CN102751178B - Method for preparing thin-film solar cell p-n junction - Google Patents
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- CN102751178B CN102751178B CN201210128151.6A CN201210128151A CN102751178B CN 102751178 B CN102751178 B CN 102751178B CN 201210128151 A CN201210128151 A CN 201210128151A CN 102751178 B CN102751178 B CN 102751178B
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Abstract
The invention discloses a method for preparing a thin-film solar cell p-n junction. The method includes the following steps of cleaning a substrate, drying the substrate by nitrogen, placing the substrate on a substrate table in a cavity of a plasma chemical vapor deposition system, placing a raw material containing tins and a raw material containing sulfurs into two crucibles respectively, placing the two crucibles into a raw material evaporation device of the plasma chemical vapor deposition system, closing the cavity, vacuumpumping, feeding argon to produce an argon plasma, subjecting the cavity of the plasma chemical vapor deposition system and the substrate in the cavity to a cleaning treatment by the argon plasma, heating the substrate, preparing an n type tin sulfur film and a p type tin sulfur film on the substrate surface which is cleaned, subjecting the prepared n type and the p type tin sulfur films to a vacuum annealing in the cavity of the plasma chemical vapor deposition system, and cooling the n type and the p type tin sulfur films subjected to the annealing treatment in an argon environment to the room temperature. The method is simple in preparing process and can meet a requirement of a large area and high speed deposition.
Description
Technical field
The invention belongs to technical field of thin-film solar, more specifically, relate to a kind of method of preparing solar battery p-n junction.
Background technology
Compare traditional fossil energy, solar energy is a kind of clean regenerative resource, and the photovoltaic effect of therefore take more and more comes into one's own as basic solar cell.And absorbed layer thin film technique is occupied considerable status in the research of the solar cell of high-efficiency and low-cost with in producing.Along with the research and development to solar cell, cheap, efficient photoelectric conversion material more and more comes into one's own.Stannous sulfide is a kind of photoelectric material of asepsis environment-protecting, and its optics direct band gap is 1.3eV, approach the best energy gap 1.5eV of solar cell material, there is the very large absorption coefficient of light simultaneously, theoretical energy conversion efficiency can reach 25%, therefore has broad application prospects.At present, by the method for physics and chemistry, all can prepare all comparatively excellent stannous sulfide thin films of quality.
At present, in the preparation process of solar cell, normally the thin-film materials such as transparent conductive film, light absorbing zone, window material and anti-reflection layer are deposited on respectively on a substrate, wherein the preparation of p-n junction is the important step in thin-film solar cells, and it affects cost of manufacture and the quality of monoblock battery.In the making of solar cell,, there is stress problem in the stack of plural layers, affects adhesion of thin film between film, and then affect cost of manufacture and the useful life of thin-film solar cells.Meanwhile, the preparation of traditional p-n/p-i-n knot, need to introduce complicated doping process, has increased cost of manufacture, has also extended the production cycle.Therefore, a kind of energy meets simply, the preparation technology of p-n junction is current problem demanding prompt solution efficiently.
Summary of the invention
Defect for prior art, the object of the present invention is to provide a kind of method of preparing hull cell p-n knot, its abundant raw material, cheap, environmental friendliness, and preparation technology is simple, can meet the requirement of large area, high-speed deposition, and this method can avoid using the impact on hull cell of stress between complicated doping process and heterogeneous membrane.
