CN103258899A - Method for preparing Cu(In1-xGax)Se2 (CIGS) absorbing layer on flexible stainless steel substrate - Google Patents
Method for preparing Cu(In1-xGax)Se2 (CIGS) absorbing layer on flexible stainless steel substrate Download PDFInfo
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- CN103258899A CN103258899A CN2012100358173A CN201210035817A CN103258899A CN 103258899 A CN103258899 A CN 103258899A CN 2012100358173 A CN2012100358173 A CN 2012100358173A CN 201210035817 A CN201210035817 A CN 201210035817A CN 103258899 A CN103258899 A CN 103258899A
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Abstract
The invention discloses a method for depositing and processing a high-photovoltaic-conversion-efficiency Cu(In1-xGax)Se2 (CIGS) absorbing layer on a flexible stainless steel substrate. According to the method, an improved three-step coevaporation method and a Na mixing processing CIGS absorbing layer method are adopted. The improved three-step coevaporation method comprises the steps of firstly, depositing a thin CuGaSe2 layer on the surface of Mo, then adopting steps similar to first two steps of the three-step coevaporation method, namely respectively depositing a (InGa)2Se3 precast layer, Cu(InGa)Se2 rich in a copper stoichiometric ratio, and twice-phase CuxSe, then etching the twice-phase CuxSe through a Br2 water solution, finally depositing a In2Se3 film on the surface of an etched sample in an evaporated mode, and carrying out annealing processing on the In2Se3 film. The Na mixing processing CIGS absorbing layer method comprises the steps of depositing a Na precast layer Na2S on the surface of the In2Se2 film, and carrying out high temperature rapid annealing processing on the Na precast layer Na2S. According to the CIGS absorbing layer obtained though the method, a rear segregation of Na is generated, CuGaSe2 and MoSe2are are formed at the position of an interface of Mo/CIGS, large columnar grains are formed, and a mirror surface structure with surface poor in copper and rich in indium is formed. Therefore, a CIGS solar cell has large open-circuit voltage VOC, a filling factor FF, short circuit current JSC and good external quantum efficiency (EQE). Therefore, the high photovoltaic conversion rate of the CIGS film solar cell is ensured.
Description
One, technical field
Patent of the present invention relates to the preparation technology of photovoltaic device CIGS thin film solar cell, relate in particular at the bottom of the flexible stainless steel lining on deposition and the processing method of absorbed layer CIGS.
Two, background technology
Concerning thin film solar battery module, up to now, with Cu (InGa) Se
2(CIGS) the film solar cell of doing absorbed layer has the highest photoelectric conversion efficiency 20.3%.The flexible CIGS thin film solar battery module of lightweight has not only been widened the scope of solar cell in Ground Application, simultaneously owing to its volume to volume technology easy to use, and its cost of electricity-generating is reduced.As the critical component of CIGS thin film solar cell, the deposition processes technology of CIGS has fundamental influence to the photoelectric conversion efficiency of its photoelectric characteristic and solar cell.
The contact of the Mo/CIGS back of the body is near CIGS absorption maximum district, and back of the body contact performance serious degradation can cause absorption efficiency to reduce.Reduce first method of back of the body contact influence for using adhesion layer, increase CIGS in the tack of Mo, reduce back of the body contact resistance, increase the collection efficiency of holoe carrier; Second method makes the Ga content maximum near the absorbed layer back side, near the Ga content minimum on absorbed layer surface for using band gap gradient.Arrange degree of order increase carrier mobility by the crystallite dimension and the crystal grain that increase absorbed layer, it is compound to reduce charge carrier.Reduce the CIGS surface roughness in addition, not only can reduce the charge carrier surface recombination, also can improve the electrology characteristic at CIGS/CdS interface.Current CIGS absorbed layer by typical three-step approach and high temperature Seization method deposition can not guarantee to form " the back segregation " that Ga distributes, big columnar grain, Mo/CIGS interface good Ohmic characteristic, absorbed layer surface are mirror-like and good CIGS/CdS interfacial characteristics.
