CN114907774B - Lyophobic coating, preparation method thereof and flower basket - Google Patents
Lyophobic coating, preparation method thereof and flower basket Download PDFInfo
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- CN114907774B CN114907774B CN202210692767.XA CN202210692767A CN114907774B CN 114907774 B CN114907774 B CN 114907774B CN 202210692767 A CN202210692767 A CN 202210692767A CN 114907774 B CN114907774 B CN 114907774B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
- C09D7/68—Particle size between 100-1000 nm
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
- C09D7/69—Particle size larger than 1000 nm
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/80—Processes for incorporating ingredients
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/673—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere using specially adapted carriers or holders; Fixing the workpieces on such carriers or holders
- H01L21/67303—Vertical boat type carrier whereby the substrates are horizontally supported, e.g. comprising rod-shaped elements
- H01L21/67306—Vertical boat type carrier whereby the substrates are horizontally supported, e.g. comprising rod-shaped elements characterized by a material, a roughness, a coating or the like
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to the field of solar cell manufacturing, and particularly relates to a lyophobic coating, a preparation method thereof and a flower basket. The lyophobic coating comprises the following raw materials in parts by weight: silicone resin, micro-nano particles, a modifier, a cross-linking agent and a solvent; the silicon resin is fluorine silicon copolymer resin and/or epoxy silicon resin, and the micro-nano particles are made of silicon nitride and/or polyether-ether-ketone. The lyophobic coating can effectively reduce the surface energy state of the silicon resin, and the micro-nano particles are combined to increase the microscopic roughness of the coating, so that the whole coating has lotus leaf effect, has more excellent lyophobic performance, and can play the purpose of no or less liquid carrying even in a certain acid-base environment, thereby fundamentally solving the problems of poor cleaning capability caused by liquid carrying in the process of recycling the flower basket, high silicon chip occupation ratio with flower basket latch marks, capacity limitation and the like.
Description
Technical Field
The invention belongs to the field of solar cell manufacturing, and particularly relates to a lyophobic coating, a preparation method thereof and a flower basket.
Background
Photovoltaic power generation is one of the main clean energy sources at present, and is a technology for directly converting light energy into electric energy by utilizing the photovoltaic effect of a semiconductor interface, and a key element of the technology is a solar cell. The main solar cell manufacturing process in the market at present comprises different procedures of texturing, diffusion, etching, coating, screen printing and the like. The surface of the solar cell can be textured through texturing, the surface reflectivity of the solar cell is effectively reduced, incident light is reflected on the surface of the solar cell for multiple times, the optical path is prolonged, the absorption of infrared photons is increased, more photons generate photogenerated carriers near the P-N junction, and the collection probability of the photogenerated carriers can be increased, so that the photoelectric conversion efficiency of the solar cell is improved. Thus, the texturing process (i.e., the silicon etching process) is the most basic, critical technique in silicon micromachining. There are generally two types of techniques for this: the dry etching and the wet etching are classified into acid etching and alkali etching according to the difference of the etchant. For the etching process, there are also dry etching and wet etching, and wet etching can be classified into acid polishing system wet etching and alkali polishing system wet etching according to the difference of etching systems.
When the wet process is adopted to prepare the solar cell, the silicon wafers are carried by the basket to carry out batch operation, and after being treated by the acid tank and the alkali tank, the silicon wafers are also required to be washed by the water tank and then dried. The current basket for carrying the silicon wafers has the following defects: (1) The basket of flowers can carry liquid after passing through the acid tank and the alkali tank, so that the cleaning water tank is acidic or alkaline and does not have the cleaning effect; (2) When the basket is provided with acid liquor or alkali liquor, the contact position of the basket latch and the silicon wafer can generate corrosion reaction, and the corrosion reaction can be continuously carried out after the basket latch leaves the acid tank or the alkali tank, so that the whole reaction of the silicon wafer presents non-uniformity, which is particularly obvious in the velvet making process, and is typically characterized in that the basket latch is printed; (3) When the waste water passes through the drying tank, the drying time is prolonged because the flower basket is seriously carried with liquid, and the drying process in the wet process is a whole production capacity limiting link.
