (99.99%) metal molybdenum (Mo) target of thickness 3mm and diameter 50.9mm, thickness 3mm0.7Ga0.3Se2) quaternary alloy target, using the length of side be 2.5cm, thickness be 1mm square Soda-lime glass as substrate, before putting soda-lime glass into chamber, first with acetone ultrasonic cleaning 20min, then with ethanol ultrasonic cleaning 5min, and dried up.The base vacuum of experiment is 4.0 × 10-4Pa, before deposition Mo thin film, carries out bias and cleans 15min substrate, and air pressure during cleaning is 2.0Pa, biases as-400V.In the process of deposition thin film, substrate constantly rotates to improve the uniformity of thin film.Under room temperature, the method utilizing magnetically controlled DC sputtering deposits the Mo back electrode that about 900nm is thick on the glass substrate, the method adopting bilayer sputtering, under the noble gas argon of 1.2Pa, first sputter 4min, under the air pressure of 0.4Pa, sputter 36min again, afterwards again by the method for rf magnetron sputtering, under the air pressure of 0.8Pa, be coated with the deposition on glass CIGS thin film of Mo back electrode by sputtering CIGS quaternary alloy target, in sputter procedure, power is 100w, and base reservoir temperature is 630 DEG C.Utilize D/MAX-2500 type X-ray diffractometer (XRD) that sample carries out thing phase and crystal structure analysis.
Embodiment 3
Film sample adopts the preparation method of magnetically controlled DC sputtering and rf magnetron sputtering to obtain in JGP-450 type magnetron sputtering deposition system, high-purity (99.99%) CIGS (CuIn of sputtering target material respectively diameter 50.9mm, high-purity (99.99%) metal molybdenum (Mo) target of thickness 3mm and diameter 50.9mm, thick 3mm0.7Ga0.3Se2) quaternary alloy target, using the length of side be 2.5cm, thickness be 1mm square Soda-lime glass as substrate, before putting soda-lime glass into chamber, first with acetone ultrasonic cleaning 20min, then with ethanol ultrasonic cleaning 5min, and dried up.The base vacuum of experiment is 4.0 × 10-4Pa, before deposition Mo thin film, carries out bias and cleans 15min substrate, and air pressure during cleaning is 2.0Pa, biases as-400V.In the process of deposition thin film, substrate constantly rotates to improve the uniformity of thin film.Under room temperature, the method utilizing magnetically controlled DC sputtering deposits the Mo back electrode that about 900nm is thick on the glass substrate, the method adopting bilayer sputtering, under the noble gas argon of 1.2Pa, first sputter 4min, then under the air pressure of 0.4Pa, sputter 36min, afterwards again by the method for rf magnetron sputtering, it is being coated with the deposition on glass CIGS thin film of Mo back electrode by sputtering CIGS quaternary alloy target under the air pressure of 0.8Pa, thickness is about 1500nm, and in sputter procedure, power is 100w, and base reservoir temperature is 630 DEG C.Thick cadmium sulfide (CdS) cushion of about 50nm is sputtered by the method for rf magnetron sputtering afterwards on CuInGaSe absorbed layer, on cadmium sulfide (CdS) cushion, thick zinc oxide (ZAO) Window layer mixing aluminum of ZnO and 500nm thick for about 50nm is sputtered successively again by the method for rf magnetron sputtering, sputter the thick Al electrode of about 1000nm by the method for magnetically controlled DC sputtering afterwards, so far obtain copper indium gallium selenium solar cell one piece complete.Prepare high efficiency CIGS solaode, it is necessary for preparing highly purified absorbed layer thin film, the crystal grain of thin film to be tried one's best greatly, surfacing, and technique is more simple more good, method in the present invention eliminates selenized annealing, both enormously simplify the complexity of technique, because selenium is poisonous, so the selenium harm to human body can also be avoided by the method for the present invention, in the present invention, we pass through Control release condition, high-quality can be obtained, thin film that crystal grain is relatively larger and found (112) of corresponding yellow copper structure by X-ray diffraction, (220)/(204), (312)/(116) peak all occurs in that, and in existing document is recorded, be mostly three stage Co-evaporation method and by two steps sputtering method obtain CIGS absorbed layer thin film, this is also the difference that the method in the present invention is maximum with additive method.So being expected to prepare high efficiency CIGS solaode by the method in the present invention.
