CN116262631A - For forming solid CdCl on thin film solar cells 2 Method and apparatus for layering - Google Patents
For forming solid CdCl on thin film solar cells 2 Method and apparatus for layering Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 72
- 239000007787 solid Substances 0.000 title claims abstract description 56
- 239000010409 thin film Substances 0.000 title description 9
- 239000007789 gas Substances 0.000 claims abstract description 96
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 67
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 67
- 239000000758 substrate Substances 0.000 claims abstract description 48
- 239000000463 material Substances 0.000 claims abstract description 46
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 16
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims description 27
- 238000000151 deposition Methods 0.000 claims description 20
- 229910052717 sulfur Inorganic materials 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910004613 CdTe Inorganic materials 0.000 description 62
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 29
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 28
- 239000000460 chlorine Substances 0.000 description 11
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- 238000006243 chemical reaction Methods 0.000 description 10
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- 238000002202 sandwich sublimation Methods 0.000 description 7
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
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- 230000008901 benefit Effects 0.000 description 5
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 5
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000005137 deposition process Methods 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
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- 239000011261 inert gas Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
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- 230000008022 sublimation Effects 0.000 description 3
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- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910007709 ZnTe Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 231100001261 hazardous Toxicity 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
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- 229910004611 CdZnTe Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000000224 chemical solution deposition Methods 0.000 description 1
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- 239000008139 complexing agent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- OISMQLUZKQIKII-UHFFFAOYSA-L dichlorocadmium;hydrate Chemical compound O.[Cl-].[Cl-].[Cd+2] OISMQLUZKQIKII-UHFFFAOYSA-L 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000219 mutagenic Toxicity 0.000 description 1
- 230000003505 mutagenic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1828—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof the active layers comprising only AIIBVI compounds, e.g. CdS, ZnS, CdTe
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention relates to a method for forming solid CdCl on the surface of a material 2 Methods and apparatus for layering. The method comprises the following steps: providing a material surface on a substrate, applying a sacrificial layer comprising cadmium on the material surface, and providing a gas comprising hydrogen chloride to the sacrificial layer for a time sufficient to convert the sacrificial layer to solid CdCl 2 A predetermined period of time of the layer. The apparatus includes a first means for applying a sacrificial layer comprising cadmium on a surface of a material on a substrate, and a second means for providing a gas comprising hydrogen chloride to the sacrificial layer.
Description
Technical Field
The present application relates to a method for forming a solid CdCl on a material surface, in particular on a CdTe or CdSeTe layer of a thin-film solar cell 2 A method of layering, and an apparatus for use in the method.
Background
According to the prior art, the photoactive layer of CdTe thin film solar cells comprises a CdTe (cadmium telluride) layer or CdSe x Te 1-x Layer (0)<x<1) Wherein CdSe x Te 1-x The layer is hereinafter referred to as a CdSeTe (cadmium telluride) layer. According to the prior art, cdTe thin film solar cells can also include additional layers of different materials or combinations of materials, typically selected from, but not limited to, cadmium, selenium, tellurium, zinc, mercury, manganese, and magnesium. Unless otherwise defined, from here on, a "CdTe or CdSeTe layer" will be synonymous with a layer or stack comprising Cd, se, te, zn, hg, mn, mg, S or a combination thereof, for brevity and applicability to the scope of the present application.
In the production process, after application of the CdTe or CdSeTe layer, the CdCl is generally used in the prior art 2 And heating to activate the CdTe or CdSeTe layer. To this end, the CdCl is applied by methods of the prior art, for example wet-chemical methods (roll coating, spray coating or dip coating) or CVD or PVD 2 The layer is applied to a CdTe or CdSeTe layer. Thereafter, the CdCl is allowed to stand at an elevated temperature (typically about 380 ℃ to 430 ℃) 2 Reacts with the CdTe or CdSeTe layer. The reaction time is about 10 minutes to 45 minutes. At this time, cdCl 2 Acts as a fluxing agent and supports the recrystallization of the CdTe or CdSeTe layer. If the CdTe or CdSeTe layer consists of a stack or combination of materials, such as ZnTe, cdSe, or a pure layer consisting of, for example, mn or Mg, activation can result in the formation of a mixed layer and a gradual material composition transition, with an atomic concentration gradient replacing the original sharp transition between the initially single deposited layers. Thus, during activation, a material, such as CdZnTe, can be formed from the CdTe and ZnTe layers,and the material CdSeTe may be formed from a combination of CdSe and CdTe. Thus, the different materials as mentioned above can be combined to introduce some material concentration gradient and intermixing from the original stack by activation over the absorber layer.