High-conversion rate chalcopyrite CIGS thin film solar cell requires to mix 0.1% Na in the CIGS absorbed layer.Na improves the growth mechanism of CIGS film, mixes simultaneously in the CIGS lattice and forms NaInSe
2, at the place, grain boundary, make donor-type defective In
CuPassivation becomes Na
CnIn addition, because the Na diffusion is accompanied by the O diffusion, Na is diffused into the V of donor-type
ScThe place easily forms neutral O
ScThereby, make increased by major defects, the P-type conduction enhancing, the compound minimizing of photo-generated carrier, photogenerated current strengthens.The preferential substrate of selecting of flexible solar cell is metal (as stainless steel) and polyimide foil, wherein do not contain the Na that the CIGS film is had material impact, so in order to optimize the performance of solar cell on the no Na substrate, need be in the optimal site of cigs layer, the Na of the optimised quantity of adding.Owing to Na can stop the diffusion of Cu, In, Ga the growth of Mo layer is changed.Deposition site and the opportunity of common several Na preformed layers in the current document, make the Na that mixes participate in the CIGS coating growth, when this feasible incorporation as Na is big, it is less to generate crystal grain easily, the CIGS rete that the degree of orientation is relatively poor, and the Na atom that occupies Cu lattice position simultaneously increases, and the P-type conduction of Mo layer is weakened, the compound enhancing of grain boundary place's photo-generated carrier, photo-generated carrier reduces, and causes the photoelectric conversion rate of solar cell not high.
Summary of the invention
In view of the problem that exists in the current C IGS absorbed layer deposition, with at the bottom of the flexible stainless steel lining of no sodium on the CIGS absorbed layer Na existing problem of mixing, the method of deposition and processing CIGS absorbed layer at the bottom of the flexible stainless steel lining below we have proposed at this, its concrete grammar is as follows: form CuGaSe between Mo and CIGS
2, at deposition (In
1-xGa
x)
3Se
5Adopt high [Ga]/[In+Ga] ratio during preformed layer, adopts 590 ℃ and high [Cu]/[In+Ga] than the Cu that satisfies stoichiometric proportion (InGa) Se of the rich copper of formation
2With two second phase Cu
xSe passes through Br at last
2Aqueous solution etching Cu (InGa) Se
2Surface two second phase Cu
xSe and deposit the InSe of the rich indium of poor copper thereon
3Rete.Hydatogenesis Na initialization layer carries out short annealing to sample again under higher temperature at low temperatures, makes it be diffused into grain surface and boundary, and this CIGS solar cell for the preparation high-photoelectric transformation efficiency provides may.
Preferably, at the bottom of the stainless steel lining of toluene, acetone, isopropyl alcohol and deionized water ultrasonic cleaning, under Ar atmosphere, the Ti rete of direct current sputtering deposition 30nm.On Ti film surface, direct current sputtering deposition Mo back contact under Ar atmosphere.
Preferably, Mo laminar surface coevaporation deposition Cu, Ga, Se at 380 ℃ make it form the CuGaSe of thick 0.2 μ m, [Cu]/[Ga]=1.55
2Rete.During the hydatogenesis, 070 ℃ of the evaporating temperature stuck-at-in Cu source, 85 ℃ of the evaporating temperature stuck-at-s in Se source, the evaporating temperature in Ga source is fixed on 890 ℃.Strengthening cigs layer in the tack that the soda-lime glass of coating Mo sinks to the bottom, reduce to carry on the back contact resistance, strengthen the ohmic contact characteristic of Mo, being conducive to simultaneously grows runs through whole thicknesses of layers, the columnar grain of arranging perpendicular to film surface.
