CN105470112A - Method and application for preparing copper zinc tin sulfur semiconductor film on FTO substrate - Google Patents
Method and application for preparing copper zinc tin sulfur semiconductor film on FTO substrate Download PDFInfo
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- CN105470112A CN105470112A CN201510801054.2A CN201510801054A CN105470112A CN 105470112 A CN105470112 A CN 105470112A CN 201510801054 A CN201510801054 A CN 201510801054A CN 105470112 A CN105470112 A CN 105470112A
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- H—ELECTRICITY
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
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- H01L21/02425—Conductive materials, e.g. metallic silicides
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
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- H01L21/02568—Chalcogenide semiconducting materials not being oxides, e.g. ternary compounds
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
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- H01L21/02628—Liquid deposition using solutions
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Abstract
The invention discloses a method for preparing a copper zinc tin sulfur semiconductor film on an FTO substrate. The method comprises steps that, a solvent, a copper source, a zinc source, a tin source, a sulfur source and a surfactant are uniformly mixed to acquire a reaction precursor solution; FTO conductive glass fully contacts the reaction precursor solution, reaction is fully realized under the microwave condition, and the copper zinc tin sulfur semiconductor film is prepared on the FTO conductive glass. The method has advantages of simple equipment and preparation technology, low cost and rapid speed, the copper zinc tin sulfur semiconductor film having properties of uniform phase, excellent crystallization and relatively high purity can be directly prepared, and the copper zinc tin sulfur semiconductor film prepared through the method has excellent prospects in preparation applications of dye sensitization solar energy cells and film solar energy cells.
Description
Technical field
The present invention relates to the field of semiconductor film membrane preparation technology and new energy development utilization, particularly relate to a kind of on FTO electro-conductive glass, directly prepare copper zinc tin sulfur semiconductor film based on microwave-assisted synthesis method and application.
Background technology
Technology word is explained:
FTO electro-conductive glass: it is the SnO of doped with fluorine F
2transparent conducting glass (SnO
2: F), referred to as FTO.
Polyvinylpyrrolidone: its English full name is polyvinylpyrrolidone, is called for short PVP.
For copper-zinc-tin-sulfur (Cu
2znSnS
4be called for short CZTS) film, it has that absorption coefficient is high, energy gap (1.5eV) close to the theory best with gap value of unijunction solar cell, cost low and containing toxic element, stable performance, the advantages such as photoinduction decay can not be there is, therefore, it is considered to the another material being suitable as the absorbed layer of thin film solar cell after cadmium antimonide film and CIGS thin-film.
At present, conventional CZTS method for manufacturing thin film generally can be divided into vacuum method and the large class of antivacuum method two, and wherein, vacuum method includes the methods such as vacuum evaporation, sputtering, pulsed laser deposition, and antivacuum method includes spray-wall interaction, hot injection method
,the methods such as electrochemical deposition, sol-gel, solvent-thermal process and Microwave synthesize.And compared to vacuum technologies of preparing such as evaporation, sputterings, microwave-assisted synthesis then has that technique is simple, cost is low, it is little to consume energy, the controllable growth of the film of nanostructure can be realized, can directly obtain thing mutually evenly, well-crystallized, the advantage such as product that purity is higher, therefore, it is widely used.But, when current employing microwave-assisted synthesis realizes the preparation of CZTS film, need first to prepare CZTS powder, and then CZTS powder preparation form slurry or ink, then adopt the method such as spin coating, silk screen printing could prepare on substrate and draw CZTS film, can obtain thus, the current method adopting microwave-assisted synthesis to prepare CZTS film is still comparatively complicated, and the CZTS film prepared is fine and close not smooth.
Summary of the invention
In order to solve the problems of the technologies described above, the object of this invention is to provide a kind of method preparing copper zinc tin sulfur semiconductor film on FTO substrate.
The technical solution adopted in the present invention is: a kind of method preparing copper zinc tin sulfur semiconductor film on FTO substrate, and the method comprises:
A, solvent, Tong Yuan, zinc source, Xi Yuan, sulphur source and surfactant are mixed obtained reaction precursor liquid;
B, FTO electro-conductive glass fully to be contacted with reaction precursor liquid, under microwave condition fully after reaction, FTO electro-conductive glass prepares copper zinc tin sulfur semiconductor film.
