CN100466298C - Method for manufacturing absorber layers for solar cell - Google Patents

Method for manufacturing absorber layers for solar cell Download PDF

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CN100466298C
CN100466298C CNB2004800213888A CN200480021388A CN100466298C CN 100466298 C CN100466298 C CN 100466298C CN B2004800213888 A CNB2004800213888 A CN B2004800213888A CN 200480021388 A CN200480021388 A CN 200480021388A CN 100466298 C CN100466298 C CN 100466298C
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CN1826697A (en
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崔寅焕
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In-Solar Tech Co Ltd
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    • E—FIXED CONSTRUCTIONS
    • E05—LOCKS; KEYS; WINDOW OR DOOR FITTINGS; SAFES
    • E05B—LOCKS; ACCESSORIES THEREFOR; HANDCUFFS
    • E05B49/00—Electric permutation locks; Circuits therefor ; Mechanical aspects of electronic locks; Mechanical keys therefor
    • E—FIXED CONSTRUCTIONS
    • E05—LOCKS; KEYS; WINDOW OR DOOR FITTINGS; SAFES
    • E05B—LOCKS; ACCESSORIES THEREFOR; HANDCUFFS
    • E05B9/00—Lock casings or latch-mechanism casings ; Fastening locks or fasteners or parts thereof to the wing
    • E05B9/08—Fastening locks or fasteners or parts thereof, e.g. the casings of latch-bolt locks or cylinder locks to the wing
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/541—CuInSe2 material PV cells

Abstract

The present invention relates to a process for producing CuInSe<SUB>2 </SUB>and CuIn<SUB>1X</SUB>Ga,Se<SUB>2 </SUB>thin films used as an absorption layer for a solar cell such that they have a structure near to chemical equivalence ratio. The present invention provides a process for producing a thin film for a solar cell, comprising forming an InSe thin film on a substrate by Metal Organic Chemical Vapor Deposition using a [Me2In-(muSeMe)]<SUB>2 </SUB>precursor; forming a Cu<SUB>2</SUB>Se thin film on the InSe thin film by Metal Organic Chemical Vapor Deposition using a (hfac)Cu(DMB) precursor, and forming a CuInSe<SUB>2 </SUB>thin film on the Cu<SUB>2</SUB>Se thin film by Metal Organic Chemical Vapor Deposition using a [Me<SUB>2</SUB>In-(muSeMe)]<SUB>2 </SUB>precursor. Further, the process may further comprise forming a CuIn<SUB>1</SUB>,Ga,Se<SUB>2 </SUB>thin film on the CuInSe<SUB>2 </SUB>thin film by Metal Organic Chemical Vapor Deposition using a [Me2Ga-(muSeMe)]<SUB>2 </SUB>precursor.

Description

The manufacture method of solar battery obsorbing layer
Technical field
The invention relates to a kind of manufacture method of solar battery obsorbing layer, make CuInSe about a kind of use MOCVD more specifically 2And CuIn 1-xGa xSe 2The method of film, the formation of described film approach stoichiometric ratio (chemical equivalence ratio).
Background technology
CuInSe 2(being hereinafter referred to as " CIS ") or CuIn 1-xGa xSe 2Triple films of (being hereinafter referred to as " CIGS ") are recently by the semiconducting compound of active research.
Different with the solar cell of traditional use silicon, the thickness of this CIS based thin film solar cell can be made less than 10 microns, even and long-time use also have stable performance.In addition, the energy conversion rate of having determined the CIS based thin film solar cell by test is better than other solar cell up to 19%, therefore its commercialization is become can replace silicon low price efficiently solar cell be very promising.
About this point, reported the method for various manufacturing CIS films recently.For example, US4523051 discloses a kind of method, and this method is the metal element of vapour deposition simultaneously under vacuum atmosphere.Yet this method is used expensive effusion cell (effusion cell), and therefore for large-scale production and the big area of realization, this method is uneconomic.US 4,798, and 660 disclose another method, and this method is at gas atmosphere that contains selenium such as H 2Se is heating and selenizing (selenize) Cu-In precursor down.Yet, H 2Se gas is very high to the toxicity of human body, is dangerous in the large-scale production of CIS film therefore.Also proposed other method such as electrodeposition process, molecular beam epitaxy method (molecular beam epitaxy) etc., but these method costs are high or only be suitable for laboratory scale, therefore are unsuitable for the large-scale production of CIS film.