Therefore, the problem of liquid carrying of the flower basket is solved, and the method is particularly suitable for acid liquid and alkali liquid treatment in a wet preparation process, and is a technical problem which needs to be solved in the current solar cell preparation process.
Disclosure of Invention
In view of the above, the present invention provides a lyophobic coating capable of improving lyophobic performance of a flower basket and a preparation method thereof, and correspondingly provides a flower basket adopting the lyophobic coating.
The invention aims at realizing the following technical scheme:
in one aspect, the invention provides a lyophobic coating, which comprises the following raw materials in parts by weight: silicone resin, micro-nano particles, a modifier, a cross-linking agent and a solvent;
the silicon resin is fluorine silicon copolymer resin and/or epoxy silicon resin, and the micro-nano particles are made of silicon nitride and/or polyether-ether-ketone.
Optionally, the lyophobic coating comprises the following raw materials: 100-120 parts of silicone resin, 30-50 parts of micro-nano particles, 10-20 parts of modifier, 0.08-0.15 part of cross-linking agent and 300-400 parts of solvent.
Preferably, the ratio of the particle size of the micro-nano particles to the thickness of the lyophobic coating is 0.4-1.
Preferably, the weight ratio of the modifier to the silicone is greater than 0.15.
Further preferably, the lyophobic coating comprises the following raw materials: 110 parts of silicon resin, 35 parts of micro-nano particles, 20 parts of modifier, 0.15 part of cross-linking agent and 350 parts of solvent; the ratio of the particle size of the micro-nano particles to the thickness of the lyophobic coating is 0.4-1.
Optionally, the micro-nano particles have a particle size of 0.1-50 μm.
Optionally, the lyophobic coating has a thickness of 10-100 μm.
Optionally, the modifier is vinyl silicone oil.
Optionally, the cross-linking agent is a platinum catalyst and/or ethyl orthosilicate.
Optionally, the solvent is toluene and/or ethyl acetate.
On the other hand, the invention also provides a preparation method of the lyophobic coating, which comprises the following steps:
respectively weighing the silicon resin, the micro-nano particles, the modifier, the cross-linking agent and the solvent according to the formula amount;
mixing the solvent, the silicone resin and the modifier, adding the cross-linking agent after stirring for a first time, continuously stirring for a second time, adding the micro-nano particles, and standing for a third time after stirring to obtain a mixed solution;
applying the mixed solution to the surface of a workpiece, and then solidifying;
the silicon resin is fluorine silicon copolymer resin and/or epoxy silicon resin, and the micro-nano particles are made of silicon nitride and/or polyether-ether-ketone.
Optionally, the formula amount is: 100-120 parts of silicone resin, 30-50 parts of micro-nano particles, 10-20 parts of modifier, 0.08-0.15 part of cross-linking agent and 300-400 parts of solvent.
Optionally, the first time is 30-60 min, the second time is 15-30 min, and the third time is 50-70 min.
Optionally, the temperature of the curing step is 150-180 ℃ and the curing time is 30-50 min.
In a third aspect, the invention also provides a flower basket, and a lyophobic coating is coated on the surface of the flower basket, wherein the lyophobic coating is the lyophobic coating or prepared by the method.
Optionally, the lyophobic coating has a thickness of 10-100 μm.