Further, described copper source is copper chloride hydrate, and described zinc source is zinc chloride, and described Xi Yuan is stannous chloride hydrate, and described sulphur source is thiocarbamide, and described surfactant is polyvinylpyrrolidone.
Further, described steps A is specially: after adding copper source, zinc source and Xi Yuan in a solvent successively, utilizes magnetic agitation to fully dissolving; Then, after adding sulphur source and surfactant, utilizing magnetic agitation to fully dissolving, mixing and obtaining reaction precursor liquid.
Further, the amount ratio of described copper source, zinc source, Xi Yuan, sulphur source, surfactant is: 1mmol:(0.4-0.6) mmol:(0.4-0.6) mmol:(1.2-3) mmol:(0.16-0.5) g.
Further, described step B is specially:
The conducting surface of FTO electro-conductive glass is put into there-necked flask down, then described reaction precursor liquid is poured in there-necked flask, there-necked flask is put into microwave oven and carries out isothermal reaction, after isothermal reaction completes, the FTO electro-conductive glass depositing copper zinc tin sulfur semiconductor film is taken out from there-necked flask, with absolute ethyl alcohol and deionized water, FTO electro-conductive glass is cleaned respectively again, more fully dry.
Further, described abundant drying, is specially: be the vacuumize carried out under the condition of 80 DEG C 5 hours in temperature by described FTO electro-conductive glass.
Prepared copper zinc tin sulfur semiconductor film is preparing DSSC to the application in electrode.
Prepared copper zinc tin sulfur semiconductor film is as the application of absorbing layer of thin film solar cell.
Load has the FTO electro-conductive glass of copper zinc tin sulfur semiconductor film, and it is according to prepared by aforesaid method.
Load has the application of the FTO electro-conductive glass of copper zinc tin sulfur semiconductor film in preparation thin-film solar cells.
The invention has the beneficial effects as follows: copper zinc tin sulfur semiconductor film preparation method of the present invention there is equipment needed thereby and simple, the with low cost and speed of preparation technology fast, can directly obtain thing mutually evenly, well-crystallized, the advantage such as copper zinc tin sulfur semiconductor film that purity is higher.And method of the present invention have employed surfactant, therefore, FTO electro-conductive glass grows the copper zinc tin sulfur semiconductor film densification obtained smooth.
In addition, for by the preparation-obtained copper zinc tin sulfur semiconductor film of method of the present invention, its can directly be used as DSSC to electrode, traditional Pt so then can be replaced electrode, reduce the cost of DSSC, be conducive to industrialization and produce; And it also can directly be used for preparing CZTS thin-film solar cells, namely FTO electro-conductive glass can directly as the back electrode of battery, the CZTS film prepared is as the absorbed layer of CZTS thin-film solar cells, then on absorbed layer, resilient coating, Window layer and top electrode is directly prepared, thus be prepared into CZTS thin-film solar cells, the production process of CZTS thin-film solar cells can not only be simplified like this, and greatly can also reduce the making input cost of CZTS thin-film solar cells.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described further:
Fig. 1 is a kind of flow chart of steps preparing the method for copper zinc tin sulfur semiconductor film on FTO substrate of the present invention;
Fig. 2 is the surperficial SEM image of the copper zinc tin sulfur semiconductor film prepared by the inventive method;
Fig. 3 is the XRD figure of the copper zinc tin sulfur semiconductor film prepared by the inventive method;
Fig. 4 is the Raman spectrum of the copper zinc tin sulfur semiconductor film prepared by the inventive method;
Fig. 5 is the high-resolution TEM image of the copper zinc tin sulfur semiconductor film prepared by the inventive method;
Fig. 6 is the ultraviolet-visible light transmission spectrum of the copper zinc tin sulfur semiconductor film prepared by the inventive method.
