CN101771099A - Preparation method of copper-indium-gallium-selenium semiconductor film - Google Patents
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Abstract
The invention relates to a preparation method of copper-indium-gallium-selenium semiconductor film. A Mo layer is sputtered on a rigid or flexible underlay through the vacuum magnetic-control sputtering method of the known technology; Cu, In and Ga are respectively sputtered on the Mo layer, a prefab layer reaction substrate is prepared, and then the prefab layer reaction substrate is encapsulated, heated and cooled to generate the copper-indium-gallium-selenium semiconductor film. Because the reactant and the substrate sputtered with a metallic prefab film are put in an independent reaction container protected by high-purity inert gasses and are heated wholly, the method can maintain sufficient selenium atmosphere; ensure the granularity of the selenium atmosphere to be reduced; realize good repetitiveness, few uncontrollable factors, little loss of raw materials, proper control of gallium impurity, benefit for selenium chemical reaction, low demand for equipment, less consumption of reactant and high photoelectric conversion efficiency, more applicable to industrial production.
Description
Technical field
The invention belongs to the thin film solar cell technical field of material, particularly relate to a kind of preparation method of copper-indium-gallium-selenium semiconductor film.
Background technology
The basic structure of Copper Indium Gallium Selenide CIGS thin film solar cell is: substrate/metal back electrode/light absorbing zone/resilient coating/Window layer/transparent electrode layer/metal gate-shaped electrode/antireflection layer, wherein as the copper-indium-gallium-selenium semiconductor film of light absorbing zone to solar cell performance decisive role.
(CIGS CIGSS) as the thin film solar cell of light absorbing zone, is considered to one of compound battery that has very much development prospect to the compound semiconductor Copper Indium Gallium Selenide of yellow copper structure.CIGS thin-film is a kind of direct gap semiconductor material, and its key property is that energy gap can be regulated by the Ga incorporation.CIGS material energy gap can change between 1.04eV～1.65eV, very be fit to adjust and optimize the energy gap of material, make the CIGS thin film solar cell have splendid optical energy gap, in thin film solar cell, the visible absorption coefficient of CIGS thin-film material reaches 10
5/ cm has realized the battery structure filming, has battery low cost of manufacture, photoelectric conversion efficiency height, strong, the steady performance of capability of resistance to radiation simultaneously.
At present, the preparation method of CIGS film mainly contains multi-source and steams selenizing method after method and the sputter altogether.
Multi-source steaming method altogether has dual mode: a kind of is a step coevaporation method, is about to Cu, In, Ga, Se or comprises the S concurrently vapour depositing, forms CIGS or CIGSS film; Another kind is three step coevaporation methods, because adopt at first in American National regenerative resource laboratory (NREL), so also be called the NREL method, this method divided for three steps carried out, at first be hydatogenesis In, Ga and Se, then hydatogenesis Cu and Se, at last in order to make III family element excessive, hydatogenesis In, Ga and Se once more.It is wayward to selenium or sulfur vapor pressure that multi-source steams method altogether, the equipment complexity.
The selenizing method is to adopt vacuum magnetic-control sputtering equipment deposited copper indium gallium (Cu-In-Ga is called for short CIG) on substrate to form the metal preformed layer after the sputter, and selenizing forms the CIGS film in Se atmosphere then.Substitute selenium with sulphur equally, also can carry out the thermo-chemical treatment of the selenium method of fractional steps behind sulphur behind vulcanization reaction or the first selenium or the first sulphur, final CIGS or the CIGSS compound semiconductor film that satisfies the stoicheiometry requirement that generate.In this method selenizing process, both available H
2Se or H
2S gas, also available solid-state Se.Wherein adopt H
2Se or H
2The CIGS compound semiconductor film of S gas preparation, the CIGS thin film solar cell conversion efficiency of preparing is higher, but H
2Se or H
2S all is hypertoxic gas, and inflammable, and is very high to the requirement of preserving and operate, and therefore had a strong impact on the practical application of this kind method.Chinese patent CN1719625 discloses the selenizing of employing Solid State Source or sulfuration method prevapourising selenizing or sulfuration, promptly earlier at metal preformed layer surface evaporation last layer selenium or sulphur, again by tungsten halogen lamp irradiation heating of metal preformed layer, preparation CIGS absorbed layer, the consumption of this method reactant is big, and is wayward.
