CN103337555B - A kind of copper and indium sulfur selenium powder body for thin-film solar cells or the preparation method of thin film - Google Patents
A kind of copper and indium sulfur selenium powder body for thin-film solar cells or the preparation method of thin film Download PDFInfo
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Abstract
The invention discloses a kind of copper and indium sulfur selenium powder body for thin-film solar cells or the preparation method of thin film；The method is first copper chloride and indium chloride to be scattered in organic solvent, obtains dispersion liquid after ultrasonic disperse；After adding sodium sulfide and selenium powder in gained dispersion liquid, stir, obtain mixed liquor；Again described mixed liquor is transferred in reactor, reacts after constant volume, sealing, after having reacted, sucking filtration, by filtering residue priority deionized water and absolute ethanol washing, vacuum drying, obtain CuIn (S, Se)2Powder body；Or described mixed liquor is moved in reactor, and add substrate of glass, after constant volume, sealing, liquid deposition, the substrate of glass priority deionized water that deposition is obtained and absolute ethanol washing, vacuum drying, obtain CuIn (S, Se)2Thin film；The equipment that the method uses is simple, and production cost is low；The CuIn (S, Se) produced2Powder body, film performance are excellent, good stability, can realize industrialized production；And can be by controlling the content of S element, so that CuIn (S, Se)2Band gap continuously adjustabe between 1.21～1.45eV.
Description
Technical field
The present invention relates to a kind of copper and indium sulfur selenium powder body for thin-film solar cells or the preparation method of thin film, belong to
In photoelectric functional material field.
Background technology
The energy is the power of social development, and the innovation of energy technology drives human society to be showing improvement or progress day by day.Solar energy quilt
It is considered one of following most potential energy, and for the utilization of solar energy mainly by solar electrical energy generation.
At present, solaode has evolved to second filial generation thin-film solar cells, copper indium diselenide therein (CIS,
CIGS, CISSe etc.) thin-film solar cells is because its absorption coefficient of light is high, photoelectric transformation efficiency is good, performance is steady
Fixed, good without photo attenuation phenomenon, low light level power generation performance, the Radiation hardness advantage such as by force and enjoy various countries' scientific research machine
Structure and the favor of photovoltaic enterprise.
In copper indium diselenide (CIS class) thin-film solar cells, absorbed layer is to affect cell photoelectric transformation efficiency
Key factor, for the core material of battery.At present, the manufacture method of CIS class absorbed layer can be divided into vacuum and non-
Vacuum two class, vacuum types includes selenizing method, ion beam sputter depositing method etc. after polynary coevaporation method, magnetron sputtering
Method.Patent CN101777604A reports a kind of employing ion beam sputter depositing method and prepares thin film solar
Battery obsorbing layer CuInSe2The method of thin film, by accurately adjusting the parameter etc. of ion beam sputtering, successively sputters
Cu, In and Se target prepares ternary lamination or ternary cycle laminate film, under same high vacuum environment, high temperature
Prepare by annealing CuInSe2Thin film.Vacuum technology can prepare the battery that photoelectric transformation efficiency is higher, gained
Battery product has some superiority, but owing to vacuum equipment needs the biggest investment, preparation condition is harsh, productivity
The highest, relatively costly, its permanent application will certainly be had influence on.
At present, increasing researcher invests low cost adopting non-vacuum process sight, such as electro-deposition, screen printing
Brush method etc..Although adopting non-vacuum process does not has vacuum technology of preparing ripe, but it has low cost, preparation condition temperature
With etc. advantage so that it is there is bigger research and development prospect.
Patent CN102683497A and patent CN101694854A report antivacuum wet-chemical legal system respectively
Standby CuIn (S, Se)2The method of thin film, compared with traditional fine vacuum technique, its technique is simple, and cost is relatively low,
Workable, but the later stage still need to carry out complex selenized annealing and process.
It is thus desirable to study a kind of new preparation CuIn (S, Se)2The adopting non-vacuum process of thin film solves the problems referred to above.