All mentioned CdCl 2 The method of application to CdTe or CdSeTe layers uses liquid or gaseous CdCl 2 This results in different disadvantages of these methods when applied, especially on an industrial scale. First, cdCl 2 Is a toxic chemical substance which is easily dissolved in water and has great harm to the environment. It has proven to be carcinogenic and mutagenic and toxic to reproduction. Due to CdCl 2 When processing CdCl during the production process 2 Special care is required when. Thus, large safety measures have to be taken, which in turn leads to high machine costs. Furthermore, wet chemistry methods cannot reliably provide CdCl with uniform layer thickness over large areas 2 Layers, and thickness is also difficult to control. Finally, but equally important, roll coating is not a non-contact fashion and thus may affect the surface of the solar CdTe or CdSeTe layer.
Disclosure of Invention
The purpose of the present application is to form CdCl for use in the activation process 2 In the present application, cdCl is obtained 2 Is safer and easier to handle, and CdCl 2 The thickness of the layer has high uniformity and controllability.
This object is achieved by the method and the device provided by the independent claims. Preferred embodiments are given in the dependent claims.
The method of the invention comprises the following steps: providing a material surface on a substrate, applying a sacrificial layer comprising cadmium on the material surface, and providing a gas comprising hydrogen chloride to the sacrificial layer for a time sufficient to convert the sacrificial layer to solid CdCl 2 A predetermined period of time of the layer. In some embodiments, the solid CdCl formed 2 The layer being crystalline CdCl 2 A layer.
It should be noted that CdCl 2 The layer not only refers to pure CdCl 2 The (cadmium chloride) layer also refers to a cadmium chloride layer containing waterSuch as a cadmium chloride hydrate layer), or a layer comprising other elements or compounds than cadmium chloride (e.g., doped with sulfur or oxygen, etc.).
The hydrogen chloride-containing gas may be pure hydrogen chloride, or may further contain chlorine as a pure element, or other elements or compounds than hydrogen chloride, i.e. it may be present independently of hydrogen chloride, for example an inert gas acting as a carrier gas, such as N 2 。
The predetermined period of time depends inter alia on the following parameters: the thickness of the sacrificial layer, the volume of the gas containing hydrogen chloride and supplied to the sacrificial layer and/or the concentration of hydrogen chloride in the gas containing hydrogen chloride and supplied to the sacrificial layer, the temperature of the material and material surface of the sacrificial layer, and the temperature of the gas containing hydrogen chloride. Conversion of the sacrificial layer to solid CdCl is affected by the existence of the catalyst 2 Many possibilities of the process of the layer, it is therefore difficult to provide specific values or even formulas for calculating the predetermined time period. However, since the skilled person is already aware of the chemical reactions underlying the transformation, the skilled person is able to determine the necessary time period with few experiments. Some examples are provided below.
Sacrificial layer to solid CdCl 2 The conversion of the layer needs to be substantially complete, i.e. complete or almost complete. The presence of some residues of the sacrificial layer may not affect the activation process of the material layer or stack on which the sacrificial layer is deposited. However, the conversion is preferably accomplished.
The method of the invention has the advantage of forming CdCl for activating CdTe or CdSeTe layers or laminates that may include Cd, se, te, zn, hg, mn, mg, S or a combination thereof 2 The layer does not require liquid or gaseous CdCl 2 . Thus, the safety requirements are lower and activation can be achieved more economically and efficiently. Other advantages are presented in certain embodiments of the invention.
The substrate may be any kind of substrate suitable for use in a thin film solar cell or in a process for manufacturing a thin film solar cell, on which a material surface is provided. The substrate may be, for example, glass or any other transparent substrate or metal, such as a metal foil, and may comprise one or more layers of other materials. For example, the substrate may be glass with a transparent front contact layer (e.g., transparent Conductive Oxide (TCO)) and a window layer (e.g., pure CdS (cadmium sulfide) or modified CdS (cadmium sulfide)) thereon. The front contact layer may also be a laminate of several different layers. Hereafter, modified CdS is understood as CdS with a doping, a crystal shape or a change in grain size, or a mixture of CdS with other substances. In some embodiments, the window layer may be omitted. To complete the fabrication of the solar cell, a CdTe or CdSeTe layer is deposited and activated on the window layer or front contact layer, and a back contact layer is applied to the CdTe or CdSeTe layer. Each of the CdTe or CdSeTe layer and the back contact layer may also be a stack of several different layers as described above. This sequence of manufacturing processes is referred to as a top liner structure.
In the prior art, it is well known that thin film solar cells can also be reverse-structured. In this case, the substrate is a back side substrate (e.g., glass) on which one or more back contact layers are deposited (also constructed in reverse order). A CdTe or CdSeTe layer is provided and activated on the back contact layer, followed by deposition of a window layer and a front contact layer. Here, the deposition of the window layer may also be omitted. This process is known as a substrate structure.
