CN103014624B - Preparation method of light-absorbing film of solar cell - Google Patents
Preparation method of light-absorbing film of solar cell Download PDFInfo
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- CN103014624B CN103014624B CN201210550143.0A CN201210550143A CN103014624B CN 103014624 B CN103014624 B CN 103014624B CN 201210550143 A CN201210550143 A CN 201210550143A CN 103014624 B CN103014624 B CN 103014624B
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Abstract
The invention discloses a preparation method of a light-absorbing film of a solar cell. A copper indium gallium selenide layer is prepared by a physical vapor deposition technology; a substrate is heated through infrared heat radiation and the substrate temperature is controlled, so that the film forming uniformity is improved; an evaporation technology is controlled, so that an indium-rich phase is generated on the surface of the copper indium gallium selenide layer; a small amount of sulfur element is introduced on the surface of the copper indium gallium selenide layer by a vulcanizing method, that is, the copper indium gallium selenide layer is heated through light source irradiation to the surface; and hydrogen sulfide gas is inflated to vulcanize the copper indium gallium selenide layer. By adopting the preparation method, the problem that in the conventional contact heating way, the distribution of the substrate temperature is non-uniform is solved; the phase structure of the surface of the copper indium gallium selenide layer is optimized; the recombination of charge carriers in a spatial charge region is reduced; and the cell efficiency can be improved easily.
Description
One, technical field
The present invention relates to thin film solar cell technologies, specifically a kind of preparation method of solar cell light absorption layer film.
Two, background technology
Copper-indium-galliun-selenium (Cu (In, Ga) Se
2being called for short CIGS) thin-film solar cells is the hull cell that current photoelectric transformation efficiency is the highest, the most high conversion efficiency in its laboratory reached 20.3% in 2010, and CIGS battery has low cost of manufacture, capability of resistance to radiation is strong, the low light level is good advantage, is considered to the most promising solar cell of new generation.
CIGS light absorbing zone is the most crucial one deck of CIGS thin film solar cell.Battery many employings physical gas-phase deposition at present with high light photoelectric transformation efficiency prepares CIGS light absorbing zone.In this technique preparation process, the accurate control of underlayer temperature and uniform spatial distribution are formed mutually to the thing of CIGS has material impact.If underlayer temperature is skewness in substrate plane, then can cause the inequality of CIGS thin film thing phase composition everywhere in substrate plane, can dephasign be produced in temperature lower region, reduce the photoelectric transformation efficiency of battery.For the preparation of area battery, especially need the uniform spatial distribution improving underlayer temperature.Traditional silicon mode is the method for Contact Heating, the hot face of well heater is close to CIGS substrate glass planar, adopt heat conducting mode to silicon, but this Fa Yiyin substrate glass heated bending, depart from hot face, thus causing underlayer temperature spatial distribution uneven, the area substrate temperature departing from hot face is relatively low.
Three, summary of the invention
The present invention aims to provide a kind of preparation method of solar cell light absorption layer film, and technical problem to be solved improves the one-tenth film uniformity of light absorbing zone film, thus improve the photoelectric transformation efficiency of battery.
The preparation method of solar cell light absorption layer film of the present invention is copper-indium-galliun-selenium (CIGSe) thin-film solar cells light absorbing zone, adopts steaming legal system altogether standby and is heated by infrared emanation, it is characterized in that operating according to the following steps:
Substrate plating molybdenum glass substrate being placed in conventional multi-source thermal evaporation coating system is evacuated to 5 × 10
-4pa, rises to 1100-1250 DEG C, 900-1000 DEG C, 950-1100 DEG C and 200-300 DEG C keep constant respectively respectively by the electron gun furnace temperature of copper, indium, gallium and selenium; By underlayer temperature from room temperature to 250-450 DEG C (3-8 minute) keep constant, first to plating molybdenum glass substrate surface evaporation indium, gallium and selenium 10-15 minute; After indium, gallium and selenium evaporation terminate, underlayer temperature is warming up to 450-650 DEG C and intensification while copper steam-plating and selenium 12-16 minute, play calculating when wherein within 12-16 minute, being and reaching 450-650 DEG C with temperature; Copper and selenium evaporation terminate the constant evaporation indium of rear maintenance underlayer temperature, gallium and selenium 3-6 minute; After indium, gallium and selenium evaporation terminate, underlayer temperature was down to 300-400 DEG C in 15-30 minute, then naturally cools to room temperature with stove, obtain CIGS thin film.