Copper indium gallium selenium solar cell has that stable performance, capability of resistance to radiation are strong, and photoelectric transformation efficiency is currently first of various thin film solar cell, close to existing market main product crystal-silicon solar cell conversion efficiency, cost be but its 1/3.Exactly because its excellent performance is called follow-on cheap solar cell in the world, no matter it is generate electricity at Terrestrial solar or there is wide market prospect in the application of space microsatellite electrical source of power.
The copper indium gallium selenium solar cell (CIGS) prepared by the present invention is of many uses in life, can be used for traffic railway signal lamp, Traffic alarm light, street lamp, and battery charging equipment etc. brings many facilities to our life.In addition to this it is possible to for the army and the people's household electricity such as outlying areas without electricity such as plateau, island, pastoral area, frontier sentry, such as illumination, TV, radio cassette player etc., the transmission line of electricity that cost is expensive so can be saved.
Claims (1)
1. the preparation method of a copper-indium-galliun-selenium film solar cell absorbed layer, it is characterised in that:
Film sample adopts the preparation method of magnetically controlled DC sputtering and rf magnetron sputtering to obtain in JGP-450 type magnetron sputtering deposition system, the high-purity 99.99% CIGS quaternary alloy target of sputtering target material respectively diameter 50.9mm, the high-purity 99.99% metal molybdenum target of thickness 3mm and diameter 50.9mm, thick 3mm, using the length of side be 2.5cm, thickness be 1mm square Soda-lime glass as substrate, before putting soda-lime glass into chamber, first with acetone ultrasonic cleaning 20min, again with ethanol ultrasonic cleaning 5min, and dried up；The base vacuum of experiment is 4.0 × 10-4Pa, before deposition Mo thin film, carries out bias and cleans 15min substrate, and air pressure during cleaning is 2.0Pa, biases as-400V；In the process of deposition thin film, substrate constantly rotates to improve the uniformity of thin film；Under room temperature, the method utilizing magnetically controlled DC sputtering deposits the Mo back electrode that 900nm is thick on the glass substrate, the method adopting bilayer sputtering, under the noble gas argon of 1.2Pa, first sputter 4min, 36min is sputtered again under the air pressure of 0.4Pa, afterwards again by the method for rf magnetron sputtering, it is being coated with the deposition on glass CIGS thin film of Mo back electrode by sputtering CIGS quaternary alloy target under the air pressure of 0.8Pa, thickness is 1500nm, in sputter procedure, power is 100w, base reservoir temperature is 630 DEG C, afterwards with the cadmium sulfide cushion that the method sputtering 50nm of rf magnetron sputtering is thick on CuInGaSe absorbed layer, on cadmium sulfide cushion, the thick zinc oxide Window layer mixing aluminum of ZnO and 500nm thick for 50nm is sputtered successively again by the method for rf magnetron sputtering, afterwards with the Al electrode that the method sputtering 1000nm of magnetically controlled DC sputtering is thick, so far copper indium gallium selenium solar cell one piece complete is obtained.
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| CN104134708B (en) * | 2014-08-13 | 2016-02-17 | 北京大学 | The method of the ohmic contact of Copper Indium Gallium Selenide and molybdenum and the preparation method of solar cell |
| CN104805407B (en) * | 2015-04-28 | 2017-05-31 | 清华大学 | Sputtering target and preparation method thereof |
| CN106129188B (en) * | 2016-09-08 | 2017-08-08 | 京东方科技集团股份有限公司 | Thin-film solar cells and preparation method thereof |
| CN106558650B (en) * | 2016-12-07 | 2019-08-13 | 北京科技大学 | A kind of preparation method of flexible copper indium gallium selenide/perovskite lamination solar cell |
| CN108511328B (en) * | 2018-05-10 | 2020-10-02 | 河南科技大学 | Double-layer molybdenum film, preparation method thereof and thin-film solar cell |
| CN109273540A (en) * | 2018-11-29 | 2019-01-25 | 中建材蚌埠玻璃工业设计研究院有限公司 | Copper-indium-galliun-selenium film solar cell electrode and preparation method thereof |
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| CN102154622A (en) * | 2010-12-06 | 2011-08-17 | 电子科技大学 | Method for preparing copper-indium-gallium-selenium thin film serving as light absorbing layer of solar cell |
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| CN102154622A (en) * | 2010-12-06 | 2011-08-17 | 电子科技大学 | Method for preparing copper-indium-gallium-selenium thin film serving as light absorbing layer of solar cell |
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| Title |
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| Fabrication of Cu（In，Ga）Se2 thin films by sputtering from a single quaternary chalcogenide target;J.H.Shi ET AL;《Progress in Photovoltaics: Research and Applications》;20110525;第19卷(第2期);第160-164页 * |
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