According to the prior art, cdTe or CdSeTe layers are typically provided by vacuum-based deposition processes, such as evaporation, sublimation (e.g., close-space sublimation (CSS)), or sputtering.
In most embodiments of the present invention, focusing on the activation step of the CdTe thin film solar cell, the surface of the material in the method of the present invention is the surface of a layer comprising at least one of Cd, se, te, zn, hg, mn, mg, S or a combination thereof. Furthermore, the material surface may be a laminate formed by depositing a series of individual layers, wherein each individual layer may likewise comprise at least one of Cd, se, te, zn, hg, mn, mg, S or a combination thereof. Notably, some of these materials are more amenable to deposition by sputtering techniques than sublimation deposition techniques. This will allow the stack to be deposited by a range of deposition techniques in the same vacuum chamber, a connected vacuum chamber, or even a different vacuum chamber, with sufficient precautions taken to atmosphere and oxygen exposure of the deposited layers. Thus, the preferred embodiment is to perform the steps of the method of the present invention in the same or a connected vacuum environment.
In an embodiment of the method of the invention, the sacrificial layer is a layer of CdS (cadmium sulfide) or CdO (cadmium oxide) or a combination thereof. The advantage of these materials is that they are almost insoluble in water and more toxic than gaseous or liquid CdCl 2 Is small.
In some embodiments, the sacrificial layer is applied using a vacuum-based deposition method, such as thermal evaporation, sublimation, vapor transport deposition, metal Organic Chemical Vapor Deposition (MOCVD), or sputter application. Vacuum deposition of the sacrificial layer has different advantages: first, cdCl 2 The layer may be formed by a non-contact process so as to avoid damage to the surface of the semi-finished solar cell. Second, cdCl with high uniformity can be formed on the surface of CdTe or CdSeTe layer with large area 2 A layer. Third, in the process of forming the sacrificial layer and providing the hydrogen chloride-containing gas, the CdCl can be simply and precisely adjusted through the thickness and process parameters of the sacrificial layer 2 Thickness of the layer. Likewise, cdS and CdO are particularly suitable for deposition by vacuum-based deposition methods.
However, the sacrificial layer may alternatively be applied by a wet deposition process (such as chemical bath deposition).
If the sacrificial layer is applied using a vacuum-based deposition method, then preferably the CdTe or CdSeTe layer is also provided using a vacuum-based deposition method as described above, and no vacuum interruption occurs between the steps of providing the CdTe or CdSeTe layer on the substrate and applying the sacrificial layer. The advantage of avoiding vacuum interruption is that no contamination of the CdTe or CdSeTe layer by impurities occurs and the whole process can be performed in a more time and cost efficient manner.
In an embodiment of the method of the invention, the step of providing a hydrogen chloride containing gas to the sacrificial layer is performed in a process chamber. The process chamber provides a closed, customizable process atmosphere at a pressure and temperature relative to the atmosphere and generally contains at least one gas inlet and at least one gas outlet. In this case, the hydrogen chloride-containing gas may be supplied from a gas source outside the process chamber.
In other embodiments, a gas source providing a hydrogen chloride-containing gas may be disposed within the processing chamber or at least near the substrate, the CdTe layer, or the CdSeTe layer and the sacrificial layer.
In some embodiments, the method further comprises the step of forming an additional solid layer on the sacrificial layer prior to providing the hydrogen chloride-containing gas to the sacrificial layer. The additional solid layer consists of a material that decomposes into a hydrogen chloride-containing gas in the temperature range of 200 ℃ to 350 ℃. In this case, the step of supplying the hydrogen chloride-containing gas to the sacrificial layer includes temperature-treating the additional solid layer formed on the sacrificial layer in a range of 200 to 350 ℃ to supply the hydrogen chloride-containing gas to the sacrificial layer by decomposing the additional solid layer. Thus, a hydrogen chloride-containing gas is generated proximate to the sacrificial layer, for example, within the processing chamber. The additional solid layer may comprise NH 4 Cl, which decomposes to gaseous NH at a temperature of about 340℃and at normal pressure 3 And HCl. Ammonium chloride (NH) 4 Cl) may be deposited as a solid film (e.g., foil) onto the sacrificial layer, or may be deposited as a liquid (i.e., a solution, such as an aqueous solution) onto the sacrificial layer, followed by drying to form a solid film. The liquid may be deposited, for example, by roll coating or spray coating.
The invention is used for forming solid CdCl on the surface of a material 2 The apparatus of the layer comprises a first device for applying a sacrificial layer comprising cadmium on a surface of a material provided on a substrate and a second device for providing a gas comprising hydrogen chloride to the sacrificial layer. The device is used for executing the method according to the invention.
