CN103132034A - Quaternary single target radio frequency magnetron sputtering preparation method for membrane of copper indium gallium diselenide light absorbing layer - Google Patents
Quaternary single target radio frequency magnetron sputtering preparation method for membrane of copper indium gallium diselenide light absorbing layer Download PDFInfo
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- CN103132034A CN103132034A CN2011103884119A CN201110388411A CN103132034A CN 103132034 A CN103132034 A CN 103132034A CN 2011103884119 A CN2011103884119 A CN 2011103884119A CN 201110388411 A CN201110388411 A CN 201110388411A CN 103132034 A CN103132034 A CN 103132034A
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Abstract
The invention relates to a quaternary single target radio frequency magnetron sputtering preparation method for a membrane of a copper indium gallium diselenide light absorbing layer. The quaternary single target radio frequency magnetron sputtering preparation method for the membrane of the copper indium gallium diselenide light absorbing layer is characterized in that a copper indium gallium diselenide membrane is prepared by quaternary single target radio frequency magnetron sputtering, and a traditional follow-up selenylation annealing process is not related to. Firstly, two layers of molybdenum membranes are prepared on a soda-lime glass substrate by direct current magnetron sputtering as a metal back electrode, and then the copper indium gallium diselenide membrane is prepared on a molybdenum back electrode by radio frequency magnetron sputtering. The key point in a preparation process of the copper indium gallium diselenide membrane is that the copper indium gallium diselenide membrane is deposited on the molybdenum back electrode of high temperature so as to achieve synchronization of membrane growth with heat treatment. The copper indium gallium diselenide membrane prepared through the method has a copper pyrites crystal structure, the grain size is big, and the preferred orientation (220/240) is obvious. Columnar crystal particles penetrate through the upper surface and the lower surface of the membrane, and the membrane can be used as the light absorbing layer of a solar cell. The quaternary single target radio frequency magnetron sputtering preparation method is simple in technology, good in repeatability, low in preparation cost, safe, environment friendly and suitable for industrialized mass production.
Description
Technical field
The present invention relates to the photoelectric fields such as solar cell, thin-film material, particularly copper-indium-galliun-selenium film solar cell light absorbing zone thin film technology.
Background technology
Sun power is considered to environmental protection, use one of energy of most convenient, and it is inexhaustible.Solar cell is the important invention that realizes solar electrical energy generation, and it is mainly to utilize photovoltaic effect (photovoltaic effect) that luminous energy is directly changed into electric energy.Wherein copper-indium-galliun-selenium (CIGS) thin film solar cell has that cost is low, efficiency of conversion is high (20.3%), stable performance, low light level characteristic is good and the advantage such as environmentally friendly, is considered to the next generation's one of the most promising thin-film solar cells.
Copper-indium-galliun-selenium light absorbing zone thin film technology technology is the core technology of CIGS thin-film solar cells.At present, copper-indium-galliun-selenium light absorbing zone thin film technology method is mainly selenizing method after polynary coevaporation method and metal preformed layer.Wherein polynary coevaporation method can access surfacing, interior solid, the high-quality thin film of good crystallinity.But its requirement is accurately controlled velocity of evaporation and the steam output of a plurality of evaporation sources, and high and consistence of composition when being difficult to guarantee the big area film forming, therefore be difficult to realize large-scale industrial production to equipment requirements.After the metal preformed layer, the selenizing method can guarantee the homogeneity of big area film forming, is the first-selected technique that present industrialization prepares light absorbing zone, but its complex process, repeatable poor, energy consumption is higher, and this has all seriously restricted its large-scale industrialization and has produced.The invention provides a kind of with low cost, environmental friendliness, technique is simple, the high-quality copper indium gallium selenium absorption layer thin film technology method of favorable repeatability.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of CIGS thin-film solar cells light absorbing zone CIGS thin-film, the method is with low cost, environmental friendliness, and technique is simple, and favorable repeatability is fit to large-scale industrial production.