Summary of the invention
The present invention is directed to adopting non-vacuum process of the prior art and prepare CuIn (S, Se)2There is preparation in the method for thin film
The defects such as condition is harsh, and Technology for Heating Processing is complicated, it is therefore intended that a kind of antivacuum preparation CuIn (S, Se) is provided2
Thin film or the method for powder body, the equipment that the method uses is simple, and cheaper starting materials, production cost are low, technological process
Simply, pollution-free, it is easy to accomplish industrialized production；The CuIn (S, Se) prepared2Thin film or powder body light are inhaled
Receipts characteristic is good, can be by the regulation and control of S amount of element realize the change of optical absorption band；Particularly prepare
CuIn(S,Se)2Film surface is regular, and adhesive force is good, difficult drop-off, good stability.
The invention provides a kind of copper and indium sulfur selenium powder body for thin-film solar cells or the preparation method of thin film,
The method is first copper chloride and indium chloride to be scattered in organic solvent, obtains dispersion liquid after ultrasonic disperse；Institute
Obtain after dispersion liquid adds sodium sulfide and selenium powder, stir, obtain mixed liquor；Again described mixed liquor is shifted
To reactor, after constant volume, sealing, reacting at 160～220 DEG C, after having reacted, sucking filtration, by filtering residue
Priority deionized water and washing with alcohol, vacuum drying, obtain CuIn (S, Se)2Powder body；Or by described
Mixed liquor moves in reactor, adds substrate of glass, and after constant volume, sealing, at 160～220 DEG C, liquid phase is sunk
Long-pending, the substrate of glass priority deionized water that deposition is obtained and washing with alcohol, vacuum drying, obtain
CuIn(S,Se)2Thin film.
In the sodium sulfide added in said method and selenium powder the molar relationship of S and Se meet S/ (S+Se)=0.1～
0.9。
In said method, between copper chloride and indium chloride and sodium sulfide and selenium powder, addition meets ideal stoichiometric
Than Cu:In:(S+Se)=1～1.05:1:2.
The described response time is 12～15h.
The time of described liquid deposition is 12～15h.
Described organic solvent be dehydrated alcohol amine, anhydrous ethylenediamine one or both.
Described ultrasonic disperse is in the ultrasonic lower dispersion 20～60min that power is 200～300W.
Described vacuum drying is at 60～80 DEG C, is vacuum dried 8～12h.
Described substrate of glass is optical glass, soda-lime glass, Mo glass or transparent electro-conductive glass；Institute
The substrate of glass specification stated is about the sheet glass of 25mm × 75mm.
Described constant volume is to add dehydrated alcohol amine or anhydrous ethylenediamine in reactor, makes the mixing in reactor
Liquor capacity accounts for the 75～85% of reactor.
Filtering residue priority deionized water and dehydrated alcohol that in said method, after reaction, sucking filtration obtains are washed the most repeatedly
Wash until the filtrate of sucking filtration is clarified, without obvious floating thing after washing.
In said method, after deposition, substrate of glass priority deionized water and the dehydrated alcohol of gained are washed the most repeatedly
Wash until washing after washing liquid clarification, without obvious floating thing.
The present invention is for the copper and indium sulfur selenium powder body of thin-film solar cells or the preparation method of thin film:
1, first by copper chloride (CuCl2·2H2O), indium chloride (InCl3·4H2O) stoichiometrically 1～1.05:1 divide
Dissipate in water-ethanol amine or anhydrous ethylenediamine, then in the ultrasonic lower dispersion 20～60min that power is 200～300W
Obtain dispersion liquid；
2, S/ (S+Se)=0.1～0.9 adds sodium sulfide (Na the most in molar ratio2S·9H2O), selenium powder (Se), stir
Mix and be uniformly transferred to reactor and obtain mixed liquor；
On the one hand directly 3, mixed liquor is transferred to reactor, then adds dehydrated alcohol amine or anhydrous ethylenediamine arrives
In reactor, make the mixed liquor volume in reactor account for reactor 75～85%, seal after 160～220
DEG C heat treatment 12～15h, sucking filtration, filtering residue for several times by deionized water, dehydrated alcohol filtering and washing respectively successively,
Transfer to vacuum drying oven at 60～80 DEG C, be vacuum dried 8～12h, obtain CuIn (S, Se)2Powder body；
4, on the other hand mixed liquor is transferred in reactor, adds substrate of glass, at 160～220 DEG C of liquid
Deposition 12～15h mutually, then takes out substrate of glass, successively washs number respectively with deionized water, dehydrated alcohol
Secondary, transfer to vacuum drying oven at 60～80 DEG C, be vacuum dried 8～12h, obtain CuIn (S, Se)2Thin film.