In an embodiment, the first device is a vacuum chamber for performing a vacuum process to apply the sacrificial layer. Such vacuum processes may be thermal evaporation processes, sublimation processes, vapor transport deposition processes, metalorganic chemical vapor deposition processes, or sputtering processes. In particular, the process is a process for applying a CdS or CdO layer.
Where the first device is a vacuum chamber, in some embodiments the first device is closely vacuum-coupled with a device that provides a layer or stack comprising Cd, se, te, zn, hg, mn, mg, S or a combination thereof on the substrate. That is, the apparatus of the present invention may also include a device that provides a CdTe or CdSeTe layer or stack on a substrate. In this case, it is particularly advantageous that the means for providing the CdTe or CdSeTe layer or stack is also a vacuum chamber. Thus, the process of providing a CdTe or CdSeTe layer or stack and applying the sacrificial layer can be performed without interrupting the vacuum between the two processes. In a particular embodiment, the first apparatus and the apparatus for providing the CdTe or CdSeTe layer or stack are the same vacuum chamber.
In some embodiments, the second means for providing a hydrogen chloride containing gas to the sacrificial layer is a vacuum chamber that includes a gas inlet for introducing the hydrogen chloride containing gas and that allows the hydrogen chloride containing gas to contact the surface of the sacrificial layer.
In some embodiments, the apparatus further comprises a third means for applying an additional solid layer on the sacrificial layer, wherein the additional solid layer is comprised of a material that decomposes to a hydrogen chloride containing gas at a temperature in the range of 200 ℃ to 350 ℃. The third device is disposed between the first device and the second device within the production line. That is, the substrate leaving the first device enters the third device, and after being processed in the third device and leaving, enters the second device. In these embodiments, the second means is a vacuum chamber comprising a temperature control unit for heating the additional solid layer formed on the sacrificial layer to provide a hydrogen chloride containing gas to the sacrificial layer by decomposing the additional solid layer. That is, the temperature control unit is adapted to heat the additional solid layer to a temperature in the range of 200 ℃ to 350 ℃, at which temperature the additional solid layer decomposes and releases hydrogen chloride.
Preferably, the substrate to be processed is provided to the first means and the second means by a continuous transport system (e.g. rollers or shafts) and may even be provided to the means for providing CdTe or CdSeTe layers or stacks, and the substrate extends through the respective means. The substrate may even be continuously moved by a conveyor system if the time frame of the different processes allows it.
All or part of the above-described features of the method according to the invention or of the device according to the invention may be combined with each other as long as they are not mutually exclusive.
Drawings
In the following detailed description, the accompanying drawings form a part hereof and are provided to reference, and in which are shown by way of illustration specific embodiments in which the invention may be practiced. In this regard, directional terminology, such as "top," "bottom," "front," "back," "leading," "trailing," etc., is used with reference to the orientation of the figure being described. Because components of embodiments of the present invention can be positioned in a number of different orientations, the directional terminology is used for purposes of illustration and is in no way limiting. It is to be understood that other embodiments may be utilized and structural or logical changes may be made without departing from the scope of the present invention, and therefore, the following detailed description is not to be taken in a limiting sense, and the scope of the present invention is defined by the appended claims.
Fig. 1 schematically shows an embodiment of the method of the invention.
Fig. 2A to 2F schematically show the layer sequence of a solar cell during the course of a superstrate structure process in different process steps including the steps of the first embodiment of the method of the invention.
Fig. 3 schematically shows a first embodiment of the device of the invention.
Fig. 4A to 4C schematically show the layer sequence of a solar cell during a process sequence of a top-liner structure in different process steps including some of the steps of the second embodiment of the method of the invention.
Fig. 5 schematically shows a second embodiment of the device of the invention.
Reference numerals:
1-a glass substrate; 2-a front contact layer; 3-window layer; a 4-CdTe or CdSeTe layer; a 4' -activated CdTe or CdSeTe layer; the surface of the 41-CdTe or CdSeTe layer; 5-a sacrificial layer; 5 a-an additional solid layer; 6-a hydrogen chloride-containing gas; 7-CdCl 2 A layer; 8-cleaning solution; 9-Back contactA layer; 10-a first device; 11-a first vacuum chamber; 12-a first vacuumizing pump; 13-a first gas outlet; 14-a first gas source; 141-a gas container; 142-mass flow controller; 15-a first gas inlet; a 16-CdTe source; a 17-CdS source; 18-a temperature control device; 20,20' -second means; 21-a second vacuum chamber; 22-a second gas source; 221, 222-gas container; 223, 224-mass flow controller; 23-a second gas inlet; 24-a second vacuumizing pump; 25-a second gas outlet; 26-a temperature control device; 30-a conveying system; 40-a control device; 50-a third device; 51-a third vacuum chamber; 52-a spraying device; 53-temperature control means; 100-equipment; 101,102, 103-gate valves; 200-substrate
Detailed Description
Method first embodiment
Fig. 1 shows an embodiment of the method of the present invention. The method comprises a first step S10 of providing a CdTe or CdSeTe layer on a substrate, thereby providing a material surface on the substrate. Next, in step S20, a sacrificial layer is applied to the material surface of the CdTe or CdSeTe layer. In step S30, a hydrogen chloride-containing gas is supplied to the sacrificial layer for a predetermined period of time, wherein the sacrificial layer is converted into a solid CdCl 2 A layer. Subsequently, in step S40, the entire stack is annealed to activate the CdTe or CdSeTe layer. After annealing, in step S50, cdCl is removed from the CdTe or CdSeTe layer 2 A layer.