Summary of the invention
The present invention is for solving problems of the prior art, a kind of no poison gas is provided, equipment is simple, reactant consumption is little, handling safety, control is prepared into the electricity conversion height of battery, and is suitable for the preparation method of a kind of copper-indium-gallium-selenium semiconductor film of suitability for industrialized production easily.
The present invention for the technical scheme that solves the technical problem employing that exists in the known technology is:
A kind of preparation method of copper-indium-gallium-selenium semiconductor film, adopt known technology vacuum magnetic-control sputtering method sputter Mo layer on rigidity or flexible substrate earlier, difference sputter Cu, In, Ga on the Mo layer, the preformed layer of making reaction substrate is characterized in comprising following preparation process:
(1) encapsulation: all pack in the container of an opening but preformed layer is reacted substrate and reactant, preformed layer reaction substrate and reactant keep certain distance in container, container is carried out vacuumizing below the 5Pa, put into pipeline behind the container closure, pipe ends is sealed, charge into inert gas to pipeline then, make the interior pressure of pipeline near an atmospheric pressure;
(2) heat up: by magnetic drive device pipeline integral body is put into temperature control furnace, be rapidly heated, preformed layer reaction substrate and reactant are reacted;
(3) cooling: after reaction is finished, pipeline integral body is carried out fast cooling, pipeline is vacuumized, vacuum degree reach 10Pa following after, once more to the pipeline processing of lowering the temperature, treat that temperature is reduced to room temperature after, take out substrate, promptly prepare copper-indium-gallium-selenium semiconductor film of the present invention.
The present invention can also adopt following technical measures:
The preparation method of described copper-indium-gallium-selenium semiconductor film is characterized in: reactant is Se in described (1), and described container is high-temperature glass tube or quartz ampoule or metal tube, and thickness of pipe wall is less than 2mm; Described inert gas is high-purity argon gas or high pure nitrogen; Before pipeline charges into high purity inert gas, high purity inert gas is carried out processed.
The preparation method of described copper-indium-gallium-selenium semiconductor film, be characterized in: be rapidly heated in described (2) for: earlier at the uniform velocity be warmed up to 200 ℃ with 50 ℃/min, be warmed up to more than 430 ℃ with 100 ℃/min speed again, temperature arrives 555 ℃, timing keeps more than the 13min, and preformed layer reaction substrate and reactant fully react.
The preparation method of described copper-indium-gallium-selenium semiconductor film, be characterized in: fast cooling is in described (3): by sectional temperature-controlled reaction vessel integral body is cooled to 250 ℃ after, after being evacuated to below the 10Pa with mechanical pump to pipeline, to be placed on the recirculated water place away from the pipeline integral body of reaction substrate one end and reduce to room temperature, and make selenium or selenium steam at first in the cold junction condensation.
The preparation method of described copper-indium-gallium-selenium semiconductor film is characterized in: described high purity inert gas dehydration is that a dehydrating tower is housed between high purity inert gas and flow quantity control instrument.
The preparation method of described copper-indium-gallium-selenium semiconductor film is characterized in: preformed layer reaction substrate and the distance of reactant in container are 10cm～15cm in described (1).
The preparation method of described copper-indium-gallium-selenium semiconductor film is characterized in: closed at both ends is the manual or electronic baffle valve of high vacuum in described (1).
The preparation method of described copper-indium-gallium-selenium semiconductor film is characterized in: pipeline charges into inert gas for to charge into to pipeline by flow quantity control instrument in described (1).