The present invention uses single quaternary CIGS target material, adopts the method for rf magnetron sputtering to prepare the CIGS thin-film that can be used as solar cell light absorption layer, and step of preparation process is as follows:
1. install Mo target and CuIn in the magnetron sputtering cavity
1-xGa
xSe
yThen target is arranged on cleaned soda lime glass substrates in cavity, and the sputter cavity is evacuated to 1x10
-3Below Pa, then substrate is heated, pass into purity greater than 99.99% Ar gas after substrate heating temperature is stable, use d.c. sputtering to deposit total thickness on substrate and be the molybdenum film of 0.5-1.5 μ m, as the molybdenum back electrode of thin-film solar cells;
2. keep certain underlayer temperature, on the soda-lime glass substrate of molybdenum back electrode, deposit thickness is the CIGS film of 1.0-3.0 μ m being coated with to use rf magnetron sputtering, obtains can be used as the CIGS thin-film of thin-film solar cells light absorbing zone;
Described CuIn
1-xGa
xSe
yTarget purity is greater than 99.9%, 0≤x in formula≤0.5,2≤y≤2.5;
In described step 1, double-deck Mo thin film technology condition is: substrate temperature is 25-600 ℃, the substrate rotating speed is 5-20rpm, target-substrate distance is 5-12cm, the Ar airshed is 20-100sccm, sputtering power is 80-200W, and the sputtering pressure of the first layer Mo is 1-5Pa, and corresponding sputtering time is 5-15min, the sputtering pressure of second layer Mo is 0.1-1.0Pa, and corresponding sputtering time is 10-25min;
In described step 2, CIGS thin film technology condition is: substrate temperature is 300-600 ℃, and the substrate rotating speed is 5-20rpm, and target-substrate distance is 3-12cm, the Ar airshed is 20-100sccm, radio-frequency sputtering power is 80-200W, and sputtering pressure is 0.1-5.0Pa, and sputtering time is 30-180min;
The complete rear sample of described step 2 plated film naturally cooling in cavity does not need through follow-up selenized annealing technique, and namely obtaining having yellow copper structure can be as the CIGS thin-film of thin-film solar cells light absorbing zone;
The prepared CIGS film surface of described step 2 is smooth, and compact structure, columnar grain run through the film upper and lower surface, and significantly (220/204) preferred orientation is arranged.
Beneficial effect of the present invention has:
1. use single quaternary CIGS target material to carry out sputter, directly obtain the CIGS film, avoided the complex control process of many targets sputter, improved the utilization ratio of material, be conducive to reduce the cost, and technique is simple, favorable repeatability;
2. control film quality by each sputtering parameter and target composition in the regulation and control sputter procedure, do not need to carry out follow-up selenizing or annealing process, more friendly to environment, be conducive to reduce the energy consumption Decrease production cost;
3. prepare film under certain substrate temperature, avoided in the traditional follow-up selenized annealing process of preparation CIGS film process at the inner stress that produces of film, thereby make film have better adhesivity, better lattice match and defective are still less arranged between rete, be conducive to prepare high-quality film.
Description of drawings
Fig. 1 is the surperficial SEM figure of CIGS thin-film prepared in the invention process case 1
Fig. 2 is the section S EM figure of CIGS thin-film prepared in the invention process case 1
Fig. 3 is that the EDS of CIGS thin-film prepared in the invention process case 1 can spectrogram
Fig. 4 is the XRD figure spectrum of CIGS thin-film prepared in the invention process case 1
Fig. 5 is the surperficial SEM figure of CIGS thin-film prepared in the invention process case 2
Fig. 6 is the section S EM figure of CIGS thin-film prepared in the invention process case 2
Fig. 7 is the XRD figure spectrum of CIGS thin-film prepared in the invention process case 2
Fig. 8 is the surperficial SEM figure of CIGS thin-film prepared in the invention process case 3
Fig. 9 is the section S EM figure of CIGS thin-film prepared in the invention process case 3
Figure 10 is that the EDS of CIGS thin-film prepared in the invention process case 3 can spectrogram
Figure 11 is the XRD figure spectrum of CIGS thin-film prepared in the invention process case 3
Concrete case study on implementation
Case study on implementation 1
Single target magnetic control sputtering preparation method of CIGS thin-film
(1) install Mo target and CuIn in the magnetron sputtering cavity
0.7Ga
0.3Se
2Then target is arranged on cleaned soda lime glass substrates in cavity, and the sputter cavity is evacuated to 1x10
-3Below Pa, then substrate is heated, pass into after a period of stabilisation purity greater than 99.99% Ar gas Deng substrate heating temperature, use d.c. sputtering to deposit the double-deck molybdenum film that total thickness is 0.5 μ m on soda lime glass substrates, its sputtering condition is: substrate temperature is 500 ℃, the substrate speed of rotation is 10rpm, target-substrate distance is 10cm, the Ar airshed is 100sccm, DC source power is 135W, and the first layer molybdenum sputtering pressure is 2.0Pa, and corresponding sputtering time is 10min, second layer molybdenum sputtering pressure is 1.0Pa, and corresponding sputtering time is 15min;
(2) the molybdenum layer sputter complete after, using radio-frequency sputtering source deposit thickness on the soda lime glass substrates that has plated the molybdenum back electrode is the CIGS film of 1.5 μ m, its sputtering condition is: substrate temperature is 500 ℃, the substrate speed of rotation is 10rpm, target-substrate distance is 4cm, and the Ar airshed is 50sccm, and radio-frequency sputtering power is 120W, sputtering pressure is 3.0Pa, and corresponding sputtering time is 30min; The complete rear sample of sputter is freely cooling in cavity, does not need through any selenized annealing technique, and namely obtaining having yellow copper structure can be as the CIGS thin-film of thin-film solar cells light absorbing zone.