The method of the present invention is further illustrated in the following exemplary embodiments, which illustrate the fabrication of a solar cell of a superstrate structure, but are not meant to be limiting of the embodiments.
Fig. 2A shows a semi-finished solar cell comprising a glass substrate 1, a front contact layer 2 (e.g. made of InO) and a window layer 3 (made of CdS). As described above, window layer 3 may also be omitted in some embodiments. Layers 1 to 3 as a whole are referred to as substrates in the sense of application. On this substrate, i.e. on the window layer 3, a CdTe or CdSeTe layer 4 is provided by using e.g. a CSS deposition method. For example, the material surface 41 of the CdTe or CdSeTe layer 4 has an area in the x-y plane in the range of (600X 1200) mm 2 Up to (1300X 2100) mm 2 。
As shown in fig. 2B, a sacrificial layer 5, for example made of CdS, is applied to the CdTe or CdSeTe layer 4. For example, the sacrificial layer 5 is deposited on the material surface 41 of the CdTe or CdSeTe layer 4 using CSS deposition. In the vacuum chamber, CSS deposition is performed at a pressure in the range of 0.1Pa to 50Pa, and at a substrate temperature in the range of 400 ℃ to 600 ℃. CSS deposition of CdS is known in the art. The thickness of the sacrificial layer 5 is in the range of 10nm to 200nm, preferably in the range of 40nm to 100 nm. The thickness of the sacrificial layer 5 may also depend on the thickness of the CdTe or CdSeTe layer 4, i.e. the greater the thickness of the CdTe or CdSeTe layer 4, the greater the thickness of the sacrificial layer 5.
Fig. 2C shows the semi-finished solar cell during a process step of providing a hydrogen chloride containing gas 6 to the sacrificial layer 5. Thus, gas 6 comprises HCl. The HCl may be "dry" HCl provided from a gas container, or may be "wet" HCl provided from an aqueous HCl solution, such as a 35% aqueous HCl solution. HCl may also be provided by chemical reactions, e.g. H 2 SO 4 And NaCl. HCl can use, for example, N 2 Is delivered to the sacrificial layer 5 for a carrier gas and thus the gas 6 may also comprise a carrier gas.
The gas 6 is supplied to the sacrificial layer for a predetermined period of time, for example a period of time in the range of 5 seconds to 5 minutes. Since the predetermined time period depends on different parameters, some examples of parameter sets are given in table 1.
TABLE 1
All parameter values of the sacrificial layer 5 made of CdS are given. For sacrificial layers made of other materials, it may be necessary to adjust parameters.
Due to the presence of the gas 6, the sacrificial layer 5 is converted into a solid CdCl as shown in FIG. 2D 2 Layer 7. The sacrificial layer 5 is preferably completely converted into CdCl 2 Layer 7. However, some portions of the sacrificial layer 5 may remain unconverted, wherein the ratio of all these unconverted portions to the entire sacrificial layer 5 is smaller than10%, preferably less than 5%. For example, the conversion is based on the following reaction:
CdS(s)+2HCl(g)→CdCl 2 (s)+H 2 s (g) (1) or
CdO(s)+2HCl(g)→CdCl 2 (s)+H 2 O(l) (2)。
The water as a reaction product in reaction (2) may be incorporated into CdCl 2 In layer 7.
Conversion of sacrificial layer 5 to CdCl 2 After layer 7, the entire stack is annealed at a temperature in the range of 380 ℃ to 450 ℃ for a period of 10 minutes to 45 minutes to activate CdTe or CdSeTe layer 4. As a result, the activated CdTe or CdSeTe layer 4' is as shown in FIG. 2E. It should be noted here that the CdTe or CdSeTe layer 4 may also have the form of a stack, or a layer comprising Cd, se, te, zn, hg, mn, mg, S or a combination thereof. After annealing, cdCl is removed using cleaning solution 8 as shown in FIG. 2E 2 Layer 7 is removed from the semi-finished solar cell. The cleaning solution 8 may contain, for example, water, EDA (ethylenediamine), HCl, organic or phosphorus-based complexing agents, or any other suitable agent for removing CdCl formed during the annealing step 2 And/or a solvent for the oxidation product. These solutions are known to those skilled in the art.