Therefore, in order to realize the large-scale production of high-quality CIS film, most preferably use the metal organic chemical vapor deposition (Metal Organic Chemical VaporDeposition below is called " MOCVD ") that is widely used in conventional semiconductor technology.
Yet, MOCVD be a kind of can be in semiconductor industry the vague generalization technology of low-cost production high-quality thin film, but run into when being to use conventional MOCVD technology to produce the CIS solar cell and the high problem relevant of production cost, make to be difficult to the large-scale production high-quality thin film with complex process.
In order to generate CIS or CIGS film, conventional method comprises that sputter wants the molybdenum of vapour deposition to the glass baseplate, the base material of using used as film former then.Yet glass baseplate does not have pliability, therefore has a problem, and promptly glass baseplate need can not be used to the occasion of Free Transform.
Summary of the invention
Therefore, finished the present invention based on the problems referred to above, an object of the present invention is to provide the method that a kind of MOCVD of use makes CIS and CIGS film, the formation of described film approaches stoichiometric ratio.
Another object of the present invention provides the method that a kind of MOCVD of use makes used for solar batteries CIS or CIGS film, and the preparation technology of this method is simple and can carry out large-scale production at low cost.
Another purpose of the present invention provides a kind of method of making used for solar batteries CIS or CIGS film, and this method is littler and environmental friendliness more to the human injury.
But a further object of the present invention provides a kind of manufacturing Free Transform or the used for solar batteries CIS of bending or the method for CIGS film.
Description of drawings
In conjunction with the accompanying drawings, by the following detailed description, can more be expressly understood above and other objects of the present invention, feature and other advantage.Wherein:
Fig. 1 describes briefly according to first embodiment of the invention and makes CuInSe 2The technological process of film;
XRD (X-ray diffraction) result's of the InSe film that Fig. 2 generates according to the present invention for expression chart;
The Cu that Fig. 3 generates according to the present invention for expression 2The XRD of Se film (X-ray diffraction) result's chart;
The CuInSe that Fig. 4 generates according to the present invention for expression 2The XRD of film (X-ray diffraction) result's chart;
Fig. 5 describes briefly according to second embodiment of the invention and makes CuIn 1-xGa xSe 2The technological process of film;
The CuIn that Fig. 6 generates according to the present invention for expression 1-xGa xSe 2The XRD of film (X-ray diffraction) result's chart;
Fig. 7 is a chart, is illustrated in the CuIn that generates according to the present invention 1-xGa xSe 2In the film, lattice constant 2a and c are with the variation of [Ga]/[In+Ga] ratio;
Fig. 8 is a chart, the CuInSe that expression forms according to the present invention 2The proportion of composing of film;
Fig. 9 is a chart, the CuIn that expression forms according to the present invention 1-xGa xSe 2The proportion of composing of film;
Figure 10 to Figure 14 is respectively the CuIn that forms according to the present invention 1-xGa xSe 2The SEM image of film sample A-E.
Embodiment
Now describe the manufacture method of the CIS or the CIGS film of the preferred embodiment for the present invention in conjunction with the accompanying drawings in detail.
Fig. 1 describes the technological process of making the CIS film according to first embodiment of the invention briefly.
As shown in Figure 1, use the single precursor [Me that contains In and Se 2In (μ SeMe)] 2, on the base material that makes by molybdenum (Mo) material, form InSe film (step S101) by mocvd method.Me represents methyl, and μ represents that Se is connected for two keys with In.Thin and the pliable and tough base material that is made by Mo can be used as described base material, replaces conventional glass baseplate, therefore can realize the solar cell of different shape.
Then, use monovalence copper precursors (hfac) Cu (DMB), on the InSe film that forms by step S101, form Cu by mocvd method 2Se film (step S102).Hfac and DMB are respectively hexafluoroacetylacetone thing (hexafluoroacetylacetonate) and 3, and 3-dimethyl-1-butylene (3, abbreviation 3-dimethyl-1-butene).
Then, use the single precursor [Me that contains In and Se 2In (μ SeMe)] 2, by mocvd method at the Cu that forms by step S102 2Form CuInSe on the Se film 2Film (step S103).Be used to form CuInSe 2Precursor [the Me of film 2In (μ SeMe)] 2With used identical of step S101.