Embodiment
As shown in Figure 1, a kind of method preparing copper zinc tin sulfur semiconductor film on FTO substrate, the method comprises:
A, solvent, Tong Yuan, zinc source, Xi Yuan, sulphur source and surfactant are mixed obtained reaction precursor liquid;
B, FTO electro-conductive glass fully to be contacted with reaction precursor liquid, under microwave condition fully after reaction, FTO electro-conductive glass prepares copper zinc tin sulfur semiconductor film.And according to the preparation-obtained copper zinc tin sulfur semiconductor film of this method, its surperficial SEM image, XRD figure, Raman spectrum, high-resolution TEM image and ultraviolet-visible light transmission spectrum are successively as shown in Fig. 2-Fig. 6.
Be further used as preferred embodiment, described copper source is copper chloride hydrate (CuCl
2.2H
2o), described zinc source is zinc chloride (ZnCl
2), described Xi Yuan is stannous chloride hydrate (SnCl
2.2H
2o), described sulphur source is thiocarbamide (CS (NH
2)
2, be called for short Tu), described surfactant is polyvinylpyrrolidone (PVP).Described solvent is preferably ethylene glycol ((CH
2oH)
2).
Be further used as preferred embodiment, described steps A is specially: after adding copper source, zinc source and Xi Yuan in a solvent successively, utilizes magnetic agitation to fully dissolving; Then, after adding sulphur source and surfactant, utilizing magnetic agitation to fully dissolving, mixing and obtaining reaction precursor liquid.
Be further used as preferred embodiment, the amount ratio of described copper source, zinc source, Xi Yuan, sulphur source, surfactant is: 1mmol:(0.4-0.6) mmol:(0.4-0.6) mmol:(1.2-3) mmol:(0.16-0.5) g.
Preferably, the amount ratio of described copper source, zinc source, Xi Yuan, sulphur source, surfactant is: 4mmol:2mmol:2mmol:(5-11) mmol:(0.64-1.92) g.
Be further used as preferred embodiment, described step B is specially:
The conducting surface of FTO electro-conductive glass is put into there-necked flask down, then described reaction precursor liquid is poured in there-necked flask, there-necked flask is put into microwave oven and carries out isothermal reaction, after isothermal reaction completes, the FTO electro-conductive glass depositing copper zinc tin sulfur semiconductor film is taken out from there-necked flask, with absolute ethyl alcohol and deionized water, FTO electro-conductive glass is cleaned respectively again, more fully dry.
Wherein, there-necked flask is put into microwave oven when carrying out isothermal reaction, it imposes a condition and is preferably: reaction temperature is 180 DEG C-200 DEG C, and microwave power is 700W-900W, and the reaction time is 40-60min.
Be further used as preferred embodiment, described abundant drying, is specially: be the vacuumize carried out under the condition of 80 DEG C 5 hours in temperature by described FTO electro-conductive glass.
Prepared copper zinc tin sulfur semiconductor film is preparing DSSC to the application in electrode.
Prepared copper zinc tin sulfur semiconductor film is as the application of absorbing layer of thin film solar cell.
Load has the FTO electro-conductive glass of copper zinc tin sulfur semiconductor film, and it is according to prepared by aforesaid method.
Load has the application of the FTO electro-conductive glass of copper zinc tin sulfur semiconductor film in preparation thin-film solar cells.
The present invention first specific embodiment
FTO substrate is prepared a method for copper zinc tin sulfur semiconductor film, and it specifically comprises:
S101, FTO electro-conductive glass cleaning step: FTO electro-conductive glass is put into successively each ultrasonic cleaning 10min of acetone, absolute ethyl alcohol and deionized water, then dry;
S102, in the ethylene glycol of 50ml, add 4mmol copper chloride hydrate, 2mmol zinc chloride and 2mmol stannous chloride hydrate successively after, utilize magnetic agitation to fully dissolving; Then, after adding 5mmol thiocarbamide and 0.64gPVP, utilizing magnetic agitation to fully dissolving, mixing and obtaining reaction precursor liquid;
S103, the conducting surface of the FTO electro-conductive glass cleaned up is put into there-necked flask down, then described reaction precursor liquid is poured in there-necked flask, there-necked flask is put into microwave oven and carries out isothermal reaction, wherein, reaction temperature is set to 180 DEG C, microwave power is set to 700W, and the reaction time is set to reaction 40min;
After isothermal reaction completes, the FTO electro-conductive glass depositing copper zinc tin sulfur semiconductor film is taken out from there-necked flask, with absolute ethyl alcohol and deionized water, three times are respectively cleaned to FTO electro-conductive glass respectively again, be the vacuumize carried out under the condition of 80 DEG C 5 hours again in temperature by described FTO electro-conductive glass, so just directly can prepare copper zinc tin sulfur semiconductor film on FTO electro-conductive glass.