The beneficial effects of the present invention is:
The present invention selects CuCl2·2H2O、InCl3·4H2O、Na2S·9H2O and Se powder as reaction raw materials,
Being not related to prohibitively expensive or have virose organic metal salt and selenizing Organic substance, cost of material is relatively low, to ring
Border close friend is pollution-free；
The equipment that the present invention uses is simple, and technological process is short, need not process by complicated selenized annealing, simple to operate,
It is widely used, it is easy to accomplish industrialized production；
CuIn (S, Se) prepared by the present invention2Powder body is figure it is seen that in thin slice tufted, thickness is about 20
Nm, mean diameter is at about 200nm, and crystallization degree is high, and specific surface area active is big, is conducive to improving the sun
Light utilization efficiency；
CuIn (S, Se) prepared by the present invention2Thin film is from figure 3, it can be seen that surface is regular, and adhesive force is good,
Difficult drop-off, good stability, optical absorption characteristics is good, all presents stronger absorption energy in ultraviolet-visible light district
Power；
The preparation method of the present invention is by controlling the initial molar ratio of each composition, it is possible to achieve element each to product becomes
The Effective Regulation divided；Along with the increase of S element, there is " blue shift " phenomenon in its absorbing properties so that it is band gap
Can be at 1.21-1.45eV continuously adjustabe.
Accompanying drawing explanation
[Fig. 1] is that the present invention prepares CuIn (S, Se)2Powder body or the process chart of thin film.
[Fig. 2] is the CuIn (S, Se) of preparation in the embodiment of the present invention 22The SEM figure of powder body.
[Fig. 3] is the CuIn (S, Se) of preparation in the embodiment of the present invention 32The SEM figure of thin film.
[Fig. 4] is CuIn (S, Se) under different S element doping amount2The absorption curves of powder body.
[Fig. 5] is the absorption curves of sample in the embodiment of the present invention 4.
Detailed description of the invention
Following example are intended to further illustrate the present invention rather than limit the present invention.
Embodiment 1
Weigh: respectively at electronic analytical balance (accuracy of reading 0.1mg) upper weighing 0.8805g InCl3·4H2O、
0.5115g CuCl2·2H2O, and transfer them in the beaker equipped with 30mL ethanolamine, and cover with preservative film
Lid is in the above.
Dispersion: beaker is put in ultrasonic disperse machine, at the ultrasonic lower dispersion about 30min that power is 300W
Obtain dispersion liquid.
Constant volume: weigh 0.2880g Na the most respectively on electronic analytical balance2S·9H2O, 0.3792g Se powder adds
In dispersion liquid, it is uniformly mixing to obtain mixed liquor；Mixed liquor after dispersion is transferred in 100mL reactor and uses
Ethanolamine is settled to about the 80% of reactor volume.
Heat treatment: tighten sealing after being added a cover by reactor, puts in calorstat and reacts 15h in 180 DEG C.
Filtering and washing: after cooling to room temperature with the furnace, divides product priority deionized water and dehydrated alcohol
Other vacuum filtration washs for several times, until filtrate clarification and liquid level are without obvious floating thing.
It is dried sampling: put into by filter paper in culture dish or beaker, as in vacuum drying oven 70 DEG C of dry 12h
Obtain CuIn (S, Se)2Powder body.
Embodiment 2
Weigh: on electronic analytical balance, weigh 0.8805g InCl respectively3·4H2O、0.5115g CuCl2·2H2O,
Transfer them to fill in the beaker that there are about 30mL ethanolamine, and with preservative film cover it face.