The preparation method of described copper-indium-gallium-selenium semiconductor film, be characterized in: magnetic drive device is to adopt the manual or electronic temperature range of limit switch control reacting pipe in vacuum tube that add in described (2), it is to finish by a quartz pushrod that reacting pipe moves in vacuum tube, one end of this quartz pushrod adopts the structure of the collar that it is connected with an end of reacting pipe, the other end of quartz pushrod is made into the pipeline of sealing, and in pipeline, place one section pig iron, be used with the high strong magnet of slideway outside.
Advantage that the present invention has and good effect: owing to have the substrate of metal prefabricated membrane to be placed on one independently in the reaction vessel reactant and sputter; reaction vessel is protected by high purity inert gas; carry out the integral body heating; keep sufficient selenium atmosphere; the granularity of the selenium atmosphere that is evaporated is reduced; good reproducibility; uncontrollable factor is few; the raw material loss is little, can suitably control the doping of gallium, helps selenylation reaction; and to equipment require low; reactant consumption is little, keeps higher photoelectric conversion efficiency, is more suitable in suitability for industrialized production.
Description of drawings
Fig. 1 is object space schematic diagram among the preparation method of copper-indium-gallium-selenium semiconductor film of the present invention.
Among the figure, the 1-reactant, 2-reacts substrate, 3-container, 4-pipeline.
Embodiment
For further understanding summary of the invention of the present invention, characteristics and effect, exemplify following examples now, and conjunction with figs. is described in detail as follows:
Embodiment 1:
Adopt the thick metal M o of magnetron sputtering deposition 1 μ m on the lime glass common receiving, adopting atomic ratio again is two targets that CuGa alloys target that 0.9: 1 CuIn alloys target and atomic ratio are 0.6: 1 constitutes, difference sputter 0.6 μ m-1.0 μ m copper indium gallium metal preformed layer on the Mo film, the reaction substrate 2 of formation copper indium gallium metal preformed layer.Volume according to container 3 utilizes log=A-B/ (T+C); The PV=NRT equation calculates the weight of reactant 1.Reaction substrate 2 and solid-state selenium Se reactant 1 are kept 10cm～15cm apart from the high-temperature glass tube that is placed on as container 3, with mechanical pump container 3 is vacuumized, vacuum degree in container 3 reaches below the 5Pa, with container 3 sealings, put into pipeline 4 then, adopt the manual or electronic baffle valve method of high vacuum with pipeline 4 sealed at both ends after, in pipeline 4, charge into high-purity argon gas with flow quantity control instrument, make the interior pressure of pipeline 4 near an atmospheric pressure; Before high-purity argon gas charges into pipeline 4, a cover is housed between high purity inert gas and flow quantity control instrument earlier adopts the silica gel dehydrating tower to dewater, prevented that steam from entering reaction vessel 3, and influence finally is prepared into the performance of copper-indium-gallium-selenium semiconductor film.The pipeline 4 that container 3 is housed is put into temperature control furnace, by the manual or electronic temperature range of limit switch control reacting pipe in vacuum tube that add, it is to finish by a quartz pushrod that reacting pipe moves in vacuum tube, one end of this quartz pushrod adopts the structure of the collar that it is connected with an end of reacting pipe, the other end of quartz pushrod is made into the pipeline of sealing, and in pipeline, place one section pig iron, be used with the high strong magnet of slideway outside.This magnetic drives mode makes the interior temperature of stove at the uniform velocity be warmed up to 200 ℃ with 50 ℃/min, kept 5 minutes, be warmed up to more than 430 ℃ with 100 ℃/min speed again, keep more than the 15min after temperature arrives 555 ℃, reaction substrate 2 and solid-state selenium Se reactant 1 are fully reacted; After reaction finishes, adopt above-mentioned magnetic drives mode that the pipeline 4 first fast coolings to 250 ℃ of container 3 will be housed by sectional temperature-controlled method again, with mechanical pump pipeline 4 is vacuumized, make vacuum degree in the pipeline 4 reach 10Pa following after, to be placed in the recirculated water earlier away from the pipeline 4 that reaction substrate 2 one ends are equipped with container 3 again, one end temperature of container is reduced, make selenium or selenium steam at first in the cold junction condensation, avoid selenium steam condensation on absorbed layer, then integral body is reduced to room temperature, take out substrate, promptly make copper-indium-gallium-selenium semiconductor film as the solar cell absorbed layer.Zhi Bei Cu (In, Ga) Se on this basis
2The open circuit voltage of solar cell is 403mv, and short-circuit current density is 34.58mA/cm
2, fill factor, curve factor is 59.1%, electricity conversion is 7.1%.