In the last step, the CdCl is completely removed 2 After layer 7, a back contact layer 9 is applied to the activated CdTe or CdSeTe layer 4'. As a result, as shown in fig. 2F, an entire solar cell is formed comprising front contact layer 2, back contact layer 9, and a photoactive stack comprising a stack of window layer 3 and activated CdTe or CdSeTe layer 4'.
First embodiment of the apparatus
FIG. 3 shows an exemplary embodiment of the apparatus of the present invention, wherein the apparatus 100 is adapted to convert a CdS sacrificial layer to solid CdCl by means of HCl on a CdTe layer or material surface 2 A layer. The apparatus 100 includes a first device 10 and a second device 20.
The first device 10 comprises a first vacuum chamber 11, a first evacuation pump 12 connected to a first gas outlet 13 and adapted to remove gas from the interior of the first vacuum chamber 11, and a first gas inlet 15A first gas source 14. The first gas source 14 comprises a gas container 141 and a mass flow controller 142, the first gas source 14 being adapted to supply a gas (e.g., an inert gas, such as N 2 Or a reaction gas) is introduced into the first vacuum chamber 11 to control the pressure within the first vacuum chamber 11. Within the first vacuum chamber 11, there is a CdTe source 16 and a CdS source 17, where both the CdTe source 16 and the CdS source 17 are adapted to apply respective materials to the substrate 200 disposed over the respective CdTe source 16, cdS source 17. The CdS source 17 is adapted to apply the sacrificial layer of the invention to the surface of the material to which the CdTe layer is applied by the CdTe source 16. The CdTe source 16 and CdS source 17 can both be CSS sources. Since both the CdTe source 16 and the CdS source 17 are disposed within the same vacuum chamber (i.e., the first vacuum chamber 11), no vacuum interruption occurs between deposition of the CdTe layer and the sacrificial CdS layer.
Although not shown, if the apparatus 100 is used in the process of a superstrate structure solar cell, there may be an additional CdS source within the first vacuum chamber 11 suitable for applying a CdS layer as a window layer. In this case, an additional CdS source would be placed to the left of the CdTe source 16 relative to the x-axis. However, as described above, the window layer is not mandatory in each embodiment of the invention, and additional CdS sources may not be present.
In order to control the temperature of the substrate 200 during deposition of CdTe and CdS, one or more temperature control devices 18 may be present within the first vacuum chamber 11. The temperature control device 18 may comprise a heater and/or cooling device as known in the art.
Of course, in the apparatus 100, i.e. inside or outside the first vacuum chamber 11, there may be CdTe or CdS or other sources of other materials including Cd, se, te, zn, hg, mn, mg, S or a combination thereof, and the temperature control device 18 may also be arranged outside the first vacuum chamber 11.
The second device 12 comprises a second vacuum chamber 21, a second gas source 22 connected to a second gas inlet 23, and a second evacuation pump 14 connected to a second gas outlet 25 and adapted to remove gas from the interior of the second vacuum chamber 21. The second gas source 22 comprises two gas containers 221 and 222 and two mass flow controllers 223 and 224, each of the mass flow controllers 223,224One connected to one of the gas containers 221 or 222. The second gas source 22 is adapted to supply hydrogen chloride and another gas (e.g., an inert gas, such as N 2 ) Introduced into the second vacuum chamber 21. Thus, gas vessel 221 contains HCl and gas vessel 222 contains N 2 . The second gas source 22 is adapted to provide at each point in time two gases HCl and N in a predetermined ratio to each other 2 . This allows the sacrificial layer to be supplied with a gas containing hydrogen chloride and to be converted into a solid CdCl 2 The step of layering can be performed in which the volume of the gas containing hydrogen chloride and the pressure and composition of the gas in the second vacuum chamber 21 can be controlled. In addition, the substrate 200 may be moved in or out by evacuating the hazardous gases (e.g., HCl and H) before opening the second vacuum chamber 2 S) with non-critical gases (e.g. N 2 ) Purging is performed to ensure safety.
To provide a gas containing hydrogen chloride to the sacrificial layer and convert the sacrificial layer into solid CdCl 2 The temperature of the substrate 200 is controlled during the step of layering, and one or more temperature control devices 26 may be present within the second vacuum chamber 21. The temperature control device 26 may comprise a heater and/or cooling device as known in the art.