Dispersion: beaker is put in ultrasonic disperse machine, at the ultrasonic lower dispersion about 30min that power is 300W
Obtain dispersion liquid.
Constant volume: weigh 0.7200g Na the most respectively on electronic analytical balance2S·9H2O, 0.2370g Se powder adds
In dispersion liquid, it is uniformly mixing to obtain mixed liquor；Mixed liquor after dispersion is transferred in 100mL reactor and uses
Ethanolamine is settled to about the 80% of reactor volume.
Heat treatment: tighten sealing after being added a cover by reactor, puts in calorstat and reacts 15h in 180 DEG C.
Filtering and washing: after cooling to room temperature with the furnace, by the trueest to product priority deionized water and dehydrated alcohol
Empty filtering and washing for several times, until filtrate clarification and liquid level are without obvious floating thing.
It is dried sampling: put into by filter paper in culture dish or beaker, as in vacuum drying oven 80 DEG C of dry 8h
Obtain CuIn (S, Se)2Powder body.
Embodiment 3
Weigh: on electronic analytical balance, weigh 0.8805g InCl respectively3·4H2O、0.5115g CuCl2·2H2O,
And transfer them in the beaker equipped with 30mL ethylenediamine, and with preservative film cover it face.
Dispersion: beaker is put in ultrasonic disperse machine, obtain at the ultrasonic lower dispersion about 30min of power 300W
Dispersion liquid.
Constant volume: weigh 1.1520g Na the most respectively on electronic analytical balance2S·9H2O, 0.0948g Se powder adds
In dispersion liquid, it is uniformly mixing to obtain mixed liquor；Mixed liquor after dispersion is transferred in 100mL reactor, with
Time to add specification be the transparent electro-conductive glass substrate of 25mm × 75mm, and be settled to reaction with ethanolamine
About the 80% of still volume.
High temperature deposition: tighten sealing after being added a cover by reactor, puts in calorstat and deposits 15h in 180 DEG C of constant temperature.
Filtering and washing: after cooling to room temperature with the furnace, takes out substrate of glass, successively by deionized water and anhydrous second
Alcohol washes away substrate of glass for several times respectively, until washing liquid is clarified and without obvious floating thing.
It is dried sampling: substrate of glass put in culture dish or beaker, does as in vacuum drying oven 70 DEG C
Dry 12h obtains CuIn (S, Se)2Thin film.
Embodiment 4
Weigh: on electronic analytical balance, weigh 0.8805g InCl respectively3·4H2O、0.5115g CuCl2·2H2O,
And transfer them in the beaker equipped with 30mL ethanolamine, and cover on it with preservative film.
Dispersion: beaker is put in ultrasonic disperse machine, at the ultrasonic lower dispersion about 30min that power is 300W
Obtain dispersion liquid.
Constant volume: weigh 0.4320g Na the most respectively on electronic analytical balance2S·9H2O, 0.3318g Se powder adds
In dispersion liquid, it is uniformly mixing to obtain mixed liquor；Mixed liquor after dispersion is transferred in 100mL reactor, with
Time to add specification be the Mo substrate of glass of 25mm × 75mm, and be settled to reactor volume with ethanolamine
About 80%.
High temperature deposition: tighten sealing after being added a cover by reactor, puts in calorstat and deposits 15h in 200 DEG C of constant temperature.
Filtering and washing: after cooling to room temperature with the furnace, takes out substrate of glass priority deionized water and dehydrated alcohol
Wash away substrate of glass respectively for several times, until washing liquid is clarified and without obvious floating thing.
It is dried sampling: substrate of glass put in culture dish or beaker, does as in vacuum drying oven 70 DEG C
Dry 12h obtains CuIn (S, Se)2Thin film.
Embodiment 5
Performance test:
Adhesive force in embodiment 3,4 measures employing [GB/T9286.1998], and (paint and varnish paint film is drawn
Lattice are tested) it is bioassay standard, its adhesive force of measurement result reaches 1～0 grade, shows that obtained thin film has relatively
High adhesive force.