The evaporation amount of copper, indium, gallium and selenium was regulated and controled by temperature and evaporation time.
The preparation method of solar cell light absorption layer film of the present invention is copper indium gallium sulphur selenium (CIGSSe) thin-film solar cells light absorbing zone, comprises common steaming and each unit process of sulfuration, it is characterized in that:
Described steam altogether be plating molybdenum glass substrate is placed in conventional multi-source thermal evaporation coating system substrate on and be evacuated to 5 × 10
-4pa, rises to 1100-1250 DEG C, 900-1000 DEG C, 950-1100 DEG C and 200-300 DEG C keep constant respectively respectively by the electron gun furnace temperature of copper, indium, gallium and selenium; By underlayer temperature from room temperature to 250-450 DEG C (3-8 minute) keep constant, first to plating molybdenum glass substrate surface evaporation indium, gallium and selenium 10-15 minute; After indium, gallium and selenium evaporation terminate, underlayer temperature is warming up to 450-650 DEG C and intensification while copper steam-plating and selenium 12-16 minute, play calculating when wherein within 12-16 minute, being and reaching 450-650 DEG C with temperature; Copper and selenium evaporation terminate the constant evaporation indium of rear maintenance underlayer temperature, gallium and selenium 3-6 minute; After indium, gallium and selenium evaporation terminate, underlayer temperature was down to 300-400 DEG C in 15-30 minute, then naturally cools to room temperature with stove, obtain CIGS thin film;
The evaporation amount of copper, indium, gallium and selenium was regulated and controled by temperature and evaporation time.
Described sulfuration described CIGS thin film is placed to be rapidly heated on the substrate of stove, is evacuated to 5 × 10 in stove
-1pa, passes into argon gas and hydrogen sulfide in stove, the total flux 300-400sccm of argon gas and hydrogen sulfide, and throughput ratio is 20-50:1; Make temperature rise to 350-550 DEG C and be incubated 5-60 minute by halogen tungsten lamp irradiation, close halogen tungsten lamp after being cooled to 200-400 DEG C subsequently, naturally cool to room temperature, obtain CIGSSe film.
The equipment that the present invention prepares CIGS thin film employing by coevaporation method is multi-source thermal evaporation coating system, is made up of parts such as mechanical pump, molecular pump, vacuum cavity, electron gun stove, temperature controller, substrate heater, substrate rotation mechanism, slide valve, vacuumometers.This system can realize multiple evaporation source independence accurate temperature controlling, simultaneously can to silicon temperature control, for the preparation of multi-element compounds semiconductor film.
The type of heating of substrate heater is noncontact heating, keeps 1-5 millimeter spacing between well heater and substrate, and well heater passes through the mode of infrared emanation to silicon, guarantees that substrate is heated evenly everywhere.
The concrete steps that coevaporation method of the present invention prepares CIGS thin film are as follows:
1, plating molybdenum glass substrate is fixed on the substrate of multi-source thermal evaporation coating system, closes cavity, with mechanical pump and molecular pump, the background vacuum of inside cavity is evacuated to 5 × 10
-4pa, starts electron gun stove well heater, and guarantees electron gun stove flapper closure.
2, the electron gun furnace temperature of copper, indium, gallium, selenium is risen to respectively 1100-1250 DEG C, 900-1000 DEG C, 950-1100 DEG C, 200-300 DEG C, and keep constant.