Fig. 1 is the surperficial SEM figure of CIGS thin-film prepared in case study on implementation 1, Fig. 2 is the section S EM figure of CIGS thin-film prepared in case study on implementation 1, can be found out by Fig. 1 and Fig. 2, prepared CIGS film thickness is 1.5 μ m, the more smooth densification in surface, subsurface defect is less, good crystallinity; Can see simultaneously that between cigs layer film and Mo layer film, combination closely, demonstrates good adhesivity.Fig. 3 is that the EDS of CIGS thin-film prepared in case study on implementation 1 can spectrogram, can find out, only contains Cu, In, Ga and Se element in prepared CIGS film, does not find other impurity elements; The actual element atomic ratio of the CIGS film that the EDS energy spectrum analysis draws is Cu: In: Ga: Se=29.91: 15.49: 8.31: 46.29.Fig. 4 is the XRD figure spectrum of CIGS thin-film prepared in case study on implementation 1, can find out, prepared CIGS film has yellow copper structure.Simultaneously, (112) peak is 1: 0.4 with the strength ratio at (220/204) peak in the CIGS standard is general, and be 1: 8.9 by the strength ratio at (112) peak in the prepared CIGS film of case study on implementation 1 and (220/204) peak as can be seen from Figure 4, significantly (220/204) preferred orientation is arranged.
Case study on implementation 2
Single target magnetic control sputtering preparation method of CIGS thin-film
(1) install Mo target and CuIn in the magnetron sputtering cavity
0.75Ga
0.25Se
2.2Then target is arranged on cleaned soda lime glass substrates in cavity, and the sputter cavity is evacuated to 1x10
-3Below Pa, then substrate is heated, pass into after a period of stabilisation purity greater than 99.99% Ar gas Deng substrate heating temperature, use d.c. sputtering to deposit the double-deck molybdenum film that total thickness is 0.5 μ m on soda lime glass substrates, its sputtering condition is: substrate temperature is 550 ℃, the substrate speed of rotation is 10rpm, target-substrate distance is 8cm, the Ar airshed is 50sccm, DC source power is 80W, and the first layer molybdenum sputtering pressure is 2.5Pa, and corresponding sputtering time is 10min, second layer molybdenum sputtering pressure is 0.5Pa, and corresponding sputtering time is 15min;
(2) the molybdenum layer sputter complete after, using radio-frequency sputtering source deposit thickness on the soda lime glass substrates that has plated the molybdenum back electrode is the CIGS film of 1.2 μ m, its sputtering condition is: substrate temperature is 550 ℃, the substrate speed of rotation is 10rpm, target-substrate distance is 8cm, and the Ar airshed is 50sccm, and radio-frequency sputtering power is 80W, sputtering pressure is 0.2Pa, and corresponding sputtering time is 90min; The complete rear sample of sputter is freely cooling in cavity, does not need through any selenized annealing technique, and namely obtaining having yellow copper structure can be as the CIGS thin-film of thin-film solar cells light absorbing zone.