Preferably, coevaporation In, Ga, Se source 16min are at 400 ℃ CuGaSe
2Film surface makes it form (InGa) of 1.6 μ m, [Ga]/[In+Ga]～0.43
3Se
5Initialization layer.Between the preformed layer depositional stage, the evaporating temperature in In source is fixed on 930 ℃, 100 ℃ of the evaporating temperature stuck-at-s in Ga source, and the evaporating temperature in In source is fixed on 215 ℃; The evaporation deposition rate of In is
/ sec, the evaporation deposition rate of Ga is
/ sec, the evaporation deposition rate of Se is
/ sec is to obtain the Ga CONCENTRATION DISTRIBUTION of back segregation.
Preferably, preformed layer (IN
1-xGa
x)
3Se
5After deposition finishes, close and close the In source again after the Ga source makes its evaporation deposition rate be reduced to zero.
Preferably, after the evaporation deposition rate in In source was reduced to zero, in Se atmosphere, 10min was interior with preformed layer (In
1-xGa
x)
3Se
5Surface temperature is increased to 590 ℃ from 400 ℃.
Preferably, Cu, Se coevaporation are deposited on 590 ℃ (InGa)
3Se
5The preformed layer surface makes the reaction of itself and preformed layer, forms 1.8 μ m, Cu in 20min]/Cu (InGa) Se of the rich copper stoichiometric proportion of [In+Ga] max=1.25
2With two second phase Cu
xSe.Between the e depositional stage, 300 ℃ of the evaporating temperature stuck-at-s in Cu source, the evaporation deposition rate of Cu is
/ sec.Cu, Se and the preformed layer (InGa) of deposition
3Se
5Obtain Cu (InGa) Se of stoichiometric proportion during reaction 16min
2
Preferably, close the Cu source after, make sample under Se atmosphere, 590 ℃ annealing 2min, close the substrate heating resistor subsequently, close the Se source when making its temperature be reduced to 300 ℃ from 590 ℃.
Preferably, use the Br of 0.23mol/L
2The aqueous solution is etching CIGS sample surfaces 8min at room temperature, wherein Br
2The aqueous solution is added with the KBr solution that concentration is 0.12mol/L.Make and removing the two second phase Cu on CIGS surface
xObtain the surface of mirror-like in the time of Se.
Preferably, under 390 ℃, at CIGS surface evaporation deposition In and Se, form the In of thick 0.12 μ m, In/Se=1.4/8
2Se
3Film.
Preferably, In
2Se
3After the film deposition finishes, close the In source, make sample under Se atmosphere, 390 ℃ of annealing 30min.
Preferably, at 80 ℃ In
2Se
3The Na preformed layer Na of deposition 23nm on the rete
2S.Na
2After S layer deposition finishes, sample is heated rapidly to 450 ℃, makes it under Se atmosphere, short annealing 20min.So that Na diffuses to grain surface and at the interface, with its place's defective effect, in and alms giver's defective, make the CIGS rete change the P type into.
Description of drawings:
Fig. 1 be at the bottom of the flexible stainless steel lining on preparation technology's flow chart of CIGS absorbed layer
Embodiment:
Below CIGS absorbed layer deposition process on the soda-lime glass substrate is described in detail:
CIGS absorbed layer depositing operation is specific as follows on the soda-lime glass substrate:
1) with 070 ℃ of the evaporating temperature stuck-at-in Cu source, 85 ℃ of the evaporating temperature stuck-at-s in Se source, the evaporating temperature in Ga source is fixed on 890 ℃, and Cu, Se, Ga are being applied on the soda-lime glass substrate of Mo layer 380 ℃ of following hydatogenesiss, forms the CuGaSe of thick 0.2 μ m, [Cu]/[Ga]=1.5
2Rete.
2) in Se atmosphere, in the 1-2min substrate is increased to 400 ℃ from 380 ℃.The evaporating temperature in In source is 930 ℃, and the evaporating temperature in Ga source is 1100 ℃, and the evaporating temperature in In source is 215 ℃.Make In, Ga, Se respectively with
/ sec,
/ sec and
The evaporation deposition rate of/sec is at CuGaSe
2Rete deposition 16min, (InGa) of formation [Ga]/[In+Ga]～0.43
3Se
5Preformed layer.