Compared with the prior art, the technical scheme of the invention has the following advantages:
1. the lyophobic coating provided by the invention comprises the following raw materials of silicon resin, micro-nano particles, a modifier, a cross-linking agent and a solvent; the silicon resin is fluorine-silicon copolymer resin and/or epoxy silicon resin, and the micro-nano particles are made of silicon nitride and/or polyether-ether-ketone. Because the application occasion of the invention is an acid tank and an alkali tank in the solar cell wet preparation process, the coating itself needs to resist acid/alkali corrosion, so the invention selects acid/alkali resistant resins such as fluorosilicon copolymer resin, epoxy silicone resin and the like as carriers, and selects acid/alkali resistant silicon nitride and polyether ether ketone micro-nano particles, thereby ensuring that the coating can keep lyophobic effect under an acid or alkali system.
In the wet preparation process of the solar cell, surfactants are added into the acid liquid and the alkali liquid used in the steps of texturing and alkali polishing, so that the solutions have smaller surface tension than water, and an effective hydrophobic effect is difficult to achieve. According to the lyophobic coating, the specific modifier is adopted, so that the surface energy state of the silicone resin is further effectively reduced, the original high polymer linear structure in the silicone resin is converted into a space reticular structure through a series of chemical reactions by using the cross-linking agent, so that the space reticular structure has excellent mechanical property and hydrolysis resistance, and the micro-nano particles with specific granularity are combined to increase the micro-roughness of the coating, so that the integral coating has a lotus leaf effect, has more excellent lyophobic performance, and achieves the purpose of no or less liquid in a wet process, thereby fundamentally solving the problems of poor cleaning capability, high silicon wafer ratio with flower basket and latch marks, limited productivity and the like caused by liquid in the cyclic use process of the flower basket.
2. According to the preparation method of the lyophobic coating, the solvent, the silicon resin and the modifier are uniformly mixed, the cross-linking agent is added, and the micro-nano particles are added and stirred, so that agglomeration of the micro-nano particles can be effectively avoided, and the preparation of the coating with uniform roughness surface is facilitated. The preparation method of the lyophobic coating does not need heating reflux, is simpler and more convenient, and is easy to operate.
Drawings
In order to more clearly illustrate the embodiments of the present invention, the drawings that are required to be used in the description of the embodiments will be briefly described below, it being apparent that the drawings in the following description are some embodiments of the present invention and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a flow chart of a method for preparing a lyophobic coating according to an embodiment of the invention;
FIG. 2 is a schematic view of a basket with lyophobic coating according to an embodiment of the present invention;
fig. 3 is a schematic view of the surface morphology of the lyophobic coating of fig. 2 when enlarged 200 times.
Wherein reference numerals are as follows:
1-the surface of a flower basket; 2-coating a body; 3-micro-nano particles.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
The technical conception of the invention is as follows: the technical problems are caused by the fact that the basket for bearing the silicon wafer is in a certain acid-base environment in the texturing process, so that the lyophobic property of the conventional lyophobic coating is reduced. Based on this, the technical scheme of this application lies in increasing the coating that one deck has better lyophobic effect at the surface of basket to improve the lyophobic performance of basket.
Although the prior art is not lack of researches on hydrophobic coatings, the object of the researches on the technologies is either pure water or rainwater, and the inventor tries to apply the existing hydrophobic coatings to flower baskets, but the problems of poor cleaning capability of a cleaning water tank, high silicon wafer ratio with flower basket latch marks, overlong drying time and the like in the solar cell preparation process cannot be solved. The inventor finds that, because the application occasion of the flower basket is not a pure water or rainwater system, but an acid liquor and alkali liquor environment used in the processes of making wool and throwing alkali, surfactants are added in the acid liquor and the alkali liquor, and the surfactants enable the solution to have smaller surface tension than water, so that the coating is more difficult to achieve an effective lyophobic effect.