Fig. 5 is the surperficial SEM picture of CIGS thin-film prepared in case study on implementation 2, Fig. 6 is the section S EM picture of CIGS thin-film prepared in case study on implementation 2, can find out that prepared CIGS film thickness is 1.2 μ m, film surface is smooth, compact structure, good crystallinity, columnar grain runs through the whole upper and lower surface of film, can find out simultaneously that between cigs layer film and Mo layer film, combination is tight, matching degree is good.Fig. 7 is the XRD figure spectrum of CIGS thin-film prepared in case study on implementation 2, can find out, prepared CIGS film has yellow copper structure.Simultaneously, (112) peak is 1: 0.4 with the strength ratio at (220/204) peak in the CIGS standard is general, and be 1: 0.8 by the strength ratio at (112) peak in the prepared CIGS film of case study on implementation 2 and (220/204) peak as can be seen from Figure 7, (220/204) face preferential growth trend is obvious.
Case study on implementation 3
Single target magnetic control sputtering preparation method of CIGS thin-film
(1) install Mo target and CuIn in the magnetron sputtering cavity
0 75Ga
0.25Se
2Then target is arranged on cleaned soda lime glass substrates in cavity, and the sputter cavity is evacuated to 1x10
-3Below Pa, then substrate is heated, pass into after a period of stabilisation purity greater than 99.99% Ar gas Deng substrate heating temperature, use d.c. sputtering to deposit the double-deck molybdenum film that total thickness is 1.0 μ m on soda lime glass substrates, its sputtering condition is: substrate temperature is 600 ℃, the substrate speed of rotation is 12rpm, target-substrate distance is 8cm, the Ar airshed is 100sccm, DC source power is 144W, and the first layer molybdenum sputtering pressure is 2.0Pa, and corresponding sputtering time is 10min, second layer molybdenum sputtering pressure is 1.0Pa, and corresponding sputtering time is 15min;
(2) the molybdenum layer sputter complete after, using radio-frequency sputtering source deposit thickness on the soda lime glass substrates that has plated the molybdenum back electrode is the CIGS film of 2.5 μ m, its sputtering condition is: substrate temperature is 600 ℃, the substrate speed of rotation is 12rpm, target-substrate distance is 5cm, and the Ar airshed is 50sccm, and radio-frequency sputtering power is 180W, sputtering pressure is 2.0Pa, and corresponding sputtering time is 90min; The complete rear sample of sputter is freely cooling in cavity, does not need through any selenized annealing technique, and namely obtaining having yellow copper structure can be as the CIGS thin-film of thin-film solar cells light absorbing zone.
Fig. 8 is the surperficial SEM picture of CIGS thin-film prepared in case study on implementation 3, Fig. 9 is the section S EM picture of CIGS thin-film prepared in case study on implementation 3, can find out that prepared CIGS film thickness is 2.5 μ m, structure is finer and close, good crystallinity and obvious columnar growth is arranged, thick columnar grain runs through the whole upper and lower surface of film, can find out that between cigs layer film and Mo layer film, combination closely, has shown good adhesivity simultaneously.Figure 10 is that the EDS of CIGS thin-film prepared in case study on implementation 3 can spectrogram, can find out, only contains Cu, In, Ga and Se element in prepared CIGS film, does not find other impurity elements; The actual element atomic ratio of the CIGS film that the EDS energy spectrum analysis draws is Cu: In: Ga: Se=24.64: 19.95: 5.95: 49.46, and very approaching with the target composition, obviously do not lack selenium.Figure 11 is the XRD figure spectrum of CIGS thin-film prepared in case study on implementation 3, can find out, prepared CIGS film has single yellow copper structure.Simultaneously, (112) peak is 1: 0.4 with the strength ratio at (220/204) peak in the CIGS standard is general, and be 1: 11 by the strength ratio at (112) peak in the prepared CIGS film of case study on implementation 3 and (220/204) peak as can be seen from Figure 11, have significantly (220/204) preferred orientation.CIGS film with (220/204) face preferential growth more is conducive to obtain high efficiency battery.