The present invention second specific embodiment
FTO substrate is prepared a method for copper zinc tin sulfur semiconductor film, and it specifically comprises:
S201, FTO electro-conductive glass cleaning step: FTO electro-conductive glass is put into successively each ultrasonic cleaning 10min of acetone, absolute ethyl alcohol and deionized water, then dry;
S202, in the ethylene glycol of 50ml, add 4mmol copper chloride hydrate, 2mmol zinc chloride and 2mmol stannous chloride hydrate successively after, utilize magnetic agitation to fully dissolving; Then, after adding 9mmol thiocarbamide and 1.28gPVP, utilizing magnetic agitation to fully dissolving, mixing and obtaining reaction precursor liquid;
S203, the conducting surface of the FTO electro-conductive glass cleaned up is put into there-necked flask down, then described reaction precursor liquid is poured in there-necked flask, there-necked flask is put into microwave oven and carries out isothermal reaction, wherein, reaction temperature is set to 200 DEG C, microwave power is set to 800W, and the reaction time is set to reaction 60min;
After isothermal reaction completes, the FTO electro-conductive glass depositing copper zinc tin sulfur semiconductor film is taken out from flask, with absolute ethyl alcohol and deionized water, three times are respectively cleaned to FTO electro-conductive glass respectively again, be the vacuumize carried out under the condition of 80 DEG C 5 hours again in temperature by described FTO electro-conductive glass, so just directly can prepare copper zinc tin sulfur semiconductor film on FTO electro-conductive glass.
The present invention the 3rd specific embodiment
FTO substrate is prepared a method for copper zinc tin sulfur semiconductor film, and it specifically comprises:
S301, FTO electro-conductive glass cleaning step: FTO electro-conductive glass is put into successively each ultrasonic cleaning 10min of acetone, absolute ethyl alcohol and deionized water, then dry;
S302, in the ethylene glycol of 50ml, add 4mmol copper chloride hydrate, 2mmol zinc chloride and 2mmol stannous chloride hydrate successively after, utilize magnetic agitation to fully dissolving; Then, after adding 11mmol thiocarbamide and 1.92gPVP, utilizing magnetic agitation to fully dissolving, mixing and obtaining reaction precursor liquid;
S303, the conducting surface of the FTO electro-conductive glass cleaned up is put into there-necked flask down, then described reaction precursor liquid is poured in there-necked flask, there-necked flask is put into microwave oven and carries out isothermal reaction, wherein, reaction temperature is set to 190 DEG C, microwave power is set to 900W, and the reaction time is set to reaction 50min;
After isothermal reaction completes, the FTO electro-conductive glass depositing copper zinc tin sulfur semiconductor film is taken out from flask, with absolute ethyl alcohol and deionized water, three times are respectively cleaned to FTO electro-conductive glass respectively again, be the vacuumize carried out under the condition of 80 DEG C 5 hours again in temperature by described FTO electro-conductive glass, so just directly can prepare copper zinc tin sulfur semiconductor film on FTO electro-conductive glass.