Embodiment 2:
On titanium is thin, adopt the thick metal M o of magnetron sputtering deposition 1 μ m, adopting atomic ratio again is two targets that CuGa alloys target that 0.9: 1 CuIn alloys target and atomic ratio are 0.6: 1 constitutes, difference sputter 0.6 μ m-1.0 μ m copper indium gallium metal preformed layer on the Mo film, the reaction substrate 2 of formation copper indium gallium metal preformed layer.Volume according to container 3 utilizes log=A-B/ (T+C); The PV=NRT equation calculates the weight of reactant 1.Reaction substrate 2 and solid-state selenium Se reactant 1 are kept 10cm～15cm apart from the high-temperature glass tube that is placed on as container 3, with mechanical pump container 3 is vacuumized, vacuum degree in container 3 reaches below the 5Pa, with container 3 sealings, put into pipeline 4 then, adopt the manual or electronic baffle valve method of high vacuum with pipeline 4 sealed at both ends after, in pipeline 4, charge into high-purity argon gas with flow quantity control instrument, make the interior pressure of pipeline 4 near an atmospheric pressure; Before high-purity argon gas charges into pipeline 4, a cover is housed between high purity inert gas and flow quantity control instrument earlier adopts the silica gel dehydrating tower to dewater, prevented that steam from entering reaction vessel 3, and influence finally is prepared into the performance of copper-indium-gallium-selenium semiconductor film.The pipeline 4 that container 3 is housed is put into temperature control furnace, by the manual or electronic temperature range of limit switch control reacting pipe in vacuum tube that add, it is to finish by a quartz pushrod that reacting pipe moves in vacuum tube, one end of this quartz pushrod adopts the structure of the collar that it is connected with an end of reacting pipe, the other end of quartz pushrod is made into the pipeline of sealing, and in pipeline, place one section pig iron, be used with the high strong magnet of slideway outside.This magnetic drives mode makes the interior temperature of stove at the uniform velocity be warmed up to 200 ℃ with 50 ℃/min, kept 5 minutes, be warmed up to more than 430 ℃ with 100 ℃/min speed again, keep more than the 15min after temperature arrives 555 ℃, reaction substrate 2 and solid-state selenium Se reactant 1 are fully reacted; After reaction finishes, adopt above-mentioned magnetic drives mode that the pipeline 4 first fast coolings to 250 ℃ of container 3 will be housed by sectional temperature-controlled method again, with mechanical pump pipeline 4 is vacuumized, make vacuum degree in the pipeline 4 reach 10Pa following after, to be placed in the recirculated water earlier away from the pipeline 4 that reaction substrate 2 one ends are equipped with container 3 again, one end temperature of container is reduced, make selenium or selenium steam at first in the cold junction condensation, avoid selenium steam condensation on absorbed layer, then integral body is reduced to room temperature, take out substrate, promptly make copper-indium-gallium-selenium semiconductor film as the solar cell absorbed layer.Zhi Bei Cu (In, Ga) Se on this basis
2The open circuit voltage of solar cell is 404mv, and short-circuit current density is 33.28mA/cm
2, fill factor, curve factor is 57.2%, electricity conversion is 6%.
Embodiment 3:
Adopt the solid-state selenium Se reactant 1 in the solid-state reaction of Salmon-Saxl thing alternate embodiment 1, other are identical with embodiment 1, finally obtain copper indium gallium sulphur solar cell light absorbing zone.