In the present invention, the device that is used for film former is a low-pressure MOCVD equipment.The used low-pressure MOCVD equipment of the present invention is equipped with a plurality of bubblers (bubbler), and described bubbler contains precursor as (hfac) Cu (DMB), [Me 2In-(μ SeMe)] 2[Me 2Ga-(μ SeMe)] 2Therefore, use according to the order of sequence and contain the bubbler of precursor separately, can in single technology, prepare the CIGS film.
Fig. 2 is illustrated in the XRD result of the InSe film of step S101 generation.Fig. 2 shows that the structure of β-InSe structure InSe film fine and that form shows good growing amount.
Fig. 3 is illustrated in the Cu that step S102 generates 2The XRD result of Se film.As can be seen, initial InSe film has become Cu 2The Se film.(X-ray fluorescencespectroscopy XRF) analyze to confirm not detect In and film fully by Cu to the X-ray fluorescence spectrum 2Se makes.That is, when using monovalence copper precursors (hfac) Cu (DMB), when generating copper by mocvd method on the InSe film, initial In has disappeared and has been substituted by Cu, therefore shows that InSe changes Cu into 2Se.
Fig. 4 is illustrated in the CuInSe that step S103 generates 2The XRD result of film.As can be seen, the CuInSe of generation 2The XRD figure shape of film and known CuInSe 2Monocrystal is consistent.The film that generates demonstrates the single phase with tetragonal lattice.
Fig. 5 describes briefly according to second embodiment of the invention and makes CuIn 1-xGa xSe 2The technological process of film.
As shown in Figure 5, step S201-S203 is identical with above-mentioned CIS film preparation process.Use contains the precursor [Me of Ga and Se 2Ga (μ SeMe)] 2, by mocvd method at the CuInSe that forms by step S203 2Form CuIn on the film 1-xGa xSe 2Film (step S204).[Me 2Ga (μ SeMe)] 2Be precursor substance, wherein [Me 2In (μ SeMe)] 2In In replace by Ga.
For the physical property relevant with the Ga proportion of composing of the CIGS film of analyzing generation with In, regulate the proportion of composing of In and Ga by the time that changes vapour deposition in step 204, preparation has 5 samples (A, B, C, D and E) of different proportion of composing.At CuIn 1-xGa xSe 2In the film, the use X-ray fluorescent spectrographic determination x value i.e. proportion of composing of [Ga]/[In+Ga] is respectively 0,0.062,0.19,0.34 and 0.96.
Fig. 6 represents the CuIn that generates in the second embodiment of the invention 1-xGa xSe 2The XRD result of film A, B, C, D and E.According to the proportion of composing of [Ga]/[In+Ga], the position at peak converts an angle (2 θ) that increases to.
Fig. 7 is a chart, and expression lattice constant 2a and c are with the i.e. variation of [Ga]/[In+Ga] ratio of x value.As shown in Figure 7, linearity reduces along with the increase of x value for lattice constant 2a and c.Therefore, lattice constant 2a and c are respectively 0.329 and 0.602 with the rate of change of [Ga]/[In+Ga] ratio, the significant difference between showing.In addition, CuInSe 2The lattice constant of film
Figure C200480021388D0008100102QIETU
With
Figure C200480021388D0008100109QIETU
The result who obtains with Gryunova is consistent.The CuIn that is obtaining 1-xGa xSe 2In the film, the peak of x is 0.96 (sample E).In this case, lattice constant
Figure C200480021388D0008100127QIETU
With
Figure C200480021388D0008100137QIETU
Lattice constant with the Gryunova report With
Figure C200480021388D0008100154QIETU
Be consistent.
Fig. 8 and Fig. 9 represent the CIS film that forms according to first embodiment of the invention respectively and the proportion of composing of the CIGS film that forms according to second embodiment of the invention.Be connected (In+Ga) of Groenink and Janse definition 2Se 3And Cu 2The line of Se and vertical line represent not have molecularity (non-molecularity) and no stoichiometric relationship (non-stoichiometry) respectively.The circle of triangle center is that proportion of composing is the point of Cu:In:Se=1:1:2.