The present invention the 4th specific embodiment
FTO substrate is prepared a method for copper zinc tin sulfur semiconductor film, and it specifically comprises:
S401, FTO electro-conductive glass cleaning step: FTO electro-conductive glass is put into successively each ultrasonic cleaning 10min of acetone, absolute ethyl alcohol and deionized water, then dry;
S402, in the ethylene glycol of 50ml, add 4mmol copper chloride hydrate, 2mmol zinc chloride and 2mmol stannous chloride hydrate successively after, utilize magnetic agitation to fully dissolving; Then, after adding 7mmol thiocarbamide and 0.95gPVP, utilizing magnetic agitation to fully dissolving, mixing and obtaining reaction precursor liquid;
S403, the conducting surface of the FTO electro-conductive glass cleaned up is put into there-necked flask down, then described reaction precursor liquid is poured in there-necked flask, there-necked flask is put into microwave oven and carries out isothermal reaction, wherein, reaction temperature is set to 200 DEG C, microwave power is set to 700W, and the reaction time is set to reaction 60min;
After isothermal reaction completes, the FTO electro-conductive glass depositing copper zinc tin sulfur semiconductor film is taken out from flask, with absolute ethyl alcohol and deionized water, three times are respectively cleaned to FTO electro-conductive glass respectively again, be the vacuumize carried out under the condition of 80 DEG C 5 hours again in temperature by described FTO electro-conductive glass, so just directly can prepare copper zinc tin sulfur semiconductor film on FTO electro-conductive glass.
Obtained by above-mentioned, advantage of the present invention includes:
1, the coring and increment of lattice structure to CZTS semiconductive thin film that the conductivity of FTO electro-conductive glass, roughness and FTO electro-conductive glass are similar to CZTS has important function.
2, by regulating the concentration of thiocarbamide and PVP, the CZTS semiconductive thin film with varying particle size composition can be synthesized, and the strong adhesion between this semiconductive thin film and FTO electro-conductive glass.
3, the CZTS semiconductive thin film prepared on FTO electro-conductive glass, can directly be used as DSSC to electrode, replace traditional Pt to electrode, reduce the cost of DSSC, be conducive to industrialization and produce.
4, CZTS semiconductive thin film prepared by FTO electro-conductive glass, can directly be used for preparing CZTS thin-film solar cells, namely FTO electro-conductive glass is directly as the back electrode of CZTS thin-film solar cells, the CZTS semiconductive thin film prepared is as the absorbed layer of CZTS thin-film solar cells, then on absorbed layer, directly resilient coating is prepared, Window layer and top electrode, just can be prepared into CZTS thin-film solar cells, the production process of CZTS thin-film solar cells can not only be simplified like this, and greatly can also reduce the making input cost of CZTS thin-film solar cells.
5, equipment needed thereby and simple, the with low cost and speed of preparation technology are very fast, can directly obtain thing mutually evenly, well-crystallized, product that purity is higher.
More than that better enforcement of the present invention is illustrated, but the invention is not limited to described embodiment, those of ordinary skill in the art also can make all equivalent variations or replacement under the prerequisite without prejudice to spirit of the present invention, and these equivalent distortion or replacement are all included in the application's claim limited range.
Claims (10)
1. on FTO substrate, prepare a method for copper zinc tin sulfur semiconductor film, it is characterized in that: the method comprises:
A, solvent, Tong Yuan, zinc source, Xi Yuan, sulphur source and surfactant are mixed obtained reaction precursor liquid;
B, FTO electro-conductive glass fully to be contacted with reaction precursor liquid, under microwave condition fully after reaction, FTO electro-conductive glass prepares copper zinc tin sulfur semiconductor film.
2. a kind of method preparing copper zinc tin sulfur semiconductor film on FTO substrate according to claim 1, it is characterized in that: described copper source is copper chloride hydrate, described zinc source is zinc chloride, described Xi Yuan is stannous chloride hydrate, described sulphur source is thiocarbamide, and described surfactant is polyvinylpyrrolidone.
3. a kind of method preparing copper zinc tin sulfur semiconductor film on FTO substrate according to claim 1 or 2, is characterized in that: described steps A is specially: after adding copper source, zinc source and Xi Yuan in a solvent successively, utilizes magnetic agitation to fully dissolving; Then, after adding sulphur source and surfactant, utilizing magnetic agitation to fully dissolving, mixing and obtaining reaction precursor liquid.
