CN101459200A - Flexible CIGS thin-film solar cell and absorption layer preparation thereof - Google Patents

Flexible CIGS thin-film solar cell and absorption layer preparation thereof Download PDF

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CN101459200A
CN101459200A CNA2007101510406A CN200710151040A CN101459200A CN 101459200 A CN101459200 A CN 101459200A CN A2007101510406 A CNA2007101510406 A CN A2007101510406A CN 200710151040 A CN200710151040 A CN 200710151040A CN 101459200 A CN101459200 A CN 101459200A
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方小红
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CETC 18 Research Institute
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention belongs to a flexible CIGS thin-film solar cell and a process for preparing an absorption layer thereof, the flexible CIGS thin-film solar cell is a multi-layer film structure, which comprises an substrate, a bottom electrode, an absorption layer, a buffer layer, a window layer, an anti-reflecting film and an upper electrode, and the flexible CIGS thin-film solar cell is characterized in that the substrate is made of flexible metals or polyimide. The process for preparing the adsorption layer of the flexible CIGS thin-film solar cell is characterized in that the substrate is made of flexible metals or polyimide, the bottom electrode Mo of the thickness of 0.5-1.5 mu m is deposited by magnetron sputtering, a metal prefabricating layer is prepared on a Mo thin-film, and is in vacuum seal to be placed in a furnace to heat, the temperature of the area of a solid selenium source is controlled between 180-300 DEG C to perform selenizing treatment, thereby enabling the metal prefabricating layer to be transformed into a semiconductor thin-film. Through performing selenizing or vulcanizing under saturation vapor pressure of selenium or sulfur in a vacuum seal silica tube, controllable repeatability of the technique process is fine, use quantity of selenium or sulfur is reduced, besides, the process is controllable and the equipment is simple.

Description

The preparation method of flexible CIGS thin-film solar cell and absorbed layer thereof
Technical field
The invention belongs to solar cell battery technology field, particularly relate to the preparation method of a kind of flexible CIGS thin-film solar cell and absorbed layer thereof.
Background technology
Compound semiconductor copper indium diselenide with yellow copper structure is CuInSe 2, being abbreviated as the miscible crystal of CIS series is the direct band gap material, with its thin film solar cell as absorbed layer, is considered to one of the most promising third generation compound photovoltaic cell, its composition comprises: CuInSe 2, CuIn 1-XGa XSe 2, CuInS 2, CuIn 1-XGa XS 2, CuIn 1-XGa XSe 2-XS 2Deng.Existing Copper Indium Gallium Selenide or S thin film solar cell, it is the novel solar cell that later development comes out in the eighties in 20th century, be in soda-lime glass, metal forming, as: stainless steel foil, titanium foil, molybdenum foil, aluminium foil etc., or the photovoltaic device that difference deposit multilayer film constitutes on the polyimide film substrate, typical structure is following multi-layer film structure: substrate/hearth electrode/absorbed layer/resilient coating/Window layer/antireflective coating/top electrode.
Studies show that absorbed layer CIGS film is to the battery performance decisive role.Because many, the complex structure of elemental composition, mainly by Cu, In, Ga, Se or/and four kinds or five kinds elements of S are synthetic, be that the stoicheiometry of an element and distribution thereof are the key factors of decision battery performance in the optical absorbing layer by multiple mutual so molten compound constitutes.
The preparation method of CIGS absorbed layer mainly is divided into two classes: first kind method is polynary coevaporation method, is that coevaporation is reacted in the source in vacuum chamber with Cu, In, Ga and Se, or with binary distribution coevaporations such as Cu+Se, In+Se, Ga+Se.Coevaporation method requires the evaporation rate and the deposition on substrate of every kind of element all to require accurate control, just can obtain uniform film; Second method is a selenizing method behind the metal preformed layer, deposits Cu, In, Ga layer by proportioning earlier on substrate, and Seization in Se atmosphere finally forms the CuIn that satisfies ratio requirement again 1-XGa XSe 2Polycrystal film.Substitute selenium with sulphur equally, carry out the thermo-chemical treatment of sulphur distribution behind vulcanization reaction or the first selenium, form CuIn 1-XGa XS 2Or CuIn 1-XGa XSe 2-XS 2Metal preformed layer film build method has the method that sputter, evaporation, electro-deposition, sputter and evaporation combine etc., and its uniformity of film is more easy to control, and deposit thickness is ripe preparation technology in grasp, and the cost of process equipment is not high.Wherein magnetically controlled sputter method technology is easy, elemental composition is easy to control, is effectively film build method.Back selenizing or sulfuration process mainly comprise chemical vapour deposition technique and chemical solid-state selenium or sulphur evaporation.The former is owing to need to adopt the hydrogen selenide of severe toxicity or hydrogen sulfide gas and domesticly there is no the hydrogen selenide gas supply and difficult enforcement; The latter adopts the lower and extensive employing of Solid State Source and equipment manufacturing cost with regard to present technology.