Round dot among Fig. 8 is represented a plurality of CuInSe by Experiment Preparation 2Sample, as can be seen, the Cu:In:Se ratio of the CIS film that generates according to the present invention is near 1:1:2.In addition, each round dot B, C, D and E among Fig. 9 represents that respectively [Ga]/[In+Ga] proportion of composing is 0.062,0.19,0.34 and 0.96 sample, therefore as can be seen, even when generating the CIGS film, change the ratio of In and Ga, Cu:(In, Ga): Se also almost remains on 1:1:2.
Below as can be seen, CIS film and the CIGS film preparation that generates according to the present invention must have very approaching stoichiometric ratio.The high-quality thin film that therefore, can have the expection equivalent proportion without difficulty simply by the MOCVD mass preparation.In addition, even also can obtain Cu:In (Ga) when adjusting the ratio of [Ga]/[In+Ga] as required: Se is near the film of 1:1:2.
Figure 10 to Figure 14 is respectively the SEM image of the CIGS film sample A, B, C, D and the E that form according to the present invention.All samples all shows the crystal growth of stablizing crystal grain, shows that no matter how the ratio of [Ga]/[In+Ga] is formed crystal growth is all carried out well.
In addition, according to the 3rd execution mode of the present invention, by using [Me 2In-(μ TeMe)] 2Or [Me 2In-(μ SMe)] 2Replace being used as among the second execution mode step S204 [Me2Ga-(the μ SeMe)] of precursor 2, a part of Se can be replaced by Te or S, consequently, obtain film CuIn (Se, S) or CuIn (Se, Te).
Although the present invention is described in the mode of preferred implementation, technical elements of the present invention is not limited to this.That is to say, even as the used for solar batteries film, to CuIn 1-xGa xSe 2(supposing 0≤x≤1) and CuIn (Se, S) preparation method of film is described, but the I-III-VI that these films just are made up of the I that is selected from the periodic table of elements, III and VI family element 2Several examples of compound.
Some special examples are described below.At first,, use the single precursor that contains III family and VI family element, form the III-VI film by Metalorganic Chemical Vapor Deposition as the first step.III family element comprises that all belong to the element of periodic table of elements 1II family, for example In, Ga or Al; VI family element comprises that all belong to the element of period of element Table VI family, for example Se, S or Te.Therefore the III-VI film that generates is InSe, GaSe, AlSe, InS, GaS, AlS, InTe, GaTe or AlTe.
In second step, use the precursor (comprising monovalence or divalence precursor) that contains I family metal (for example Ag or Cu), on the III-VI film, form I by Metalorganic Chemical Vapor Deposition 2-VI film.I family element comprises that all belong to the element of period of element Table I family, for example Cu or Ag.Therefore, the I of generation 2-VI film is Cu 2Se, Cu 2S, Cu 2Te, Ag 2Se, Ag 2S or Ag 2Te.
In the 3rd step, use the single precursor contain III and VI family element, by Metalorganic Chemical Vapor Deposition at I 2Form I-III-VI on the-VI film 2Therefore film has been finished according to used for solar batteries film of the present invention.At this, the used element of III and the VI family element and the first step is identical.
In addition,, can use the single precursor of the other element that contains III and VI family in the 4th step, by Metalorganic Chemical Vapor Deposition at I-III-VI 2Prepare I-III-VI on the film 2The solid solution semiconducting compound of film.In this case, different at used element of this used III and VI family element and the first step and the 3rd step.Therefore, the film that obtains comprises CuIn 1-xGa xSe 2, CuIn 1-xAl xSe 2, CuGa 1-xAl xSe 2, AgIn 1-xGa xSe 2, AgIn 1-xAl xSe 2, AgIn 1-xGa xSe 2, CuIn (Se, S) 2, CuGa (Se, S) 2, AgIn (Se, S) 2, AgGa (Se, S) 2, CuIn (Se, Te) 2, CuGa (Se, Te) 2, AgIn (Se, Te) 2, AgGa (Se, Te) 2, CuIn (S, Te) 2, CuGa (S, Te) 2, AgIn (S, Te) 2And AgGa (S, Te) 2
Therefore, technical elements of the present invention also ought be understood that to disclose a kind of preparation I-III-VI 2The method of compound and solid solution thereof.