Mol ratio S/ (S+Se)=0.2,0.4,0.6,0.8 sample are carried out UV-Vis analysis, compares different S
The absorbing properties of CuIn (S, Se) 2 powder body under element doping amount, result is as shown in Figure 4.From map analysis,
CuIn (S, Se) 2 powder body is the strongest at the light absorpting ability in ultraviolet-visible light district.But it is as S doping
Increasing and reduce, i.e. under same isophotal wavelength, the optical absorption edge of CuIn (S, Se) 2 powder body occurs that " blue shift " is existing
As.It is respectively as follows: 1.27eV, 1.32eV, 1.36eV by the energy gap of absorbing properties formula estimation sample
And 1.40eV, show to realize the Effective Regulation to samples band-gap by the doping controlling S element.
Using the blank glass substrate in embodiment 4 as comparison, use UV-2100 type UV-vis spectroscopy light
The absorption curves of degree meter measuring samples, experimental result is as it is shown in figure 5, it can be seen that embodiment 4
Obtained film sample also has preferable light absorpting ability in ultraviolet-visible light region, particularly visible
The absorbance in light region is higher, shows that it has good visible light response activity, can be used as thin film solar
The absorbed layer material of battery.
Claims (6)
1. the preparation method for the copper and indium sulfur-selenium thin film of thin-film solar cells, it is characterised in that first by chlorine
Change copper and indium chloride is scattered in organic solvent, after ultrasonic disperse, obtain dispersion liquid；Gained dispersion liquid adds
After sodium sulfide and selenium powder, stirring, obtain mixed liquor, in the sodium sulfide of addition and selenium powder, S's and Se rubs
You meet S/ (S+Se)=0.1～0.9 at relation；Move to, in reactor, add substrate of glass by described mixed liquor,
Constant volume, sealing, liquid deposition at 160～220 DEG C, the substrate of glass deionized water that deposition is obtained and nothing
Water-ethanol washs, vacuum drying, obtains CuIn (S, Se)2Thin film.
2. preparation method as claimed in claim 1, it is characterised in that the time of described liquid deposition is 12～15h.
3. preparation method as claimed in claim 1, it is characterised in that described organic solvent be dehydrated alcohol amine,
In anhydrous ethylenediamine one or both.
4. preparation method as claimed in claim 1, it is characterised in that described ultrasonic disperse is to be at power
The ultrasonic lower dispersion 20～60min of 200～300W.
5. preparation method as claimed in claim 1, it is characterised in that described vacuum drying is at 60～80 DEG C
Under, it is vacuum dried 8～12h.
6. the preparation method as described in any one of Claims 1 to 5, it is characterised in that described substrate of glass is light
Learn glass.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011194A (en) * | 2010-10-11 | 2011-04-13 | 中国科学院青岛生物能源与过程研究所 | Photovoltaic semiconductor nanocrystalline and preparation method and application thereof |
| 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 |
| CN102249549A (en) * | 2011-04-01 | 2011-11-23 | 中南大学 | Copper-indium-selenium photovoltaic film, powder and coating material for solar batteries and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102011194A (en) * | 2010-10-11 | 2011-04-13 | 中国科学院青岛生物能源与过程研究所 | Photovoltaic semiconductor nanocrystalline and preparation method and application thereof |
| CN102249549A (en) * | 2011-04-01 | 2011-11-23 | 中南大学 | Copper-indium-selenium photovoltaic film, powder and coating material for solar batteries and preparation method thereof |
| 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 |
Non-Patent Citations (2)
| Title |
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| Colloidal synthesis of monodisperse quaternary CuInSSe nanocrystals;Yu Zou, Dongsheng Li, Deren Yang;《Materials Chemistry and Physics》;20120215;第132卷(第2-3期);865-869 * |
| Low-temperature processing of a solution-deposited CuInSSe thin-film solar cell;William W. Hou, Brion Bob, Sheng-han Li, Yang Yang;《Thin Solid Films》;20090626;6853-6856 * |
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