Embodiment 4:
In embodiment 1 the solid-state selenium of reactant is replaced with solid-state selenium and sulphur, other are identical with embodiment 1, finally obtain Copper Indium Gallium Selenide sulfur solar energy light absorbed layer.
Claims (9)
1. the preparation method of a copper-indium-gallium-selenium semiconductor film, adopt known technology vacuum magnetic-control sputtering method sputter Mo layer on rigidity or flexible substrate earlier, difference sputter Cu, In, Ga on the Mo layer, the preformed layer of making reaction substrate is characterized in that comprising following preparation process:
(1) encapsulation: all pack in the container of an opening but preformed layer is reacted substrate and reactant, preformed layer reaction substrate and reactant keep certain distance in container, container is carried out vacuumizing below the 5Pa, put into pipeline behind the container closure, pipe ends is sealed, charge into inert gas to pipeline then, make the interior pressure of pipeline near an atmospheric pressure;
(2) heat up: by magnetic drive device pipeline integral body is put into temperature control furnace, be rapidly heated, preformed layer reaction substrate and reactant are reacted;
(3) cooling: after reaction is finished, pipeline integral body is carried out fast cooling, pipeline is vacuumized, vacuum degree reach 10Pa following after, once more to the pipeline processing of lowering the temperature, treat that temperature is reduced to room temperature after, take out substrate, promptly prepare copper-indium-gallium-selenium semiconductor film of the present invention.
2. according to the preparation method of the described copper-indium-gallium-selenium semiconductor film of claim 1, it is characterized in that: reactant is Se in described (1), and described container is high-temperature glass tube or quartz ampoule or metal tube, and thickness of pipe wall is less than 2mm; Described inert gas is high-purity argon gas or high pure nitrogen; Before pipeline charges into high purity inert gas, high purity inert gas is carried out processed.
3. according to the preparation method of the described copper-indium-gallium-selenium semiconductor film of claim 1, it is characterized in that: be rapidly heated in described (2) for: earlier at the uniform velocity be warmed up to 200 ℃ with 50 ℃/min, be warmed up to more than 430 ℃ with 100 ℃/min speed again, temperature arrives 555 ℃, timing keeps more than the 13min, and preformed layer reaction substrate and reactant fully react.
4. according to the preparation method of the described copper-indium-gallium-selenium semiconductor film of claim 1, it is characterized in that: fast cooling is in described (3): by sectional temperature-controlled reaction vessel integral body is cooled to 250 ℃ after, after being evacuated to below the 10Pa with mechanical pump to pipeline, to be placed on the recirculated water place away from the pipeline integral body of reaction substrate one end and reduce to room temperature, and make selenium or selenium steam at first in the cold junction condensation.
5. according to the preparation method of the described copper-indium-gallium-selenium semiconductor film of claim 2, it is characterized in that: described high purity inert gas dehydration is that a dehydrating tower is housed between high purity inert gas and flow quantity control instrument.
6. according to the preparation method of the described copper-indium-gallium-selenium semiconductor film of claim 1, it is characterized in that: preformed layer reaction substrate and the distance of reactant in container are 10cm～15cm in described (1).
7. according to the preparation method of the described copper-indium-gallium-selenium semiconductor film of claim 1, it is characterized in that: closed at both ends is the manual or electronic baffle valve of high vacuum in described (1).
8. according to the preparation method of the described copper-indium-gallium-selenium semiconductor film of claim 1, it is characterized in that: pipeline charges into inert gas for to charge into to pipeline by flow quantity control instrument in described (1).