3) close the Ga source, close the In source again after making its evaporation rate be reduced to zero, after In evaporation rate deposition is reduced to zero, in Se atmosphere, in 7min, substrate is increased to 590 ℃ from 400 ℃.The evaporating temperature in Cu source is adjusted to 1300 ℃, make Cu with
The hydatogenesis of/sec and Se codeposition are at (InGa)
3Se
5On the preformed layer, behind Cu, the Se hydatogenesis 20min, [Cu]/[In+Ga] max=1.25.
4) close the Cu source after, make sample under Se atmosphere, 590 ℃ of following annealing 2min, close lining heat subsequently, close the Se source when making its temperature be reduced to 300 ℃ from 590 ℃.
5) with being added with the Br of 0.23mol/L that concentration is the KBr solution of 0.12mol/L
2The aqueous solution, at room temperature etching CIGS surface 8min behind deionized water rinsing 5min, dries up it in drying nitrogen, and is subsequently that it is also indoor as ultra high vacuum.
6) underlayer temperature is elevated to 390 ℃ from room temperature, hydatogenesis In and Se make it form the In of thick 0.12 μ m, In/Se=1.4/8 on the CIGS surface
2The Se film.Close the In source subsequently, make sample under Se atmosphere, 390 ℃ of annealing 30min.
7) at 80 ℃ In
2Se
3The Na preformed layer Na of deposition 23nm on the rete
2S.Heavy Na
2After S layer deposition finishes, sample is heated rapidly to 450 ℃, makes it under Se atmosphere, short annealing 20min.
Claims (10)
1. the layer preparation method that CIGS absorbs at the bottom of the flexible stainless steel lining, it is characterized in that it comprises: on the cleaned stainless steel substrate, the Ti rete that sputtering sedimentation 30nm is thick, deposit thereon subsequently the Mo layer with Cu, Ga, Se hydatogenesis on the Mo layer, form CuGaSe
2Layer to strengthen the adhesion property of Mo/CIGS interlayer, forms the Ga gradient simultaneously.
With In, Ga, Se hydatogenesis at CuGaSe
2On the layer, form (In
1-xGa
x)
3Se
5Preformed layer.
With Cu and Se hydatogenesis at (In
1-xGa
x)
3Se
5On the preformed layer, form rich copper Cu (InGa) Se
2With two second phase Cu
xSe, Br
2Aqueous solution etching two second phase Cu
xSe is again with In, Se hydatogenesis Cu (InGa) Se after etching
2The surface forms the In of the rich indium of poor copper
2Se
3Layer forms In to the surface
2Se
3The sample of layer carries out annealing in process.
At In
2Se
3Hydatogenesis Na on the layer
2The S initialization layer carries out The high temperature anneal to sample again.
2. the deposition process of CIGS absorbed layer according to claim 1, it is characterized in that: under Ar gas, on at the bottom of the stainless steel lining behind toluene, acetone and the isopropyl alcohol ultrasonic cleaning successively, the Ti layer of magnetron sputtering deposition 30nm is then at Ti laminar surface sputtering sedimentation Mo layer.
3. the deposition process of CIGS absorbed layer according to claim 1 is characterized in that: deposit Cu, Ga, Se at 380 ℃ Mo laminar surface coevaporations, form thick 0.2 μ m, the CuGaSe of [Cu]/[Ga]=1.55
2Rete.During the hydatogenesis, 070 ℃ of the evaporating temperature stuck-at-in Cu source, 85 ℃ of the evaporating temperature stuck-at-s in Se source, the evaporating temperature in Ga source is fixed on 890 ℃.
4. the deposition process of CIGS absorbed layer according to claim 1 is characterized in that: in Se atmosphere, in the 1-2min substrate is increased to 400 ℃ from 380 ℃, under this temperature, coevaporation In, Ga, Se source 16min make In, Ga, Se at CuGaSe
2Film surface forms (InGa) of 1.6 μ m, [Ga]/[In+Ga]～0.43
3Se
5Initialization layer.(InGa)
3Se
5Between the preformed layer depositional stage, the evaporating temperature in In source is fixed on 930 ℃, 100 ℃ of the evaporating temperature stuck-at-s in Ga source, and the evaporating temperature in In source is fixed on 215 ℃; The evaporation deposition rate of In is
/ sec, the evaporation deposition rate of Ga is
/ sec, the evaporation deposition rate of Se is
/ sec.