Conventional Solid State Source selenizing or sulfuration are to make it be vaporized into steam on selenium or sulphur heating in vacuum chamber, generate CuIn with the reaction of metal preformed layer after reaching uniform temperature 1-XGa XSe 2Or CuIn 1-XGa XS 2, because the uniformity of whole warm area is uncontrollable in the vacuum chamber, and need selenium or sulphur steam to be covered with whole vacuum chamber, meet cold then condensation at vacuum-chamber wall, cause selenizing technology instability, the uncontrollable absorbed layer film performance that causes is not good, influences the performance of thin film solar cell.If by adding reacting gas hydrogen or argon gas+hydrogen, then produced hypertoxic hydrogen selenide, vent gas treatment is a big problem; If only feed inert gas (as: argon gas), then can not control the pressure of selenium steam or sulphur steam, cause selenizing technology instability, poor controllability.
Summary of the invention
The present invention is for solving problems of the prior art, provides that a kind of equipment is simple, process is controlled, the preparation method of the flexible CIGS thin-film solar cell of good process repeatability and absorbed layer thereof.
The present invention for solving the technical scheme that technical problem adopted that exists in the known technology is:
Flexible CIGS thin-film solar cell is multi-layer film structure, comprises substrate, hearth electrode, absorbed layer, resilient coating, Window layer, antireflective coating and top electrode, is characterized in: substrate layer is flexible metallic material or polyimides.
The absorbed layer preparation method of flexible CIGS thin-film solar cell, be characterized in: substrate is with flexible metal or polyimide film, the hearth electrode Mo that magnetron sputtering deposition 0.5-1.5 μ m is thick, prepare the metal preformed layer with CuIn and CuGa alloy target material with magnetron sputtering method again on the Mo film, thickness is 0.6-1.2 μ m.The substrate that deposits hearth electrode Mo and copper indium gallium metal preformed layer is placed quartz ampoule, in pipe, place the solid-state selenium source of 0.5-5g simultaneously, vacuum seal.Put into the tube furnace of sectional temperature programmed control, heat up uniformly fast,, make substrate region temperature be controlled at 400-590 ℃, solid-state selenium source region temperature is controlled at 180-300 ℃, thickness according to the metal preformed layer, carry out the selenizing of 10-30min and handle, make the metal preformed layer change CuIn fully into 1-XGa XSe 2Compound semiconductor film.
The present invention can also adopt following technical measures to realize:
Flexible CIGS thin-film solar cell is characterized in: substrate is thick to be 10-100 μ m, and flexible metallic material is titanium foil, stainless steel foil, molybdenum foil or aluminium foil.
Flexible CIGS thin-film solar cell is characterized in: duplicature hearth electrode Mo and copper indium gallium metal preformed layer are arranged on the substrate.
The preparation method of flexible CIGS thin-film solar cell absorbed layer, be characterized in: substrate is with flexible metal or polyimide film, the hearth electrode Mo that magnetron sputtering deposition 0.5-1.5 μ m is thick, prepare the metal preformed layer with CuIn and CuGa alloy target material with magnetron sputtering method again on the Mo film, thickness is 0.6-1.2 μ m.The substrate that deposits hearth electrode Mo and copper indium gallium metal preformed layer is placed quartz ampoule, in pipe, place the solid-state sulphur source of 0.5-5g simultaneously, vacuum seal.Put into the tube furnace of sectional temperature programmed control, heat up uniformly fast,, make substrate region temperature be controlled at 400-590 ℃, region, solid-state sulphur source temperature is controlled at 180-300 ℃, thickness according to the metal preformed layer, carry out the vulcanizing treatment of 10-30min, make the metal preformed layer change CuIn fully into 1-XGa XS 2Compound semiconductor film.