For achieving the above object, the invention provides a kind of method of preparing thin-film solar cells p-n junction, comprise the steps:
(1) clean substrate, and with nitrogen drying;
(2) will clean and dried substrate is placed on the chip bench in the cavity of plasma chemical vapor deposition system;
(3) stanniferous and raw material sulphur are put in respectively in two crucibles, and put into the raw materials evaporate device of plasma chemical vapor deposition system;
(4) close the cavity of plasma chemical vapor deposition system, be evacuated to 5 * 10-3～8 * 10-5Pa;
(5) pressure with 30～150Pa passes into argon gas 20～100sccm, to produce argon plasma;
(6) utilize the cavity of argon plasma plasma chemical gas-phase deposition system and the substrate in cavity to carry out clean, in 10～30 minutes processing times, the power of argon plasma is 10～100W;
(7) open the heater on chip bench, substrate is heated, heating-up temperature is 200～400 ℃;
(8) open raw materials evaporate device, in plasma chemical vapor deposition system, pass into argon gas and hydrogen, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared N-shaped tin sulphur film, wherein argon flow amount is 10～80sccm, hydrogen flowing quantity is 5～40sccm, and plasma power is 50～300W, pressure 50～150Pa, raw materials evaporate temperature 50 C～1200 ℃, sedimentation time 20～150 minutes;
(9) close hydrogen, in plasma chemical vapor deposition system, pass into argon gas, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared p-type tin sulphur film, argon flow amount 10～80sccm wherein, plasma power is 50～300W, plasma pressure 100～150Pa, raw materials evaporate temperature 50 C～1200 ℃, sedimentation time 20～120 minutes;
(10) close plasma, and stop passing into argon gas;
(11) the heater temperature on rising chip bench is carried out vacuum annealing to the N-shaped tin sulphur film of preparing and p-type tin sulphur film, 300～550 ℃ of annealing temperatures, annealing time 30～150 minutes in the cavity of plasma chemical vapor deposition system;
(12) in the cavity of plasma chemical vapor deposition system, pass into argon gas, the N-shaped tin sulphur film after annealing in process and p-type tin sulphur film are cooled to room temperature in ar gas environment, to form p-n junction.
Stanniferous and raw material sulphur comprises the sub-tin powder of nano-sulfurization, the compound of simple substance tin, elemental sulfur or stanniferous and element sulphur.
Substrate comprises silicon chip, soda-lime glass, quartz glass, transparent conducting glass.
The quantity of raw materials evaporate device is more than 2 or 2, and raw materials evaporate device is provided with baffle plate, for controlling raw materials evaporate time and speed.
Stanniferous and raw material sulphur can be put into respectively different raw materials evaporate devices.
Plasma activated chemical vapour deposition method applying plasma can be microwave plasma, radio frequency plasma.
The above technical scheme of conceiving by the present invention, compared with prior art, the present invention has following beneficial effect:
1, preparation method is simple: the difference of tin and element sulphur proportioning, thereby make tin sulphur film to the transformation of N-shaped, prepare p-n by p-type, therefore, this method is utilized the characteristic of tin sulphur thin-film material self, adopt hydrogen obtain hydrogen sulfide with reacting of element sulphur in cavity and extract out from cavity by vacuum system, and then the proportioning of two kinds of elements in change cavity, thereby prepare the p-n junction of solar cell; This preparation method has avoided the introducing of the preparation of multilayer film in the preparation process of p-n junction and the doping process of complexity, greatly reduces cost of manufacture, has shortened fabrication cycle; Meanwhile, this method can, by the proportioning of the suitable various elements of adjusting, obtain having the semi-conducting material of different energy gaps.
2, abundant raw material, nontoxic: adopt tin and element sulphur in this method, two kinds of elements are environment-friendly material, avoid the pollution to environment, simultaneously, thiostannate belongs to IV-VI family semi-conducting material, is also important semi-conducting material, and it comprises multiple compounds form.Stannous sulfide is a kind of important semi-conducting material wherein, its asepsis environment-protecting, and abundant raw material, theoretical energy conversion efficiency can reach 25%.
3, p-n junction constituent is simple: in this method, the preparation of p-n junction forms by tin and sulphur, does not carry out complicated doping process, therefore, has avoided the impact on adhesive force of stress between heterogeneous membrane, has increased the useful life of film.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The method that the present invention prepares thin-film solar cells p-n junction comprises the steps:
(1) clean substrate, and with nitrogen drying;
(2) will clean and dried substrate is placed on the chip bench in the cavity of plasma chemical vapor deposition system; In the present embodiment, substrate comprises silicon chip, soda-lime glass, quartz glass, transparent conducting glass;
(3) stanniferous and raw material sulphur are put in respectively in two crucibles, and put into the raw materials evaporate device of plasma chemical vapor deposition system; Stanniferous and raw material sulphur comprises the sub-tin powder of nano-sulfurization, the compound of simple substance tin, elemental sulfur or stanniferous and element sulphur, and can put into different raw materials evaporate devices; The quantity of raw materials evaporate device is more than 2 or 2, and raw materials evaporate device is provided with baffle plate, for controlling raw materials evaporate time and speed.
