CN103474128A - Method for manufacturing copper indium gallium diselenide thin-film solar cells - Google Patents
Method for manufacturing copper indium gallium diselenide thin-film solar cells Download PDFInfo
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- CN103474128A CN103474128A CN2013104187845A CN201310418784A CN103474128A CN 103474128 A CN103474128 A CN 103474128A CN 2013104187845 A CN2013104187845 A CN 2013104187845A CN 201310418784 A CN201310418784 A CN 201310418784A CN 103474128 A CN103474128 A CN 103474128A
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Abstract
The invention discloses a method for manufacturing copper indium gallium diselenide thin-film solar cells. The method comprises the steps that (1), compound conductive molybdenum thick liquid is arranged on a ceramic substrate in a silk-screen printing or blade coating or spraying mode, and back electrodes are obtained after drying of 150-250 DEG C, heat processing of 450-1150 DEG C and annealing of 150-250 DEG C, wherein the compound conductive molybdenum thick liquid comprises the following components, by weight, 50-80 parts of molybdenum powder, 5-15 parts of glass powder, 10-25 parts of organic carriers and 5-10 parts of annexing agents; the organic carriers comprise epoxy resin and organic solvent, and the mass ratio between the epoxy resin and the organic solvent is (1-5):(9-20); the annexing agents comprise moderate NaOH, thickening agents, plasticizer and surface active agents; (2), the copper indium gallium diselenide thin-film solar cells are processed based on the back electrodes. Compared with the prior art, the compound conductive molybdenum thick liquid adopted in the method can process the back electrodes of the copper indium gallium diselenide thin-film solar cells through a non-vacuum processing technology, namely, the silk-screen printing method or the spraying method or the blade coating method, the process is simple and the manufacturing cost is lowered.
Description
Technical field
The invention belongs to the electrode of solar battery preparation field, be specifically related to a kind of method for preparing copper-indium-galliun-selenium film solar cell.
Background technology
Day by day serious today in energy crisis, the research of new forms of energy and application seem and become more and more important.Solar energy is as the important a member in New Energy Industry, has cleanliness without any pollution, the advantage such as inexhaustible, safe and harmless.The characteristics such as the CIGS solar cell has stable performance, capability of resistance to radiation is strong, production cost is low, environment-friendly high-efficiency, may become follow-on commercial thin-film solar cells.But the solar energy industry still exists the inferior positions such as expensive, unstable, in China, the application of solar energy also substantially also rests on large-scale power station, and large-scale power station is distributed in the low areas of the density of population such as the Northwest substantially, in other areas of China, particularly in big city, apply also seldom.As a promising important directions of tool of current solar energy industry development, BIPV can well solve the application of solar energy in urban area.Current BIPV is mainly that the silica-based solar panel that waits is integrated in to the building surfaces such as roof, and this mode both can increase extra cost, affected again attractive in appearance.
Summary of the invention
The object of the invention is to overcome the prior art defect, a kind of method for preparing copper-indium-galliun-selenium film solar cell is provided.
Technical scheme of the present invention is as follows:
A kind of method for preparing copper-indium-galliun-selenium film solar cell comprises:
(1) the composite conducting molybdenum is starched by silk screen printing, blade coating or is sprayed on ceramic substrate, then through 150-250 ℃ of oven dry, 450-1150 ℃ heat treatment and (150-250 ℃) annealing, make back electrode, this composite conducting molybdenum slurry comprises the component of following weight portion:
Wherein organic carrier comprises epoxy resin and the organic solvent that mass ratio is 1-5:9-20, and additive comprises appropriate NaOH, thickener, plasticizer and surfactant;
(2) prepare copper-indium-galliun-selenium film solar cell on the basis of above-mentioned back electrode.
NaOH is mainly used in providing sodium element to promote the grain growth of CIGS thin-film, favourable raising solar battery efficiency; Thickener is a kind of auxiliary rheological agents, and its Main Function is viscosity and the plasticity for regulating electrocondution slurry, improves caking property.
In a preferred embodiment of the invention, the molybdenum powder that described molybdenum powder is particle diameter 0.01-50 μ m.When the molybdenum powder particle used is excessive, in the process of molybdenum slurry sintering, the defective tightness of combination between the molybdenum particle, rete is coarse, and the sintering defect is many, and the properties of electrode can descend; And too small when the molybdenum powder particle diameter, because surface can be excessive, between particle, more easily reuniting is not easy to disperse, and just is not easy printing and levelling more than a certain constant concentration, electrode preparation difficulty, and cost is corresponding also to be increased greatly.