The absorbed layer preparation method of flexible CIGS thin-film solar cell, be characterized in: substrate is with flexible metal or polyimide film, the hearth electrode Mo that magnetron sputtering deposition 0.5-1.5 μ m is thick, prepare the metal preformed layer with CuIn and CuGa alloy target material with magnetron sputtering method again on the Mo film, thickness is 0.6-1.2 μ m.The substrate that deposits hearth electrode Mo and copper indium gallium metal preformed layer is placed quartz ampoule, in pipe, place the solid-state selenium source of 0.5-5g simultaneously, vacuum seal.Put into the tube furnace of sectional temperature programmed control, heat up uniformly fast,, make substrate region temperature be controlled at 400-590 ℃, solid-state selenium source region temperature is controlled at 180-300 ℃, thickness according to the metal preformed layer, carry out the selenizing of 10-30min and handle, make the metal preformed layer change CuIn fully into 1-XGa XSe 2Compound semiconductor film replaces selenium source with the sulphur source again, carries out sulfidation, finally forms CuIn 1-XGa XSe 2-XS 2Compound semiconductor film.
The absorbed layer preparation method of flexible CIGS thin-film solar cell, be characterized in: substrate is with flexible metal or polyimide film, the hearth electrode Mo that magnetron sputtering deposition 0.5-1.5 μ m is thick, prepare the metal preformed layer with CuIn and CuGa alloy target material with magnetron sputtering method again on the Mo film, thickness is 0.6-1.2 μ m.The substrate that deposits hearth electrode Mo and copper indium gallium metal preformed layer is placed quartz ampoule, in pipe, place the solid-state sulphur source of 0.5-5g simultaneously, vacuum seal.Put into the tube furnace of sectional temperature programmed control, heat up uniformly fast,, make substrate region temperature be controlled at 400-590 ℃, region, solid-state sulphur source temperature is controlled at 180-300 ℃, thickness according to the metal preformed layer, carry out the vulcanizing treatment of 10-30min, make the metal preformed layer change CuIn fully into 1-XGa XS 2Compound semiconductor film replaces the sulphur source with selenium source again, carries out the selenizing process, finally forms CuIn 1-XGa XSe 2-XS 2Compound semiconductor film.
Advantage and good effect that the present invention has are: depress by the saturated steam that adopts selenium in the vacuum seal quartz ampoule or sulphur and carry out selenizing or sulfuration, the technical process controllable repeatability has reduced the consumption of selenium or sulphur, and process is controlled, and equipment is simple.
Description of drawings
Fig. 1 is a flexible CIGS thin-film solar cell structural representation of the present invention.
Label among the figure is respectively: 1. top electrode; 2. antireflective coating; 3. Window layer; 4. resilient coating; 5. absorbed layer; 6. hearth electrode; 7. substrate.
Embodiment
For further understanding summary of the invention of the present invention, characteristics and effect, enumerate following examples now, and conjunction with figs. is described in detail as follows:
Please refer to Fig. 1:
CIGS thin-film solar cell, by substrate, hearth electrode, absorbed layer, resilient coating, Window layer, antireflective coating and top electrode constitute, described substrate is a flexible substrate, comprise flexible titanium foil or stainless steel or polyimides, aspect the preparation of absorbed layer, CIGS thin-film solar cell is with flexible titanium foil, flexible material such as stainless steel foil or polyimide film is as substrate, the method for preparing duplicature with magnetron sputtering method or increase the metal/metal oxide transition zone on flexible substrate prepares hearth electrode Mo, then adopt sputtering method to prepare copper indium gallium metal preformed layer, in stopped pipe, heat the reaction of carrying out selenizing or sulfuration again, described substrate is thick to be 10-100 μ m, and flexible metallic material is titanium foil or stainless steel foil; Duplicature hearth electrode Mo is arranged on the described substrate; On flexible metal substrate of plating molybdenum or polyimide film substrate, prepare copper indium gallium metal preformed layer with sputtering method, then substrate is placed the glass tube of vacuum sealing, again under specific temperature with solid-state selenium source or/the sulphur source is in selenizing, guarantee to depress selenizing at the saturated vapor of selenium or sulphur, equipment is simple, and process is controlled, and selenizing or sulfuration are thoroughly, fully, evenly, make the metal preformed layer change Copper Indium Gallium Selenide or sulphur absorbed layer into, satisfy the requirement of thin film solar cell.In the method, can take a kind of of following dual mode that the metal preformed layer is carried out selenizing or/and sulfuration.