3, substrate heater heats up by room temperature, within 3-8 minute, rise to 250-450 DEG C and keep constant, now open indium, gallium, selenium electron gun fender plate start first stage evaporation, to the evaporation of plating molybdenum glass substrate indium, gallium, selenium, after 10-15 minute, evaporation terminates the first stage, close indium, gallium electron gun fender plate, selenium electron gun fender plate is opened all the time in evaporate process; Subordinate phase evaporation, substrate heater heats up by 250-450 DEG C, open copper electron gun stove plate washer simultaneously, to the evaporation of plating molybdenum glass substrate copper, selenium, within 3-6 minute, back substrate heater temperature rises to 450-650 DEG C and keeps constant, start timing, after 12-16 minute, subordinate phase evaporation terminates this moment, closes copper electron gun stove plate washer; Phase III evaporation, this step silicon actuator temperature is still 450-650 DEG C and keeps constant, open indium, gallium electron gun fender plate, to the evaporation of plating molybdenum glass substrate indium, gallium, selenium, after 3-6 minute, evaporation terminates the phase III, close indium, gallium, selenium electron gun fender plate, substrate heater slow cooling, is down to 300-400 DEG C after 15-30 minute, then closes substrate heater, Temperature fall, to room temperature, obtains CIGS thin film.
CIGS thin film good crystallinity prepared by the inventive method, its X-ray diffraction spectrum (Fig. 1) shows that this CIGS thin film is yellow copper structure, it is larger that scanning electron microscope (SEM) image (Fig. 2) shows CIGS grain-size, and Raman spectrum (Raman) (Fig. 3) shows that CIGS top layer exists the rich indium phase (Cu (In, Ga) useful to battery performance
3se
5).
The equipment that hydrogen sulfide sulfuration CIGS thin film prepares CIGSSe film adopts the stove that is rapidly heated, be made up of parts such as mechanical pump, silica tube vacuum cavity, halogen tungsten lamp well heater, temperature control system, air-path control system, vacuumometer, exhaust treatment systems, concrete steps are as follows:
4, open the silica tube cavity of the atmosphere furnace that is rapidly heated, CIGS thin film is placed on substrate, close cavity, with mechanical pump, the background vacuum of inside cavity is evacuated to 5 × 10
-1pa.
5, regulate the throughput ratio of argon gas and hydrogen sulfide to 20-50:1.
6, substrate heating system is opened, with halogen tungsten lamp irradiation CIGS thin film surface, it is heated, within 5-20 minute, rise to 350-550 DEG C and be incubated 5-60 minute, slow cooling closes halogen tungsten lamp to during 200-400 DEG C afterwards, naturally cool to room temperature, obtain CIGSSe film, close argon gas and hydrogen sulfide, sulfuration terminates.
Adopt contactless substrate heating method can improve the uniform spatial distribution of underlayer temperature, especially for the suitability for industrialized production of area battery and the preparation of flexible solar battery significant.
The one-tenth phase control of CIGS thin film has vital impact for battery efficiency.Research shows, the existence of the rich indium phase in CIGS thin film top layer, and introduces a small amount of element sulphur generation copper indium gallium sulphur on top layer, being with of CIGS/CdS heterojunction can be made to be optimized, and reduce the Carrier recombination of space charge region, improve battery efficiency.
The inventive method not only avoid the problem of conventional contact type of heating substrate temperature profile inequality, also optimizes the Surface Phases structure of copper-indium-galliun-selenium, decreases the Carrier recombination of space charge region, is conducive to improving battery efficiency.
Four, accompanying drawing explanation
Fig. 1 is the XRD spectra of CIGS thin film of the present invention.
Fig. 2 is the SEM image of CIGS thin film of the present invention
Fig. 3 is the Raman spectrogram of CIGS thin film of the present invention.
Fig. 4 is the structural representation of CIGS battery.
Fig. 5 is the section SEM image of CIGS battery.
Fig. 6 is the IV curve of CIGS battery.
Fig. 7 is the Raman spectrogram of CIGSSe film of the present invention.