In a preferred embodiment of the invention, described glass dust is lead-free glass powder.Make that molybdenum slurry connects in heat treatment process, tension, fixing conductive phase molybdenum particle, form fine and close conductive film and whole rete and substrate be bonded together securely.In addition, adding of this glass dust can improve conductive paste liquid system various aspects of performance, such as making to conduct electricity each composition of slurries, disperses more even; The difference that the glass dust percentage composition is chosen can also be adjusted the heat treatment temperature of regulating the molybdenum slurry, the molybdenum slurry used under 400～1200 ℃ of preparation heat treatment temperatures.
In a preferred embodiment of the invention, described epoxy resin is a kind of or mixing in E44 and E51 epoxy resin.It has good cohesive force, anti-oxidant, corrosion resistant characteristic, can also regulate the slurries viscosity, can add in addition trace polyurethane-modified, and it is more easily solidified.
In a preferred embodiment of the invention, described organic solvent comprises Macrogol 200.
In a preferred embodiment of the invention, described organic solvent also comprises terpinol and/or PEG400, and the mass ratio of terpinol and Macrogol 200 is 0-30:55-100, and the mass ratio of PEG400 and Macrogol 200 is 0-15:55-100.
Above-mentioned these organic solvents are nontoxic, wettability to molybdenum powder is relatively good, the molybdenum powder uniform particles can be wrapped up and be beneficial to the dispersed of molybdenum powder particle, making electrocondution slurry be not easy to produce reunites and precipitation, wherein terpinol is colourless thick liquid, boiling point is 220.85 ℃, contain oxygen atom in structure, can reduce the reunion of molybdenum nano-scale particle, can also control evaporation rate when slurry drying, prevent from applying the local rete that causes because solvent evaporates is too fast of rete and shrink the uneven cracking that produces simultaneously; The polyethylene glycol that relative molecular weight is lower has the extensive compatibility with various solvents, is good solvent and solubilizer, makes whole slurries system mix more even, and the solubility of additives such as the rate of drying of control slurry and thickener.PEG-4000 or defoamer can play and avoid liquid level bubble to occur in the process stirred in addition, and polyethylene glycol-200 are also as NMF, and the viscosity diluent, if the too high polyethylene glycol-200 that can add of slurries viscosity is regulated.In sintering process, these solvents can progressively volatilize or decompose, and avoid, in film surface and the inner cavity that produces, volatilizing while arriving certain temperature clean the noresidue ash content.
In a preferred embodiment of the invention, described thickener is a kind of or mixing in ethyl cellulose, butyl cellulose, hydroxyethylcellulose and methyl hydroxyethylcellulose; Not only can make the slurry thickening, there is certain mechanical strength after the slurry sintering, can also make slurry be not easy oxidation and precipitation, improve slurry rheological property, give mechanical performance and the bin stability of electrocondution slurry excellence, form at a certain temperature tough film after organic solvent volatilization, under high temperature, (approximately more than 300 ℃) can the thermal decomposition effusion and the noresidue ash content
Described plasticizer is the organic polymer plasticizer with flexible group;
Described surfactant comprises a kind of or mixing in ethanol, toluene, SPAN85, lecithin.Wherein SPAN85 has good intermiscibility in organic media, improves the wetability of organic solvent, and higher hydroxyl value and molecular weight can guarantee that in the more metallic particles of absorption it suspends in addition, and the stability of slurry is had to facilitation; Ethanol is good to the wetability of molybdenum powder particle, and to other additives such as solubility of ethylcellulose is good.
In a preferred embodiment of the invention, described plasticizer comprises dibutyl phthalate, polyesters plasticizer or polyalcohol ester plasticizer.Above-mentioned plasticizer can increase polymer plasticity and electrocondution slurry viscosity, reaches the purpose of optimizing electrocondution slurry levelability and thixotropy and processing characteristics.
Finally can also such as different substrates, add the auxiliary agents such as other flow control agents, gelling agent, thixotropic agent according to different application conditions, change the performances such as the rheological characteristic of electrocondution slurry and thixotropy.
The invention has the beneficial effects as follows:
1, compared with prior art, the composite conducting molybdenum slurry that method of the present invention is used can adopt antivacuum technology of preparing to prepare the back electrode of copper-indium-galliun-selenium film solar cell, adopt silk screen print method, spraying process or knife coating, technique is simple, reduces manufacturing cost;
2, the solar cell that prepared by the present invention can directly be integrated on construction material, is conducive to realize BIPV.