First method: on flexible metal substrate of plating molybdenum or polyimide film substrate, prepare copper indium gallium metal preformed layer with sputtering method, then substrate and solid-state selenium source are placed quartz ampoule, vacuum seal, and be placed in the tube furnace of sectional temperature control, make the substrate region be heated to 400-590 ℃, solid-state selenium source region temperature is heated to 180-300 ℃, make selenium atom and copper indium gallium metal atom react, make the deep diffusion of selenium atom simultaneously along copper indium gallium metal preformed layer film, copper indium gallium atom spreads to film surface, thereby copper indium gallium preformed layer generation qualitative change is until forming CuIn 1-XGa XSe 2Compound semiconductor film.Change solid-state selenium source into the sulphur source, other condition is constant, then forms CuIn 1-XGa XS 2Compound semiconductor film.
Second method, in two steps copper indium gallium metal preformed layer is carried out selenizing and vulcanizing treatment, promptly with solid-state selenium source copper indium gallium metal preformed layer is carried out selenizing processing back earlier and carry out the phototvulcanization processing with solid-state sulphur source, or earlier with solid-state sulphur source copper indium gallium metal preformed layer being carried out after the vulcanizing treatment carrying out the light selenizing with solid-state selenium source, to handle its process conditions identical with first method with requirement, finally forms CuIn 1-XGa XSe 2-XS 2Compound semiconductor film.
Embodiment 1: prepare duplicature hearth electrode Mo with direct current magnetron sputtering process on 20-100 μ m titanium foil, the thickness of hearth electrode is 0.5-1.5 μ m, prepare the metal preformed layer with CuIn and CuGa alloy target material with magnetron sputtering method again on the Mo film, thickness is 0.6-1.2 μ m.The substrate that deposits hearth electrode Mo and copper indium gallium metal preformed layer is placed quartz ampoule, in pipe, place the solid-state selenium source of 0.5-5g simultaneously, vacuum seal.Put into the tube furnace of sectional temperature programmed control, heat up uniformly fast,, make substrate region temperature be controlled at 400-590 ℃, solid-state selenium source region temperature is controlled at 180-300 ℃, thickness according to the metal preformed layer, carry out the selenizing of 10-30min and handle, make the metal preformed layer change CuIn fully into 1-XGa XSe 2Compound semiconductor film.
Embodiment 2: change backing material into stainless steel foil, other condition is identical with embodiment 1, makes CuIn 1-XGa XSe 2Compound semiconductor film.
Embodiment 3: change solid-state selenium source into solid-state sulphur source, other condition is identical with embodiment 1, makes CuIn 1-XGa XS 2Compound semiconductor film.
Embodiment 4: change backing material into polyimide film, substrate region temperature is controlled at 400-450 ℃, and other condition is identical with embodiment 1, makes CuIn 1-XGa XSe 2Compound semiconductor film.
Embodiment 5: in the selenizing later stage of embodiment 1, the method for pressing embodiment 3 increases sulfidation, makes CuIn 1-XGa XSe 2The part selenium atom is replaced by sulphur atom, makes CuIn 1-XGa XSe 2-XS 2Compound semiconductor film.
Embodiment 6: in the sulfuration later stage of embodiment 3, the method for pressing embodiment 3 increases the selenizing process, makes CuIn 1-XGa XS 2The part sulphur atom is replaced by selenium atom, makes CuIn 1-XGa XSe 2-XS 2Compound semiconductor film.
Embodiment 7: change backing material into molybdenum foil, other condition is identical with embodiment 1, makes CuIn 1 -XGa XSe 2Compound semiconductor film.
Embodiment 8: change backing material into aluminium foil, other condition is identical with embodiment 1, makes CuIn 1 -XGa XSe 2Compound semiconductor film.

Claims (7)

1. flexible CIGS thin-film solar cell is multi-layer film structure, comprises substrate, hearth electrode, absorbed layer, resilient coating, Window layer, antireflective coating and top electrode, it is characterized in that: substrate layer is flexible metallic material or polyimides.
2. flexible CIGS thin-film solar cell according to claim 1 is characterized in that: substrate is thick to be 10-100 μ m, and flexible metallic material is titanium foil, stainless steel foil, molybdenum foil or aluminium foil.