The single precursor of III of containing of the present invention and VI family element is not limited to employed [Me in the present invention first, second and the 3rd execution mode 2(III)-(μ (VI) Me)] the type precursor skilled in the art will recognize that the precursor that can use other type of not enumerating in the present invention significantly.In brief, have similar chemical property,, also can access similar result even therefore use different precursors owing to belong to periodic table of elements element of the same clan.Similarly, the precursor that contains copper is not limited to (hfac) Cu (DMB).
Industrial usability
Can obviously find out from the above description, according to the present invention, by simply controlling the formation condition of semiconducting compound, can make the high-quality used for solar batteries CuIn with expection equivalent proportion1-xGa xSe 2Film.
And, according to the present invention, by simple manufacturing process, can realize used for solar batteries CuIn1-NGa xSe 2The low-cost large-scale production of film.
In addition, according to the present invention, by using the relatively low compound of toxicity as making used for solar batteries CuIn1-NGa xSe 2The precursor of film can make safer, the environmental friendliness more of production technology.
Further, the present invention uses has flexible metal as base material, so solar cell Shape can change as required freely, has therefore enlarged application.
Although for purpose of description discloses preferred implementation of the present invention, but it will be appreciated by those skilled in the art that under the situation that does not depart from the disclosed the scope and spirit of the present invention of claims of enclosing, can make various variations, interpolation and replacement.

Claims (10)

1, a kind of manufacturing I-III-VI 2The method of film, this method comprises:
The first step: use the single precursor that contains III family and VI family element, on base material, form the III-VI compound film by Metalorganic Chemical Vapor Deposition;
Second step: use the precursor that contains I family metal, on the III-VI compound film, form I by Metalorganic Chemical Vapor Deposition 2-VI compound film; And
The 3rd step: use the single precursor contain III and VI family element, by Metalorganic Chemical Vapor Deposition at I 2Form I-III-VI on the-VI compound film 2Compound film.
2, the method for claim 1, this method also comprised for the 4th step: use the single precursor that contains III and VI family element, by the I-III-VI of Metalorganic Chemical Vapor Deposition formation in the 3rd step 2Prepare I-III-VI on the compound film 2Compound film, wherein to go on foot used element different for used III family element of the 4th step and the first step and the 3rd.
3, the method for claim 1, this method also comprised for the 4th step: use the single precursor that contains III and VI family element, by the I-III-VI of Metalorganic Chemical Vapor Deposition formation in the 3rd step 2Prepare I-III-VI on the compound film 2Compound film, wherein to go on foot used element different for used VI family element of the 4th step and the first step and the 3rd.
4, as any described method among the claim 1-3, wherein the first step and used precursor of the 3rd step are [Me 2In-(μ SeMe)] 2
5, as any described method among the claim 1-3, wherein second the step used precursor be (hfac) Cu (DMB).
6, method as claimed in claim 2, wherein the 4th the step used precursor be [Me 2Ga-(μ SeMe)] 2
7, method as claimed in claim 2, the wherein I-III-VI that forms in the 4th step 2Compound film is for being selected from by CuIn 1-xGa xSe 2, CuIn 1-xAl xSe 2, CuGa 1-xAl xSe 2, AgIn 1-xGa xSe 2, AgIn 1-xAl xSe 2And AgIn 1-xGa xSe 2In the group of being formed.
8, method as claimed in claim 3, the wherein I-III-VI that forms in the 4th step 2Compound film for be selected from by CuIn (Se, S) 2, CuGa (Se, S) 2, AgIn (Se, S) 2, AgGa (Se, S) 2, CuIn (Se, Te) 2, CuGa (Se, Te) 2, AgIn (Se, Te) 2, AgGa (Se, Te) 2, CuIn (S, Te) 2, CuGa (S, Te) 2, AgIn (S, Te) 2And AgGa (S, Te) 2In the group of being formed.
9, a kind of method of making solar battery obsorbing layer, this method comprises:
Use contains the single precursor of In and Se, forms the InSe film by Metalorganic Chemical Vapor Deposition on base material;
Use the Cu precursor, on the InSe film, form Cu by Metalorganic Chemical Vapor Deposition 2The Se film; And
Use contains the single precursor of In and Se, by Metalorganic Chemical Vapor Deposition at Cu 2Form CuInSe on the Se film 2Compound film.
10, method as claimed in claim 9, this method also comprise uses the single precursor contain Ga and Se, by Metalorganic Chemical Vapor Deposition at CuInSe 2Form CuIn on the compound film 1-xGa xSe 2The step of film.
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