For this purpose, the invention provides the following technical scheme:
in one aspect, the invention provides a lyophobic coating, which comprises the following raw materials in parts by weight:
silicone, as a carrier material, providing a low surface energy;
micro-nano particles for increasing the micro roughness of the surface of the coating and providing a lotus leaf effect;
a modifier for further reducing the surface energy of the silicone resin;
a cross-linking agent for converting the original linear structure of the silicone resin into a space network structure;
a solvent;
wherein the silicone resin is fluorine silicone copolymer resin and/or epoxy silicone resin, and the resin has acid/alkali resistance; the micro-nano particles are made of silicon nitride and/or polyether-ether-ketone, and have good acid/alkali resistance. According to the lyophobic coating, acid/alkali resistant resins such as fluorosilicone copolymer resin, epoxy silicone resin and the like are selected as carriers, and meanwhile, acid/alkali resistant silicon nitride and polyether-ether-ketone micro-nano particles are selected, so that the lyophobic coating can act under an acidic or alkaline system, and a good lyophobic effect is obtained.
As an optional embodiment, the lyophobic coating comprises the following raw materials in parts by weight: 100-120 parts of silicone resin, 30-50 parts of micro-nano particles, 10-20 parts of modifier, 0.08-0.15 part of cross-linking agent and 300-400 parts of solvent.
Preferably, the ratio of the particle size of the micro-nano particles to the thickness of the lyophobic coating is 0.4-1; and/or the weight ratio of the modifier to the silicone is greater than 0.15. Experiments show that the lyophobic coating has better lyophobic performance when meeting any condition.
Preferably, the modifier is vinyl silicone oil; the cross-linking agent is a platinum catalyst and/or ethyl orthosilicate; the particle size of the micro-nano particles is 0.1-50 mu m; the thickness of the lyophobic coating is 10-100 mu m. According to the lyophobic coating, the surface energy state of the silicon resin is further effectively reduced by adopting the specific modifier, the original high polymer linear structure in the silicon resin is converted into a space reticular structure through a series of chemical reactions by utilizing the cross-linking agent, so that the space reticular structure has excellent mechanical property and hydrolysis resistance, and the micro-nano particles with specific granularity are combined to increase the micro-roughness of the coating, so that the integral coating has a lotus leaf effect, has more excellent lyophobic performance, ensures that the lyophobic coating can be suitable for acid liquid and alkali liquid treatment in a wet preparation process, and achieves the purpose of no or less liquid in the wet preparation process, thereby fundamentally solving the problems of poor cleaning capability, silicon chip ratio with flower basket latch marks, capacity limitation and the like caused by liquid in the cyclic use process of the flower basket.
On the other hand, as shown in fig. 1, the invention provides a preparation method of a lyophobic coating for a flower basket, which comprises the following steps:
respectively weighing the silicon resin, the micro-nano particles, the modifier, the cross-linking agent and the solvent according to the formula amount;
mixing the solvent, the silicone resin and the modifier, adding the cross-linking agent after stirring for a first time, continuously stirring for a second time, adding the micro-nano particles, and standing for a third time after stirring to obtain a mixed solution;
applying the mixed solution to the surface of a workpiece, and then solidifying;
the silicon resin is fluorine silicon copolymer resin and/or epoxy silicon resin, and the micro-nano particles are made of silicon nitride and/or polyether-ether-ketone.
Preferably, the solvent is mixed with the silicone resin and the modifier, the high-speed dispersing machine is used for stirring for 30-60 min, the cross-linking agent is added for continuous stirring for 15-30 min, the micro-nano particles are added for stirring for 50-70 min, and the mixture is kept stand for 30-50 min to obtain a mixed solution; spraying the mixed solution onto the surface of a flower basket, and then placing the flower basket into a constant temperature curing box at 150-180 ℃ for curing for 30-50 min to obtain the lyophobic coating with the thickness of 10-100 mu m.
In the lyophobic coating, the silicon resin is fluorine-silicon copolymer resin and/or epoxy silicon resin; the micro-nano particles are made of silicon nitride and/or polyether-ether-ketone, and the modifier is vinyl silicone oil; the cross-linking agent is platinum catalyst and/or tetraethoxysilane; the solvent is toluene and/or ethyl acetate. The surface energy state of the silicon resin can be effectively reduced by using the modifier, the silicon resin forms a space network structure by using the cross-linking agent, the mechanical property and the hydrolysis resistance of the silicon resin are improved, and the micro-nano particles can be used for increasing the micro-roughness of the coating, so that the coating has more excellent lyophobic property.