3, the molybdenum film that the composite conducting molybdenum that prepared by the present invention slurry forms on pottery is high temperature resistant, facilitates high-temperature process when other layer of preparation Copper Indium Gallium Selenide.
The accompanying drawing explanation
Composite conducting molybdenum slurry one of stereoscan photograph after 1100 ℃ of heat treatment on ceramic substrate that Fig. 1 is the embodiment of the present invention 1 preparation;
The composite conducting molybdenum slurry that Fig. 2 is the embodiment of the present invention 1 preparation on ceramic substrate the stereoscan photograph after 1100 ℃ of heat treatment two;
Composite conducting molybdenum slurry one of stereoscan photograph after 900 ℃ of heat treatment on ceramic substrate that Fig. 3 is the embodiment of the present invention 2 preparations;
The composite conducting molybdenum slurry that Fig. 4 is the embodiment of the present invention 2 preparation on ceramic substrate the stereoscan photograph after 900 ℃ of heat treatment two.
Embodiment
Below by embodiment, technical scheme of the present invention is further detailed and describes.
By 7g molybdenum powder (particle diameter 0.01-50 μ m), 0.5g glass dust (lead-free glass powder), 0.5g terpinol, 1g polyethylene glycol-200,0.25g PEG-4000,0.1g epoxy resin E44(or E51), 0.005gNaOH, 0.1g ethyl cellulose, 0.01g dibutyl phthalate, the 85(of class of 0.03g department SPAN85), 0.5g ethanol, 0.005g organic silicone oil puts together and mixes, and makes composite conducting molybdenum slurry.
Molybdenum is starched to silk screen printing or blade coating on ceramic substrate, and 200 ℃ of oven dry, then 1100 ℃ of lower heat treatments 0.5 hour, insulation is 2 hours under 200 ℃, prepares conduction molybdenum film electrode (being described back electrode).By using scanning electron microscopy (SEM) to observe their surface and cross section (as depicted in figs. 1 and 2), use the four point probe resistance meter to measure film rectangular resistance and characterized, and the calculated resistance rate.Adopt (the American Society for Testing Materials of American Society Testing and Materials, ASTM) standard test method ASTM-D3359-08, the caking property test that Standard Test Methods for Measuring Adhesion by Tape Test carries out film characterizes, and test result is as shown in table 1 below:
Table 1 sample resistivity and caking property test result
Continuation prepares copper-indium-galliun-selenium film solar cell on this conduction molybdenum film electrode.
Embodiment 2
By 7g molybdenum powder (particle diameter 0.01-50 μ m), 0.5g glass dust (lead-free glass powder), 0.5g terpinol, 1g polyethylene glycol-200,0.25g PEG-4000,0.1g epoxy resin E44(or E51), 0.005gNaOH, 0.1g ethyl cellulose, 0.01g dibutyl phthalate, the 85(of class of 0.03g department SPAN85), 0.5g ethanol, 0.005g organic silicone oil puts together and mixes, and makes composite conducting molybdenum slurry.
Molybdenum is starched to silk screen printing or blade coating on ceramic substrate, and 200 ℃ of oven dry, then 900 ℃ of lower heat treatments 0.5 hour, insulation is 2 hours under 200 ℃, prepares conduction molybdenum film electrode.By using scanning electron microscopy (SEM) to observe their surface and cross section (as shown in Figure 3 and Figure 4), use the four point probe resistance meter to measure film rectangular resistance and characterized, and the calculated resistance rate.Adopt (the American Society for Testing Materials of American Society Testing and Materials, ASTM) standard test method ASTM-D3359-08, the caking property test that Standard Test Methods for Measuring Adhesion by Tape Test carries out film characterizes, and test result is as shown in table 2 below:
Table 2 sample resistivity and caking property test result
Continuation prepares copper-indium-galliun-selenium film solar cell on this conduction molybdenum film electrode.
Those skilled in the art can be adjusted in following process conditions, and obtain same as the previously described embodiments or close technique effect:
Annealing temperature 150-250 ℃;
Described organic solvent also comprises terpinol and/or PEG400, and the mass ratio of terpinol and Macrogol 200 is 0-30:55-100, and the mass ratio of PEG400 and Macrogol 200 is 0-15:55-100.