Claims (6)
1. the single target radio frequency magnetron sputter of the quaternary of copper-indium-galliun-selenium light absorbing zone film preparation method, it is characterized in that, use single quaternary CIGS target material, sputtering parameter and selection target composition proportion by the regulation and control rf magnetron sputtering, directly preparation can be as the CIGS thin-film of solar cell light absorption layer, need not follow-up selenized annealing technique, it is characterized in that, the method preparation process is as follows:
(1) install Mo target and CuIn in the magnetron sputtering cavity
1-xGa
xSe
yThen target is arranged on cleaned soda lime glass substrates in cavity, and the sputter cavity is evacuated to 1x10
-3Below Pa, then substrate is heated, pass into purity greater than 99.99% Ar gas after substrate heating temperature is stable, use d.c. sputtering to deposit total thickness on substrate and be the molybdenum film of 0.5-1.5 μ m, as the molybdenum back electrode of thin-film solar cells;
(2) keep certain underlayer temperature, on the soda-lime glass substrate of molybdenum back electrode, deposit thickness is the CIGS film of 1.0-3.0 μ m being coated with to use rf magnetron sputtering, obtains can be used as the CIGS thin-film of thin-film solar cells light absorbing zone.
2. the single target radio frequency magnetron sputter of the quaternary of copper-indium-galliun-selenium light absorbing zone film according to claim 1 preparation method, is characterized in that described CuIn
1-xGa
xSe
yTarget purity is greater than 99.9%, 0≤x in formula≤0.5,2≤y≤2.5.
3. the single target radio frequency magnetron sputter of the quaternary of copper-indium-galliun-selenium light absorbing zone film according to claim 1 preparation method, it is characterized in that, in described step (1), double-deck Mo thin film technology condition is: substrate temperature is 25-600 ℃, the substrate rotating speed is 5-20rpm, target-substrate distance is 5-12cm, the Ar airshed is 20-100sccm, sputtering power is 80-200W, the sputtering pressure of the first layer Mo is 1-5Pa, corresponding sputtering time is 5-15min, the sputtering pressure of second layer Mo is 0.1-1.0Pa, and corresponding sputtering time is 10-25min.
4. the single target radio frequency magnetron sputter of the quaternary of copper-indium-galliun-selenium light absorbing zone film according to claim 1 preparation method, it is characterized in that, in described step (2), CIGS thin film technology condition is: substrate temperature is 300-600 ℃, the substrate rotating speed is 5-20rpm, target-substrate distance is 3-12cm, and the Ar airshed is 20-100sccm, and radio-frequency sputtering power is 80-200W, sputtering pressure is 0.1-5.0Pa, and sputtering time is 30-180min.
5. the single target radio frequency magnetron sputter of the quaternary of copper-indium-galliun-selenium light absorbing zone film according to claim 1 preparation method, it is characterized in that, the complete rear sample of plated film naturally cooling in cavity, do not need through follow-up selenized annealing technique, namely obtaining having yellow copper structure can be as the CIGS thin-film of thin-film solar cells light absorbing zone.
6. the single target radio frequency magnetron sputter of the quaternary of copper-indium-galliun-selenium light absorbing zone film according to claim 1 preparation method, it is characterized in that, prepared CIGS film surface is smooth, compact structure, thick columnar grain runs through the film upper and lower surface, and significantly (220/204) preferred orientation is arranged.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103531661A (en) * | 2013-10-22 | 2014-01-22 | 西南交通大学 | Preparation method of (220) orientated copper indium gallium selenium film |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102154622A (en) * | 2010-12-06 | 2011-08-17 | 电子科技大学 | Method for preparing copper-indium-gallium-selenium thin film serving as light absorbing layer of solar cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102154622A (en) * | 2010-12-06 | 2011-08-17 | 电子科技大学 | Method for preparing copper-indium-gallium-selenium thin film serving as light absorbing layer of solar cell |
Non-Patent Citations (1)
| Title |
|---|
| J.H.SHI等: ""Fabrication of Cu（In，Ga）Se2 thin films by sputtering from a single quaternary chalcogenide target"", 《PROGRESS IN PHOTOVOLTAICS: RESEARCH AND APPLICATIONS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103531661A (en) * | 2013-10-22 | 2014-01-22 | 西南交通大学 | Preparation method of (220) orientated copper indium gallium selenium film |
| CN103531661B (en) * | 2013-10-22 | 2016-02-03 | 西南交通大学 | A kind of CIGS thin-film preparation method of (220) orientation |
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Application publication date: 20130605 |