The apparatus 100 further comprises a transport system 30 (e.g. comprising a shaft with rollers), a control device 40 and gate valves 101 to 103. The transport system 30 is adapted to transport the substrate 200 through the apparatus 100, i.e. from the first gate valve 101 (wherein the substrate 200 moves into the first vacuum chamber 11), through the first vacuum chamber 11, through the second gate valve 102 (wherein the substrate 200 leaves the first vacuum chamber 11 and enters the second vacuum chamber 21), through the second vacuum chamber 21, and out of the third gate valve 103. As known to those skilled in the art, the second gate valve 102 may be replaced by two separate gate valves, one belonging to the first vacuum chamber 11 and the other belonging to the second vacuum chamber 21. The substrate 200 may be continuously or discontinuously moved along the x-axis as indicated by the arrow with respect to the substrate 200 within the second vacuum chamber 21. The control means 40 is adapted to control the functions of some or all controllable components of the apparatus 100, such as the evacuation pumps 12 and 24, the mass flow controllers 142, 223 and 224, the temperature control means 18 and 26, the delivery apparatus 30 and the gate valves 101 to 103. The control signals may be transmitted wirelessly or by wire. In fig. 3, control of the mass flow controllers 223 and 224 by the control device 40 is shown as an example.
Second embodiment of the method
Fig. 4A to 4C show some steps of a second exemplary embodiment of the method of the present invention. Fig. 4A shows a glass substrate 1 on which a front contact layer 2, a window layer 3, a CdTe or CdSeTe layer 4 and a sacrificial layer 5 are deposited in this order. The window layer 3 may also be omitted. For detailed information on the deposition process of each layer, please refer to the description of fig. 2A and 2B. Fig. 4A is substantially the same as fig. 2B.
As shown in fig. 4B, an additional solid layer 5a is formed on the sacrificial layer 5. The additional solid layer 5a is NH 4 And (3) a Cl film. For example, by reacting NH 4 An aqueous Cl solution is sprayed onto the sacrificial layer 5 and will then comprise a solution containing NH 4 The entire stack of liquid films of Cl is heated to a temperature in the range of 50 ℃ to 300 ℃ to deposit the additional solid layer 5a. Due to heating, contains NH 4 Water evaporation of the Cl liquid film and formation of solid NH 4 The Cl film, in which the thickness of the additional solid layer 5a may be determined by the amount of aqueous solution sprayed onto the sacrificial layer 5 or the number of spraying and drying steps performed in sequence. NH may also be initiated if the drying step is performed at a sufficiently high temperature 4 Decomposition of Cl. For example, the thickness of the additional solid layer 5a is in the range of 100nm to 1 μm.
Fig. 4C shows the semi-finished solar cell during a process step of providing a hydrogen chloride containing gas 6 to the sacrificial layer 5. Here, due to the temperature higher than NH 4 The decomposition temperature of the Cl film, thus providing gas 6 by decomposition of the additional solid layer 5a. This decomposition temperature is about 340 ℃ at atmospheric pressure, and may be lower at lower ambient pressures. Thus, the entire stack or at least the additional solid layer 5a is heated to a temperature between 200 ℃ and 350 ℃. As a result, the additional solid layer 5a is decomposed according to the following reaction equation:
NH 4 Cl(s)→NH 3 (g)+HCl(g)(3)
thus, the gas 6 contains HCl, which reacts with the sacrificial layer 5 to form CdCl 2 A layer. Subsequent steps of the methodAs shown in fig. 2D to 2F, and thus will not be repeated here.
Second embodiment of the apparatus
Fig. 5 shows a second exemplary embodiment of the device of the invention, wherein the device 110 is adapted to resort to NH on a sacrificial layer 4 HCl released during decomposition of the Cl-attached solid layer converts the CdS sacrificial layer to solid CdCl 2 A layer. The apparatus 110 includes a first device 10, a second device 20', and a third device 50 disposed between the first device 10 and the second device 20' in the production line.
The first device 10 is identical to the first device 10 of the apparatus 100 of fig. 3. Therefore, it will not be described again.
The third device 50 comprises a third vacuum chamber 51, a spraying device 52 (e.g. a nozzle array) and a temperature control device 53. Although not shown, the third apparatus may further include a gas inlet and a gas outlet or a vacuum pump for adjusting the composition and pressure of the atmosphere within the third vacuum chamber 51. The spraying device 52 is adapted to spray a solution of a material that releases hydrogen chloride upon decomposition onto the substrate 200. The temperature control means 53 is adapted to control the temperature of the substrate 200 such that the solution sprayed onto the substrate 200 dries and forms an additional solid layer. The temperature control means 53 may comprise a heater and/or cooling means as known in the art.