5. the deposition process of CIGS absorbed layer according to claim 1 is characterized in that: close the Ga source, close the In source after making the Ga evaporation rate be reduced to zero.After the In evaporation deposition rate is reduced to zero, in Se atmosphere, in the 7min substrate is increased to 590 ℃ from 400 ℃ again.
6. the deposition process of CIGS absorbed layer according to claim 1 is characterized in that: (InGa) that Cu, Se coevaporation is deposited on 590 ℃
3Se
5The preformed layer surface forms 1.8 μ m, Cu in 20min]/Cu (InGa) Se of the rich copper stoichiometric proportion of [In+Ga] max=1.25
2With two second phase Cu
xSe.Cu (InGa) Se
2And Cu
xBetween the Se depositional stage, 300 ℃ of the evaporating temperature stuck-at-s in Cu source, the evaporation deposition rate of Cu is
/ sec.
7. the deposition process of CIGS absorbed layer according to claim 1 is characterized in that: close the Cu source, make sample in Se atmosphere, close lining heat behind the annealing 2min down, close the Se source when making underlayer temperature be reduced to 300 ℃ from 590 ℃ for 590 ℃.
8. the deposition process of CIGS absorbed layer according to claim 1 is characterized in that: under the room temperature, with being added with the Br of 0.23mol/L that concentration is the KBr solution of 0.12mol/L
2Aqueous solution etching CIGS surface 8min.
9. the deposition process of CIGS absorbed layer according to claim 1 is characterized in that: the CIGS surface temperature is elevated to 390 ℃ from room temperature, at CIGS surface evaporation deposition In, Se, forms the In of thick 0.12 μ m, In/Se=1.4/8
2Se
3Rete is closed the In source subsequently, makes sample under Se atmosphere, 390 ℃ of annealing 30min.
10. at 80 ℃ In
2Se
3The Na preformed layer Na of deposition 23nm on the rete
2S.Heavy Na
2After S layer deposition finishes, sample is heated rapidly to 450 ℃, makes it under Se atmosphere, short annealing 20min.
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Cited By (4)
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| CN105633206A (en) * | 2014-11-06 | 2016-06-01 | 中物院成都科学技术发展中心 | Method for electrochemical modification of surface properties of copper indium gallium selenide thin film without water |
| CN105870247A (en) * | 2014-10-20 | 2016-08-17 | 台积太阳能股份有限公司 | Absorber surface modification |
| CN108172665A (en) * | 2017-12-30 | 2018-06-15 | 凯盛光伏材料有限公司 | A kind of processing method on CIGS solar battery obsorbing layers surface |
| CN108878558A (en) * | 2018-06-27 | 2018-11-23 | 北京铂阳顶荣光伏科技有限公司 | CIGS solar battery and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105870247A (en) * | 2014-10-20 | 2016-08-17 | 台积太阳能股份有限公司 | Absorber surface modification |
| CN105633206A (en) * | 2014-11-06 | 2016-06-01 | 中物院成都科学技术发展中心 | Method for electrochemical modification of surface properties of copper indium gallium selenide thin film without water |
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| CN108172665A (en) * | 2017-12-30 | 2018-06-15 | 凯盛光伏材料有限公司 | A kind of processing method on CIGS solar battery obsorbing layers surface |
| CN108878558A (en) * | 2018-06-27 | 2018-11-23 | 北京铂阳顶荣光伏科技有限公司 | CIGS solar battery and preparation method thereof |
| EP3621125A4 (en) * | 2018-06-27 | 2020-03-25 | Beijing Apollo Ding Rong Solar Technology Co. Ltd. | Cigs solar cell and preparation method thereof |
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Application publication date: 20130821 |