Five, embodiment
The preparation of embodiment 1:CIGS film
1, plating molybdenum glass substrate is fixed on the substrate of multi-source thermal evaporation coating system, closes cavity, with mechanical pump and molecular pump, the background vacuum of inside cavity is evacuated to 5 × 10
-4pa, starts electron gun stove well heater, and guarantees electron gun stove flapper closure.
2, the electron gun furnace temperature of copper, indium, gallium, selenium is risen to respectively 1100-1250 DEG C, 900-1000 DEG C, 950-1100 DEG C, 200-300 DEG C, and keep constant.
3, substrate heater heats up by room temperature, within 3-8 minute, rise to 250-450 DEG C and keep constant, now open indium, gallium, selenium electron gun fender plate start first stage evaporation, to the evaporation of plating molybdenum glass substrate indium, gallium, selenium, after 10-15 minute, evaporation terminates the first stage, close indium, gallium electron gun fender plate, selenium electron gun fender plate is opened all the time in evaporate process; Subordinate phase evaporation, substrate heater heats up by 250-450 DEG C, open copper electron gun stove plate washer simultaneously, to the evaporation of plating molybdenum glass substrate copper, selenium, within 3-6 minute, back substrate heater temperature rises to 450-650 DEG C and keeps constant, start timing, after 12-16 minute, subordinate phase evaporation terminates this moment, closes copper electron gun stove plate washer; Phase III evaporation, this step silicon actuator temperature is still 450-650 DEG C and keeps constant, open indium, gallium electron gun fender plate, to the evaporation of plating molybdenum glass substrate indium, gallium, selenium, after 3-6 minute, evaporation terminates the phase III, close indium, gallium, selenium electron gun fender plate, substrate heater slow cooling, is down to 300-400 DEG C after 15-30 minute, then closes substrate heater, Temperature fall, to room temperature, obtains CIGS thin film.
Embodiment 2:
Prepare solar cell by CIGS thin film of the present invention, as shown in Figure 4, preparation method is ordinary method to its structure, and idiographic flow is as follows:
1, on soda-lime glass, the molybdenum dorsum electrode layer of 600 nanometer thickness is plated with direct current magnetron sputtering process;
2, on plating molybdenum glass, the CIGS thin film light absorbing zone of 1.8 micron thickness is prepared with coevaporation method;
3, the Cadmium Sulfide buffer layer of 50 nanometer thickness is prepared with chemical baths;
4, the native oxide zinc layers of 100 nanometer thickness is prepared with magnetron sputtering method;
5, the aluminum-doped zinc oxide transparent conducting window layer of 1.5 micron thickness is prepared with magnetron sputtering method;
6, nickel aluminum gate electrode is prepared by method of evaporation.
As shown in Figure 5, test under the condition of illumination AM1.5, its battery IV rational curve is shown in Fig. 6 to its section of CIGS thin film solar cell SEM photo prepared by the present embodiment, and the open circuit voltage of this battery is 547mV, and short-circuit current is 31.5mA/cm
2, packing factor is 60%, and photoelectric transformation efficiency is 10.3%.
The preparation of embodiment 3:CIGSSe film
1, open the silica tube cavity of the atmosphere furnace that is rapidly heated, CIGS thin film prepared by embodiment 1 is placed on substrate, close cavity, with mechanical pump, the background vacuum of inside cavity is evacuated to 5 × 10
-1pa.
2, regulate the throughput ratio of argon gas and hydrogen sulfide to 20-50:1, total flux 300-400sccm.
3, substrate heating system is opened, with halogen tungsten lamp irradiation CIGS thin film surface, it is heated, within 5-20 minute, rise to 350-550 DEG C and be incubated 5-60 minute, slow cooling closes halogen tungsten lamp to during 200-400 DEG C afterwards, naturally cool to room temperature, obtain CIGSSe film, close argon gas and hydrogen sulfide, sulfuration terminates.
As shown in Figure 7, as can be seen from Figure 7 CIGSSe film surface cures the Raman spectrum of CIGSSe film prepared by the present embodiment, generates copper indium gallium sulphur (Cu (In, Ga) S
2), inside is still copper-indium-galliun-selenium (Cu (In, Ga) Se
2) phase.