(4) close the cavity of plasma chemical vapor deposition system, be evacuated to 5 * 10-3～8 * 10-5Pa;
(5) pressure with 30～150Pa passes into argon gas 20～100sccm, to produce argon plasma;
(6) utilize the cavity of argon plasma plasma chemical gas-phase deposition system and the substrate in cavity to carry out clean, in 10～30 minutes processing times, the power of argon plasma is 10～100W;
(7) open the heater on chip bench, substrate is heated, heating-up temperature is 200～400 ℃;
(8) open raw materials evaporate device, in plasma chemical vapor deposition system, pass into argon gas and hydrogen, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared N-shaped tin sulphur film, wherein argon flow amount is 10～80sccm, hydrogen flowing quantity is 5～40sccm, and plasma power is 50～300W, pressure 50～150Pa, raw materials evaporate temperature 50 C～1200 ℃, sedimentation time 20～150 minutes; Plasma activated chemical vapour deposition method applying plasma can be microwave plasma, radio frequency plasma;
(9) close hydrogen, in plasma chemical vapor deposition system, pass into argon gas, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared p-type tin sulphur film, argon flow amount 10～80sccm wherein, plasma power is 50～300W, plasma pressure 100～150Pa, raw materials evaporate temperature 50 C～1200 ℃, sedimentation time 20～120 minutes;
(10) close plasma, and stop passing into argon gas;
(11) the heater temperature on rising chip bench is carried out vacuum annealing to the N-shaped tin sulphur film of preparing and p-type tin sulphur film, 300～550 ℃ of annealing temperatures, annealing time 30～150 minutes in the cavity of plasma chemical vapor deposition system;
(12) in the cavity of plasma chemical vapor deposition system, pass into argon gas, the N-shaped tin sulphur film after annealing in process and p-type tin sulphur film are cooled to room temperature in ar gas environment, to form p-n junction.
Embodiment 1
(1) clean to be the substrate of transparent conducting glass, and with nitrogen drying;
(2) will clean and dried substrate is placed on the chip bench in the cavity of plasma chemical vapor deposition system;
(3) take respectively stannous chloride and sodium thiosulfate 4.75g and 12.4g, be placed in two crucibles, and put into the raw materials evaporate device of plasma chemical vapor deposition system;
(4) close the cavity of plasma chemical vapor deposition system, be evacuated to 6 * 10-3Pa;
(5) pressure with 40Pa passes into argon gas 30sccm, to produce argon plasma;
(6) utilize the cavity of argon plasma plasma chemical gas-phase deposition system and the substrate in cavity to carry out clean, in 20 minutes processing times, the power of argon plasma is 30W;
(7) open the heater on chip bench, substrate is heated, heating-up temperature is 300 ℃;
(8) open raw materials evaporate device, in plasma chemical vapor deposition system, pass into argon gas and hydrogen, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared N-shaped tin sulphur film, wherein argon flow amount is 30sccm, hydrogen flowing quantity is 30sccm, and plasma power is 150W, pressure 90Pa, 600 ℃ of raw materials evaporate temperature, sedimentation time 40 minutes;
(9) close hydrogen, in plasma chemical vapor deposition system, pass into argon gas, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared p-type tin sulphur film, argon flow amount 50sccm wherein, plasma power is 150W, plasma pressure 80Pa, 600 ℃ of raw materials evaporate temperature, sedimentation time 40 minutes;
(10) close plasma, and stop passing into argon gas;
(11) the heater temperature on rising chip bench is carried out vacuum annealing to the N-shaped tin sulphur film of preparing and p-type tin sulphur film, 350 ℃ of annealing temperatures, annealing time 60 minutes in the cavity of plasma chemical vapor deposition system;
(12) in the cavity of plasma chemical vapor deposition system, pass into argon gas, the N-shaped tin sulphur film after annealing in process and p-type tin sulphur film are cooled to room temperature in ar gas environment, to form p-n junction.