Described thickener is a kind of or mixing in ethyl cellulose, butyl cellulose, hydroxyethylcellulose and methyl hydroxyethylcellulose;
Described plasticizer is the organic polymer plasticizer with flexible group, preferably includes dibutyl phthalate, polyesters plasticizer or polyalcohol ester plasticizer;
Described surfactant comprises a kind of or mixing in ethanol, toluene, SPAN85, lecithin.
The above, be only preferred embodiment of the present invention, therefore can not limit according to this scope of the invention process, the equivalence done according to the scope of the claims of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.
Claims (8)
1. a method for preparing copper-indium-galliun-selenium film solar cell is characterized in that: comprising:
(1) the composite conducting molybdenum is starched by silk screen printing, blade coating or is sprayed on ceramic substrate, then through 150-250 ℃ of oven dry, 450-1150 ℃ heat treatment and (150-250 ℃) annealing, make back electrode, this composite conducting molybdenum slurry comprises the component of following weight portion:
Wherein organic carrier comprises epoxy resin and the organic solvent that mass ratio is 1-5:9-20, and additive comprises appropriate NaOH, thickener, plasticizer and surfactant;
(2) prepare copper-indium-galliun-selenium film solar cell on the basis of above-mentioned back electrode.
2. a kind of composite conducting molybdenum slurry as claimed in claim 1, is characterized in that: the molybdenum powder that described molybdenum powder is particle diameter 0.01-50 μ m.
3. a kind of composite conducting molybdenum as claimed in claim 1 is starched, and it is characterized in that: described glass dust is lead-free glass powder.
4. a kind of composite conducting molybdenum as claimed in claim 1 is starched, and it is characterized in that: described epoxy resin is a kind of or mixing in E44 and E51 epoxy resin.
5. a kind of composite conducting molybdenum as claimed in claim 4 is starched, and it is characterized in that: described organic solvent comprises Macrogol 200.
6. a kind of composite conducting molybdenum as claimed in claim 5 is starched, it is characterized in that: described organic solvent also comprises terpinol and/or PEG400, the mass ratio of terpinol and Macrogol 200 is 0-30:55-100, and the mass ratio of PEG400 and Macrogol 200 is 0-15:55-100.
7. a kind of composite conducting molybdenum as claimed in claim 1 is starched, and it is characterized in that: described thickener is a kind of or mixing in ethyl cellulose, butyl cellulose, hydroxyethylcellulose and methyl hydroxyethylcellulose; Described plasticizer is the organic polymer plasticizer with flexible group; Described surfactant comprises a kind of or mixing in ethanol, toluene, SPAN85, lecithin.
8. a kind of composite conducting molybdenum as claimed in claim 7 is starched, and it is characterized in that: described plasticizer comprises dibutyl phthalate, polyesters plasticizer or polyalcohol ester plasticizer.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109887641A (en) * | 2019-02-18 | 2019-06-14 | 邓建明 | It is a kind of to effectively improve and CuInSe2The Mo layer of layer ohm contact performance |
| CN110148639A (en) * | 2019-05-15 | 2019-08-20 | 王崧 | A kind of preparation method of CIGS thin film Mo back electrode used for solar batteries |
| CN112786232A (en) * | 2019-11-11 | 2021-05-11 | 江西佳银科技有限公司 | N-type solar cell silver paste doped with organic gallium and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107634146B (en) * | 2015-12-22 | 2020-11-13 | 山西绿普光电新材料科技有限公司 | Precursor emulsion for preparing photovoltaic material with flexible perovskite structure and preparation method thereof |
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| US4576735A (en) * | 1983-10-14 | 1986-03-18 | Hitachi, Ltd. | Electroconductive molybdenum paste |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109887641A (en) * | 2019-02-18 | 2019-06-14 | 邓建明 | It is a kind of to effectively improve and CuInSe2The Mo layer of layer ohm contact performance |
| CN110148639A (en) * | 2019-05-15 | 2019-08-20 | 王崧 | A kind of preparation method of CIGS thin film Mo back electrode used for solar batteries |
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| CN112786232A (en) * | 2019-11-11 | 2021-05-11 | 江西佳银科技有限公司 | N-type solar cell silver paste doped with organic gallium and preparation method thereof |
| CN112786232B (en) * | 2019-11-11 | 2023-01-03 | 江西佳银科技有限公司 | N-type solar cell silver paste doped with organic gallium and preparation method thereof |
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