The second device 20' differs from the second device 20 of the apparatus 100 in fig. 3 in that it does not necessarily comprise a gas source and a gas inlet. The second device 20' comprises a second vacuum chamber 21, a second evacuation pump 24 connected to a second gas outlet 25 and adapted to remove gas from the interior of the second vacuum chamber 21, and one or more temperature control devices 26. The one or more temperature control devices 23 control the temperature of the substrate 200 such that the additional solid layer formed in the third device decomposes and releases hydrogen chloride. In addition, one or more temperature control devices 26 control the temperature of the substrate 200 such that the sacrificial layer reacts with the released hydrogen chloride to convert the sacrificial layer to solid CdCl 2 A layer. The one or more temperature control devices 26 may include heaters and/or cooling devices as known in the art. The second vacuum pump 24 discharges the solid CdCl converted in the sacrificial layer 2 Layer periodGas not consumed in the room. In addition, a second evacuation pump 24 and an optional gas source may be used to determine the composition and pressure of the atmosphere within the second vacuum chamber 21. Safety may be ensured by evacuating the hazardous gas and purging with a non-critical gas before opening the second vacuum chamber to move in or out of the substrate 200.
The apparatus 110 further comprises a delivery system 30 and gate valves 101 to 103 as described for the apparatus 100 in fig. 3. Furthermore, it comprises control means 40, similar to those described in fig. 3, adapted to control the functioning of some or all of the controllable components of the apparatus 110. In fig. 5, control of the temperature control devices 26 and 53 by the control device 40 is shown as an example.
In the above description, the embodiments of the present invention are given as examples by way of illustration, and the present invention is not limited thereto. Any combination of modifications, variations, and equivalent arrangements and embodiments should be considered to be included within the scope of the present invention.
Claims (13)
1. A kind of CdCl used for forming the solid on the surface of material 2 A method of layering comprising the steps of:
providing a surface of material on a substrate,
-applying a sacrificial layer containing cadmium on the surface of the material, and
-providing a hydrogen chloride containing gas to the sacrificial layer for a time sufficient to convert the sacrificial layer into solid CdCl 2 A predetermined period of time of the layer.
2. The method of claim 1, wherein the material surface is a surface of a layer comprising Cd, se, te, zn, hg, mn, mg, S or a combination thereof or a surface of a laminate.
3. The method according to claim 1 or 2, characterized in that the sacrificial layer is a CdS layer or a CdO layer.
4. A method according to claim 1 or 3, wherein the sacrificial layer is applied using a vacuum-based deposition method.
5. The method according to any one of claims 2 to 4, wherein the layer or stack is provided using a vacuum-based deposition method and no vacuum interruption occurs between the step of providing the layer or stack on the substrate and the step of applying the sacrificial layer.
6. The method of any one of claims 1 to 5, wherein the step of providing a hydrogen chloride containing gas to the sacrificial layer is performed within a process chamber and the hydrogen chloride containing gas is provided from a gas source outside the process chamber.
7. The method according to any one of claim 1 to 5, wherein,
-before the step of providing the sacrificial layer with a hydrogen chloride containing gas, the method further comprises the step of forming an additional solid layer on the sacrificial layer, wherein the additional solid layer consists of a material that decomposes into hydrogen chloride containing gas in the temperature range of 200 ℃ to 350 ℃ and
-the step of providing the sacrificial layer with a hydrogen chloride containing gas comprises temperature treating the additional solid layer formed on the sacrificial layer in the range of 200 ℃ to 350 ℃ to provide the sacrificial layer with a hydrogen chloride containing gas by decomposing the additional solid layer.
8. The method of claim 7, wherein the additional solid layer comprises NH 4 Cl。
9. A kind of CdCl used for forming the solid on the surface of material 2 An apparatus of layers, comprising:
a first device for applying a sacrificial layer containing cadmium on a material surface on a substrate, and
-second means for providing a hydrogen chloride containing gas to the sacrificial layer.
10. The apparatus of claim 9, wherein the first means is a vacuum chamber for performing a vacuum process to apply the sacrificial layer.
11. The apparatus of claim 10, wherein the first means is closely vacuum-coupled with means for providing a layer or stack comprising Cd, se, te, zn, hg, mn, mg, S or a combination thereof on the substrate.
12. The apparatus according to any one of claims 9 to 11, wherein the second device is a vacuum chamber comprising a gas inlet for introducing the hydrogen chloride containing gas and which allows the hydrogen chloride containing gas to be in contact with the surface of the sacrificial layer.
13. The apparatus according to any one of claims 9 to 12, characterized in that
The device further comprises third means for applying an additional solid layer on the sacrificial layer, wherein the additional solid layer consists of a material that decomposes into a gas containing hydrogen chloride in the temperature range of 200 ℃ to 350 ℃ and
-the second means is a vacuum chamber comprising a temperature control unit for heating the additional solid layer formed on the sacrificial layer to provide a hydrogen chloride containing gas to the sacrificial layer by decomposing the additional solid layer.
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