4. a kind of method preparing copper zinc tin sulfur semiconductor film on FTO substrate according to claim 1 or 2, is characterized in that: the amount ratio of described copper source, zinc source, Xi Yuan, sulphur source, surfactant is: 1mmol:(0.4-0.6) mmol:(0.4-0.6) mmol:(1.2-3) mmol:(0.16-0.5) g.
5. a kind of method preparing copper zinc tin sulfur semiconductor film on FTO substrate according to claim 1, is characterized in that: described step B is specially:
The conducting surface of FTO electro-conductive glass is put into there-necked flask down, then described reaction precursor liquid is poured in there-necked flask, there-necked flask is put into microwave oven and carries out isothermal reaction, after isothermal reaction completes, the FTO electro-conductive glass depositing copper zinc tin sulfur semiconductor film is taken out from there-necked flask, with absolute ethyl alcohol and deionized water, FTO electro-conductive glass is cleaned respectively again, more fully dry.
6. a kind of method preparing copper zinc tin sulfur semiconductor film on FTO substrate according to claim 5, is characterized in that: described abundant drying, is specially: be the vacuumize carried out under the condition of 80 DEG C 5 hours in temperature by described FTO electro-conductive glass.
7. preparing DSSC to the application in electrode according to the copper zinc tin sulfur semiconductor film prepared by the method described in any one of claim 1-6.
8. according to the application of the copper zinc tin sulfur semiconductor film prepared by the method described in any one of claim 1-6 as absorbing layer of thin film solar cell.
9. load has the FTO electro-conductive glass of copper zinc tin sulfur semiconductor film, it is characterized in that: it is prepared according to the method for any one in claim 1-6.
10. load according to claim 9 has the application of the FTO electro-conductive glass of copper zinc tin sulfur semiconductor film in preparation thin-film solar cells.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109037042A (en) * | 2018-07-27 | 2018-12-18 | 金陵科技学院 | A method of copper-zinc-tin-sulfur film is prepared based on water nano ink |
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| CN103011261A (en) * | 2012-12-02 | 2013-04-03 | 桂林理工大学 | Solvothermal synthesis method of wurtzite structure CZTS(Se) (Copper Zinc Tin Sulfide) semiconductor material under synergistic effect of ultrasonic waves and microwaves |
| CN103050575A (en) * | 2012-12-15 | 2013-04-17 | 北京工业大学 | Method for preparing copper-zinc-tin-sulfide film through microwave method |
| CN103420411A (en) * | 2013-07-11 | 2013-12-04 | 南京航空航天大学 | Ultrasonic-assisted microwave controllable preparation method of Cu2ZnSnS4 nano-particles |
| WO2014106694A1 (en) * | 2013-01-02 | 2014-07-10 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Process for producing particles of chalcopyrite chosen from cu(inga)se2 and cu2znsns4 and pulverulent composition of particles thus obtained |
-
2015
- 2015-11-18 CN CN201510801054.2A patent/CN105470112A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011261A (en) * | 2012-12-02 | 2013-04-03 | 桂林理工大学 | Solvothermal synthesis method of wurtzite structure CZTS(Se) (Copper Zinc Tin Sulfide) semiconductor material under synergistic effect of ultrasonic waves and microwaves |
| CN103050575A (en) * | 2012-12-15 | 2013-04-17 | 北京工业大学 | Method for preparing copper-zinc-tin-sulfide film through microwave method |
| WO2014106694A1 (en) * | 2013-01-02 | 2014-07-10 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Process for producing particles of chalcopyrite chosen from cu(inga)se2 and cu2znsns4 and pulverulent composition of particles thus obtained |
| CN103420411A (en) * | 2013-07-11 | 2013-12-04 | 南京航空航天大学 | Ultrasonic-assisted microwave controllable preparation method of Cu2ZnSnS4 nano-particles |
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| CN109037042A (en) * | 2018-07-27 | 2018-12-18 | 金陵科技学院 | A method of copper-zinc-tin-sulfur film is prepared based on water nano ink |
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