9. according to the preparation method of the described copper-indium-gallium-selenium semiconductor film of claim 1, it is characterized in that: magnetic drive device is to adopt the manual or electronic temperature range of limit switch control reacting pipe in vacuum tube that add in described (2), it is to finish by a quartz pushrod that reacting pipe moves in vacuum tube, one end of this quartz pushrod adopts the structure of the collar that it is connected with an end of reacting pipe, the other end of quartz pushrod is made into the pipeline of sealing, and in pipeline, place one section pig iron, be used with the high strong magnet of slideway outside.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101958371A (en) * | 2010-10-13 | 2011-01-26 | 中国科学院深圳先进技术研究院 | Device for manufacturing copper indium gallium selenium (CIGS) thin-film solar cells |
| CN102249199A (en) * | 2011-05-06 | 2011-11-23 | 桂林理工大学 | Microwave-assisted solvothermal synthesis method of I-III-VI semiconductor material nano-powder |
| CN102623571A (en) * | 2012-04-13 | 2012-08-01 | 山东大学 | Method for producing copper indium gallium diselenide (CIGS) solar battery absorption layer through evaporation method |
| CN102790123A (en) * | 2011-05-17 | 2012-11-21 | 正峰新能源股份有限公司 | Rapid-crystallization annealing furnace for selenium steam |
| CN103022243A (en) * | 2011-09-27 | 2013-04-03 | 绿阳光电股份有限公司 | Thin Film Solar Cell Manufacturing System |
| CN103343323A (en) * | 2013-07-03 | 2013-10-09 | 深圳先进技术研究院 | Preparation method of copper-indium-gallium-selenium film |
| CN105008583A (en) * | 2013-02-14 | 2015-10-28 | 威科仪器有限公司 | Variable-temperature material growth stages and thin film growth |
Family Cites Families (4)
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| US5730852A (en) * | 1995-09-25 | 1998-03-24 | Davis, Joseph & Negley | Preparation of cuxinygazsen (X=0-2, Y=0-2, Z=0-2, N=0-3) precursor films by electrodeposition for fabricating high efficiency solar cells |
| CN1151560C (en) * | 2002-03-08 | 2004-05-26 | 清华大学 | Copper-indium-galliun-selenium film solar cell and its preparation method |
| CN1257560C (en) * | 2003-12-05 | 2006-05-24 | 南开大学 | Method for preparing selenide or sulfide semiconductor film material of copper-indium-gallium |
| CN100413097C (en) * | 2005-06-03 | 2008-08-20 | 清华大学 | Process for preparing Cu-In-Ga-Se or Cu-In-Ga-S film solar battery obsorbing layer |
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- 2008-12-30 CN CN200810154678XA patent/CN101771099B/en not_active Expired - Fee Related
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| CN101958371A (en) * | 2010-10-13 | 2011-01-26 | 中国科学院深圳先进技术研究院 | Device for manufacturing copper indium gallium selenium (CIGS) thin-film solar cells |
| CN102249199A (en) * | 2011-05-06 | 2011-11-23 | 桂林理工大学 | Microwave-assisted solvothermal synthesis method of I-III-VI semiconductor material nano-powder |
| CN102790123A (en) * | 2011-05-17 | 2012-11-21 | 正峰新能源股份有限公司 | Rapid-crystallization annealing furnace for selenium steam |
| CN103022243A (en) * | 2011-09-27 | 2013-04-03 | 绿阳光电股份有限公司 | Thin Film Solar Cell Manufacturing System |
| CN102623571A (en) * | 2012-04-13 | 2012-08-01 | 山东大学 | Method for producing copper indium gallium diselenide (CIGS) solar battery absorption layer through evaporation method |
| CN102623571B (en) * | 2012-04-13 | 2014-08-06 | 山东大学 | Method for producing copper indium gallium diselenide (CIGS) solar battery absorption layer through evaporation method |
| CN105008583A (en) * | 2013-02-14 | 2015-10-28 | 威科仪器有限公司 | Variable-temperature material growth stages and thin film growth |
| CN103343323A (en) * | 2013-07-03 | 2013-10-09 | 深圳先进技术研究院 | Preparation method of copper-indium-gallium-selenium film |
| CN103343323B (en) * | 2013-07-03 | 2015-12-23 | 深圳先进技术研究院 | CIGS thin-film preparation method |
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