Embodiment 2
(1) clean to be the substrate of quartz glass, and with nitrogen drying;
(2) will clean and dried substrate is placed on the chip bench in the cavity of plasma chemical vapor deposition system;
(3) take respectively stannous chloride and elemental sulfur 4.75g and 1.6g, be placed in respectively in two crucibles, and put into the raw materials evaporate device of plasma chemical vapor deposition system;
(4) close the cavity of plasma chemical vapor deposition system, be evacuated to 2 * 10-4Pa;
(5) pressure with 50Pa passes into argon gas 50sccm, to produce argon plasma;
(6) utilize the cavity of argon plasma plasma chemical gas-phase deposition system and the substrate in cavity to carry out clean, in 30 minutes processing times, the power of argon plasma is 50W;
(7) open the heater on chip bench, substrate is heated, heating-up temperature is 350 ℃;
(8) open raw materials evaporate device, in plasma chemical vapor deposition system, pass into argon gas and hydrogen, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared N-shaped tin sulphur film, wherein argon flow amount is 50sccm, hydrogen flowing quantity is 20sccm, and plasma power is 150W, pressure 100Pa, 450 ℃ of raw materials evaporate temperature, sedimentation time 40 minutes;
(9) close hydrogen, in plasma chemical vapor deposition system, pass into argon gas, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared p-type tin sulphur film, argon flow amount 50sccm wherein, plasma power is 150W, plasma pressure 100Pa, 450 ℃ of raw materials evaporate temperature, sedimentation time 40 minutes;
(10) close plasma, and stop passing into argon gas;
(11) the heater temperature on rising chip bench is carried out vacuum annealing to the N-shaped tin sulphur film of preparing and p-type tin sulphur film, 400 ℃ of annealing temperatures, annealing time 60 minutes in the cavity of plasma chemical vapor deposition system;
(12) in the cavity of plasma chemical vapor deposition system, pass into argon gas, the N-shaped tin sulphur film after annealing in process and p-type tin sulphur film are cooled to room temperature in ar gas environment, to form p-n junction.
Embodiment 3
(1) clean to be the substrate of transparent conducting glass, and with nitrogen drying;
(2) will clean and dried substrate is placed on the chip bench in the cavity of plasma chemical vapor deposition system;
(3) will take respectively 1.3g and 3.75g and be placed in respectively in two crucibles containing butter of tin and sodium thiosulfate, and put into the raw materials evaporate device of plasma chemical vapor deposition system;
(4) close the cavity of plasma chemical vapor deposition system, be evacuated to 8 * 10-3Pa;
(5) pressure with 50Pa passes into argon gas 40sccm, to produce argon plasma;
(6) utilize the cavity of argon plasma plasma chemical gas-phase deposition system and the substrate in cavity to carry out clean, in 25 minutes processing times, the power of argon plasma is 50W;
(7) open the heater on chip bench, substrate is heated, heating-up temperature is 250 ℃;
(8) open raw materials evaporate device, in plasma chemical vapor deposition system, pass into argon gas and hydrogen, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared N-shaped tin sulphur film, wherein argon flow amount is 50sccm, hydrogen flowing quantity is 30sccm, and plasma power is 200W, pressure 100Pa, 550 ℃ of raw materials evaporate temperature, sedimentation time 30 minutes;
(9) close hydrogen, in plasma chemical vapor deposition system, pass into argon gas, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared p-type tin sulphur film, argon flow amount 50sccm wherein, plasma power is 200W, plasma pressure 120Pa, 550 ℃ of raw materials evaporate temperature, sedimentation time 30 minutes;
(10) close plasma, and stop passing into argon gas;
(11) the heater temperature on rising chip bench is carried out vacuum annealing to the N-shaped tin sulphur film of preparing and p-type tin sulphur film, 350 ℃ of annealing temperatures, annealing time 90 minutes in the cavity of plasma chemical vapor deposition system;
(12) in the cavity of plasma chemical vapor deposition system, pass into argon gas, the N-shaped tin sulphur film after annealing in process and p-type tin sulphur film are cooled to room temperature in ar gas environment, to form p-n junction.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (6)
1. a method of preparing thin-film solar cells p-n junction, is characterized in that, comprises the steps:
(1) clean substrate, and with nitrogen drying;
(2) will clean and dried substrate is placed on the chip bench in the cavity of plasma chemical vapor deposition system;
(3) stanniferous and raw material sulphur are put in respectively in two crucibles, and put into the raw materials evaporate device of plasma chemical vapor deposition system;
(4) close the cavity of plasma chemical vapor deposition system, be evacuated to 5 * 10-3～8 * 10-5Pa;
(5) pressure with 30～150Pa passes into argon gas 20～100sccm, to produce argon plasma;
(6) utilize the cavity of argon plasma plasma chemical gas-phase deposition system and the substrate in cavity to carry out clean, in 10～30 minutes processing times, the power of argon plasma is 10～100W;
(7) open the heater on chip bench, substrate is heated, heating-up temperature is 200～400 ℃;
(8) open raw materials evaporate device, in plasma chemical vapor deposition system, pass into argon gas and hydrogen, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared N-shaped tin sulphur film, wherein argon flow amount is 10～80sccm, hydrogen flowing quantity is 5～40sccm, and plasma power is 50～300W, pressure 50～150Pa, raw materials evaporate temperature 50 C～1200 ℃, sedimentation time 20～150 minutes;
(9) close hydrogen, in plasma chemical vapor deposition system, pass into argon gas, the substrate surface of the method for utilizing plasma activated chemical vapour deposition after cleaning prepared p-type tin sulphur film, argon flow amount 10～80sccm wherein, plasma power is 50～300W, plasma pressure 100～150Pa, raw materials evaporate temperature 50 C～1200 ℃, sedimentation time 20～120 minutes;
(10) close plasma, and stop passing into argon gas;
(11) the heater temperature on rising chip bench is carried out vacuum annealing to the N-shaped tin sulphur film of preparing and p-type tin sulphur film, 300～550 ℃ of annealing temperatures, annealing time 30～150 minutes in the cavity of plasma chemical vapor deposition system;
(12) in the cavity of plasma chemical vapor deposition system, pass into argon gas, the N-shaped tin sulphur film after annealing in process and p-type tin sulphur film are cooled to room temperature in ar gas environment, to form p-n junction.
2. according to the method for claim 1, it is characterized in that, stanniferous and raw material sulphur comprises the compound of simple substance tin, elemental sulfur or stanniferous and element sulphur.
3. according to the method for claim 1, it is characterized in that, substrate comprises silicon chip, soda-lime glass, quartz glass, transparent conducting glass.
4. according to the method for claim 1, it is characterized in that, the quantity of raw materials evaporate device is more than 2 or 2, and raw materials evaporate device is provided with baffle plate, for controlling raw materials evaporate time and speed.
5. according to the method for claim 1, it is characterized in that, stanniferous and raw material sulphur can be put into respectively different raw materials evaporate devices.
6. according to the method for claim 1, it is characterized in that, plasma activated chemical vapour deposition method applying plasma can be microwave plasma, radio frequency plasma.
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| CN104167469B (en) * | 2014-08-12 | 2016-04-13 | 华中科技大学 | A kind of SnS 2the one time to produce method of/SnS hetero-junction thin-film solar cell |
| CN105551946A (en) * | 2016-01-07 | 2016-05-04 | 广东工业大学 | Preparation method for stannous sulfide nanosheet and photoelectric detector prepared based on stannous sulfide nanosheet |
| CN111489969A (en) * | 2019-01-29 | 2020-08-04 | 东莞新科技术研究开发有限公司 | Heat treatment method of semiconductor silicon wafer |
| CN113511638B (en) * | 2021-06-30 | 2022-12-06 | 南京邮电大学 | Preparation method of TiN-S composite anode material by plasma chemical vapor codeposition |
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| CN101195909A (en) * | 2007-11-30 | 2008-06-11 | 华南师范大学 | Direct current plasma chemical vapor deposition equipment |
| CN101378090A (en) * | 2008-09-26 | 2009-03-04 | 合肥工业大学 | Tin sulfide film solar battery |
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| CN101195909A (en) * | 2007-11-30 | 2008-06-11 | 华南师范大学 | Direct current plasma chemical vapor deposition equipment |
| CN101378090A (en) * | 2008-09-26 | 2009-03-04 | 合肥工业大学 | Tin sulfide film solar battery |
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