According to the lyophobic coating, the thickness of the coating is 10-100 mu m, so that micro-nano particles with the particle size of 0.1-50 mu m are selected, if the particle size is too small, rough surfaces are difficult to form, and if the particle size is too large, the organic carrier is difficult to wrap and fix the particles, so that the particles are easy to separate from the carrier surface, and a better lyophobic effect cannot be achieved. Experiments show that when the ratio of the particle size of the micro-nano particles to the thickness of the coating is in the range of 0.4-1 and the mass ratio of the modifier to the resin is more than 0.15, the lyophobic performance of the coating is best.
In yet another aspect, the present invention provides a basket, as shown in fig. 2 and 3, wherein a lyophobic coating is coated on the surface 1 of the basket, wherein the lyophobic coating is the lyophobic coating or the lyophobic coating prepared by the method. From the microstructure, the lyophobic coating comprises a coating body 2 and micro-nano particles 3, wherein the micro-nano particles 3 are uniformly embedded on the surface of the coating body 2, and the coating body 2 is formed by reacting silicone resin, a modifier and a cross-linking agent, and specifically comprises the following components: under the dispersion action of the solvent, the silicone resin is fully contacted with the modifier and the cross-linking agent and reacts, namely, the surface energy state of the silicone resin is reduced by the modifier, the silicone resin forms a space network structure by the cross-linking agent, and then the silicone resin is solidified to volatilize the solvent, so that the coating body is obtained. The micro-nano particles 3 are uniformly embedded on the surface of the coating body 2, so that the lotus leaf effect can be better exerted.
According to the flower basket provided by the invention, as the lyophobic coating is coated on the surface, the flower basket can be free of liquid in the solar cell wet preparation process, so that the problems of poor cleaning capability, high silicon wafer occupation ratio with flower basket latch marks, limited productivity and the like caused by liquid in the process of recycling the flower basket are fundamentally solved.
Specific lyophobic coating, preparation method thereof and flower basket will be described in detail by examples.
Example 1
In the preparation method of the lyophobic coating of the embodiment, 100g of fluorine-silicon copolymer resin, 50g of silicon nitride particles with the particle size of 20-50 mu m, 10g of vinyl silicone oil, 0.15g of platinum catalyst and 300g of toluene are respectively weighed;
mixing toluene, fluorosilicone copolymer resin and vinyl silicone oil, stirring for 30min by using a high-speed dispersing machine, adding a platinum catalyst, continuously stirring for 30min, adding silicon nitride particles, stirring for 50min, and standing for 50min to obtain a mixed solution;
spraying the mixed solution on the surface of the flower basket, and then placing the flower basket into a constant temperature curing box at 180 ℃ for curing for 30min to obtain the flower basket with the lyophobic coating with the thickness of 10 mu m.
Example 2
In the preparation method of the lyophobic coating of the embodiment, 120g of epoxy silicon resin, 30g of silicon nitride particles with the particle size of 0.1-10 mu m, 15g of vinyl silicone oil, 0.1g of tetraethoxysilane and 400g of ethyl acetate are respectively weighed;
mixing toluene, epoxy silicone resin and vinyl silicone oil, stirring for 45min by using a high-speed dispersing machine, adding tetraethoxysilane, continuously stirring for 15min, adding silicon nitride particles, stirring for 50min, and standing for 40min to obtain a mixed solution;
spraying the mixed solution on the surface of the flower basket, and then placing the flower basket into a constant temperature curing box at 150 ℃ for curing for 30 minutes to obtain the flower basket with the lyophobic coating with the thickness of 30 mu m.