3. flexible CIGS thin-film solar cell according to claim 1 is characterized in that: duplicature hearth electrode Mo and copper indium gallium metal preformed layer are arranged on the substrate.
4. the absorbed layer preparation method of flexible CIGS thin-film solar cell according to claim 1, it is characterized in that: substrate is with flexible metal or polyimide film, the hearth electrode Mo that magnetron sputtering deposition 0.5-1.5 μ m is thick, prepare the metal preformed layer with CuIn and CuGa alloy target material with magnetron sputtering method again on the Mo film, thickness is 0.6-1.2 μ m; The substrate that deposits hearth electrode Mo and copper indium gallium metal preformed layer is placed quartz ampoule, in pipe, place the solid-state selenium source of 0.5-5g simultaneously, vacuum seal; Put into the tube furnace of sectional temperature programmed control, heat up uniformly fast,, make substrate region temperature be controlled at 400-590 ℃, solid-state selenium source region temperature is controlled at 180-300 ℃, thickness according to the metal preformed layer, carry out the selenizing of 10-30min and handle, make the metal preformed layer change CuIn fully into 1-XGa XSe 2Compound semiconductor film.
5. the preparation method of flexible CIGS thin-film solar cell absorbed layer according to claim 3, it is characterized in that: substrate is with flexible metal or polyimide film, the hearth electrode Mo that magnetron sputtering deposition 0.5-1.5 μ m is thick, prepare the metal preformed layer with CuIn and CuGa alloy target material with magnetron sputtering method again on the Mo film, thickness is 0.6-1.2 μ m; The substrate that deposits hearth electrode Mo and copper indium gallium metal preformed layer is placed quartz ampoule, in pipe, place the solid-state sulphur source of 0.5-5g simultaneously, vacuum seal; Put into the tube furnace of sectional temperature programmed control, heat up uniformly fast,, make substrate region temperature be controlled at 400-590 ℃, region, solid-state sulphur source temperature is controlled at 180-300 ℃, thickness according to the metal preformed layer, carry out the vulcanizing treatment of 10-30min, make the metal preformed layer change CuIn fully into 1-XGa XS 2Compound semiconductor film.
6. the absorbed layer preparation method of flexible CIGS thin-film solar cell according to claim 5, it is characterized in that: substrate is with flexible metal or polyimide film, the hearth electrode Mo that magnetron sputtering deposition 0.5-1.5 μ m is thick, prepare the metal preformed layer with CuIn and CuGa alloy target material with magnetron sputtering method again on the Mo film, thickness is 0.6-1.2 μ m; The substrate that deposits hearth electrode Mo and copper indium gallium metal preformed layer is placed quartz ampoule, in pipe, place the solid-state selenium source of 0.5-5g simultaneously, vacuum seal; Put into the tube furnace of sectional temperature programmed control, heat up uniformly fast,, make substrate region temperature be controlled at 400-590 ℃, solid-state selenium source region temperature is controlled at 180-300 ℃, thickness according to the metal preformed layer, carry out the selenizing of 10-30min and handle, make the metal preformed layer change CuIn fully into 1-XGa XSe 2Compound semiconductor film replaces selenium source with the sulphur source again, carries out sulfidation, finally forms CuIn 1-XGa XSe 2-XS 2Compound semiconductor film.
7. the absorbed layer preparation method of flexible CIGS thin-film solar cell according to claim 6, it is characterized in that: substrate is with flexible metal or polyimide film, the hearth electrode Mo that magnetron sputtering deposition 0.5-1.5 μ m is thick, prepare the metal preformed layer with CuIn and CuGa alloy target material with magnetron sputtering method again on the Mo film, thickness is 0.6-1.2 μ m; The substrate that deposits hearth electrode Mo and copper indium gallium metal preformed layer is placed quartz ampoule, in pipe, place the solid-state sulphur source of 0.5-5g simultaneously, vacuum seal; Put into the tube furnace of sectional temperature programmed control, heat up uniformly fast,, make substrate region temperature be controlled at 400-590 ℃, region, solid-state sulphur source temperature is controlled at 180-300 ℃, thickness according to the metal preformed layer, carry out the vulcanizing treatment of 10-30min, make the metal preformed layer change CuIn fully into 1-XGa XS 2Compound semiconductor film replaces the sulphur source with selenium source again, carries out the selenizing process, finally forms CuIn 1-XGa XSe 2-XS 2Compound semiconductor film.
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