Claims (2)
1. a preparation method for solar cell light absorption layer film, is characterized in that operating according to the following steps:
Substrate plating molybdenum glass substrate being placed in multi-source thermal evaporation coating system is evacuated to 5 × 10
-4pa, rises to 1100-1250 DEG C, 900-1000 DEG C, 950-1100 DEG C and 200-300 DEG C keep constant respectively respectively by the electron gun furnace temperature of copper, indium, gallium and selenium; Underlayer temperature be warming up to 250-450 DEG C and keep constant, first to plating molybdenum glass substrate surface evaporation indium, gallium and selenium 10-15 minute; After indium, gallium and selenium evaporation terminate, underlayer temperature is warming up to 450-650 DEG C and intensification while copper steam-plating and selenium 12-16 minute; Copper and selenium evaporation terminate rear maintenance underlayer temperature constant evaporation again indium, gallium and selenium 3-6 minute; After indium, gallium and selenium evaporation terminate, underlayer temperature is down to room temperature and obtains CIGS thin film;
The type of heating of substrate heater is noncontact heating, keeps 1-5 millimeter spacing between well heater and substrate, and well heater passes through the mode of infrared emanation to silicon, guarantees that substrate is heated evenly everywhere.
2. a preparation method for solar cell light absorption layer film, comprises common steaming and each unit process of sulfuration, it is characterized in that:
Described steam altogether be plating molybdenum glass substrate is placed in multi-source thermal evaporation coating system substrate on and be evacuated to 5 × 10
-4pa, rises to 1100-1250 DEG C, 900-1000 DEG C, 950-1100 DEG C and 200-300 DEG C keep constant respectively by the electron gun furnace temperature of copper, indium, gallium and selenium; Underlayer temperature be warming up to 250-450 DEG C and keep constant, first to plating molybdenum glass substrate surface evaporation indium, gallium and selenium 10-15 minute; After indium, gallium and selenium evaporation terminate, underlayer temperature is warming up to 450-650 DEG C and intensification while copper steam-plating and selenium 12-16 minute; Copper and selenium evaporation terminate rear maintenance underlayer temperature constant evaporation again indium, gallium and selenium 3-6 minute; After indium, gallium and selenium evaporation terminate, underlayer temperature is down to room temperature and obtains CIGS thin film; The type of heating of substrate heater is noncontact heating, keeps 1-5 millimeter spacing between well heater and substrate, and well heater passes through the mode of infrared emanation to silicon, guarantees that substrate is heated evenly everywhere;
Described sulfuration described CIGS thin film is placed to be rapidly heated on the substrate of stove, is evacuated to 5 × 10 in stove
-1pa, passes into argon gas and hydrogen sulfide in stove, the total flux 300-400sccm of argon gas and hydrogen sulfide, and the throughput ratio of argon gas and hydrogen sulfide is 20-50:1; Make temperature rise to 350-550 DEG C and be incubated 5-60 minute by halogen tungsten lamp irradiation, be down to room temperature subsequently, obtain CIGSSe film.
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| CN103710668B (en) * | 2013-12-12 | 2015-09-16 | 深圳先进技术研究院 | The preparation method of CIGS thin-film |
| CN107248534B (en) * | 2017-05-27 | 2018-10-16 | 华中科技大学 | A kind of semiconducting alloy film of ingredient continuous gradation and its preparation method and application |
| CN107475681B (en) * | 2017-08-09 | 2020-01-31 | 领凡新能源科技(北京)有限公司 | Method for uniformly controlling temperature of large-area flexible substrate |
| CN109385602B (en) * | 2018-07-05 | 2020-11-27 | 研创应用材料（赣州）股份有限公司 | Uniform surface shape deposition evaporation device and method |
| CN110416367B (en) * | 2019-08-14 | 2020-12-01 | 尚越光电科技股份有限公司 | Method for preparing large-area uniform CIGS thin-film solar cell by using In-Ga alloy evaporation source |
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