Example 3
In the preparation method of the lyophobic coating of the embodiment, 110g of epoxy silicone resin, 50g of polyether-ether-ketone particles with the particle size of 10-30 mu m, 20g of vinyl silicone oil, 0.08g of tetraethoxysilane and 360g of toluene are respectively weighed;
mixing toluene, epoxy silicone resin and vinyl silicone oil, stirring for 60min by using a high-speed dispersing machine, adding tetraethoxysilane, continuously stirring for 20min, adding polyether-ether-ketone particles, stirring for 60min, and standing for 40min to obtain a mixed solution;
spraying the mixed solution on the surface of the flower basket, and then placing the flower basket into a constant temperature curing box at 170 ℃ for curing for 50min to obtain the flower basket with the lyophobic coating with the thickness of 80 mu m.
Example 4
In the preparation method of the lyophobic coating of the embodiment, 120g of fluorosilicone copolymer resin, 40g of polyether-ether-ketone particles with the particle size of 10-25 mu m, 18g of vinyl silicone oil, 0.12g of platinum catalyst and 330g of ethyl acetate are respectively weighed;
mixing toluene, fluorosilicone copolymer resin and vinyl silicone oil, stirring for 50min by using a high-speed dispersing machine, adding a platinum catalyst, continuously stirring for 25min, adding polyether-ether-ketone particles, stirring for 70min, and standing for 40min to obtain a mixed solution;
spraying the mixed solution on the surface of the flower basket, and then placing the flower basket into a constant temperature curing box at 160 ℃ for curing for 40min to obtain the flower basket with the lyophobic coating with the thickness of 100 mu m.
Example 5
In the preparation method of the lyophobic coating of the embodiment, 110g of fluorine-silicon copolymer resin, 35g of silicon nitride particles with the particle size of 20-50 mu m, 20g of vinyl silicone oil, 0.15g of platinum catalyst and 350g of toluene are respectively weighed;
mixing toluene, fluorosilicone copolymer resin and vinyl silicone oil, stirring for 30min by using a high-speed dispersing machine, adding a platinum catalyst, continuously stirring for 20min, adding silicon nitride particles, stirring for 70min, and standing for 40min to obtain a mixed solution;
spraying the mixed solution on the surface of the flower basket, and then placing the flower basket into a constant temperature curing box at 180 ℃ for curing for 30min to obtain the flower basket with the lyophobic coating with the thickness of 50 mu m.
Example 6
In the preparation method of the lyophobic coating of the embodiment, 110g of epoxy silicone resin, 25g of polyether-ether-ketone particles with the particle size of 10-20 mu m, 15g of vinyl silicone oil, 0.12g of tetraethoxysilane and 350g of toluene are respectively weighed;
mixing toluene, epoxy silicone resin and vinyl silicone oil, stirring for 45min by using a high-speed dispersing machine, adding tetraethoxysilane, continuously stirring for 15min, adding polyether-ether-ketone particles, stirring for 60min, and standing for 30min to obtain a mixed solution;
spraying the mixed solution on the surface of the flower basket, and then placing the flower basket into a constant temperature curing box at 180 ℃ for curing for 30min to obtain the flower basket with the lyophobic coating with the thickness of 60 mu m.
Comparative example 1
In the preparation method of the lyophobic coating of this comparative example, the contents are the same as in example 5 except for the following.
Heptadecafluorodecyl trimethoxysilane is used instead of vinyl silicone oil.
Comparative example 2
In the preparation method of the lyophobic coating of this comparative example, the contents are the same as in example 5 except for the following.
The silicon nitride particles with the particle size of 10-35 nm replace the silicon nitride particles with the particle size of 20-50 mu m.
Comparative example 3
In the preparation method of the lyophobic coating of this comparative example, the contents are the same as in example 5 except for the following.
Silicon nitride particles having a particle diameter of 60 to 100 μm replace silicon nitride particles having a particle diameter of 20 to 50. Mu.m.
Comparative example 4
In this comparative example, an existing basket of flowers was used, i.e. without lyophobic coating.
Comparative example 5
In the preparation method of the lyophobic coating of the comparative example, the hydrophobic coating liquid prepared in example 3 of chinese patent document CN109627980 a was sprayed onto the surface of the basket, and then placed in a constant temperature curing oven at 180 ℃ for curing for 30min, to obtain a basket with a lyophobic coating having a thickness of 50 μm.
Experimental example
In the preparation method of the lyophobic coating of this experimental example, a pickling tank was used as an example, and a basket having the coatings of examples 3, 5 to 6 and comparative examples 1 to 5 and a basket having no lyophobic coating of the prior art were used for the silicon wafer texturing treatment and the drying treatment, and the results are shown in table 1.
Meanwhile, table 1 also shows the surface contact angle of the basket of flowers in the acid solution measured at 25 ℃. The difference of the lyophobic performance can be intuitively reflected by the different contact angles. In general, the larger the contact angle, the better the hydrophobic properties, i.e. the better the lyophobic properties.
TABLE 1
The inventors have found through long-time multiple experiments that the lyophobic performance of the hydrophobic coating is best when the ratio of the particle size of the micro-nano particles to the thickness of the coating is in the range of 0.4-1 and the mass ratio of the modifier to the resin is more than 0.15. As is clear from Table 1, in examples 3 and 5 to 6, example 5 satisfies both of the above two conditions (micro-nano particle size 20 to 50 μm, lyophobic coating thickness 50 μm, modifier mass 20g, fluorosilicone copolymer resin mass 110 g), example 6 satisfies only the former condition (micro-nano particle size 10 to 20 μm, lyophobic coating thickness 60 μm, modifier mass 15g, epoxy silicone resin 110 g), and example 3 satisfies only the latter condition (micro-nano particle size 10 to 30 μm, lyophobic coating thickness 80 μm, modifier mass 20g, epoxy silicone resin 110 g). Example 5 is the best mode. Compared with comparative examples 1 to 5, the flower basket of examples 3 and 5 to 6 has larger contact angle in acid solution and stronger lyophobic capability, and meanwhile, as can be seen from table 1, the flower basket has no liquid due to the increased contact angle of the flower basket caused by the coating, so the flower basket can stabilize the pH value of the liquid in the cleaning tank (namely, the flower basket does not carry liquid from the acid tank, the alkali tank or less liquid), and the flower basket of examples 3 and 5 to 6 can stabilize the pH value of the liquid in the cleaning tank at 6 to 7; the card mark ratio of the basket is reduced, or the card tooth mark ratio of the basket is smaller; the drying time is shortened, so that the drying time is shorter and the drying is easier.
Taking a pickling tank as an example, using a flower basket with the hydrophobic coating, wherein the pH value of the pickling tank is stabilized at 6-7, the card tooth mark ratio of the flower basket is 0.01%, and the drying time is 500s. In the prior art, the pH value of the pickling tank is 4-5, the card tooth mark ratio of the basket is 0.02%, and the drying time is 600s.
Therefore, the lyophobic coating of the invention adopts acid/alkali resistant resins such as fluorine-silicon copolymer resin, epoxy silicon resin and the like as carriers, and adopts acid/alkali resistant silicon nitride and polyether-ether-ketone micro-nano particles, so that the lyophobic coating of the invention can keep lyophobic effect under an acidic or alkaline system. Furthermore, the lyophobic coating reduces the surface energy state of the carrier through the modifier, combines the lotus leaf effect of the micro-nano particles, can ensure that the coating has more excellent lyophobic performance, can ensure that the basket is free from liquid in the wet preparation process of the solar cell, and fundamentally avoids the problems of poor cleaning capability, high silicon wafer occupation ratio with basket latch marks, limited productivity and the like caused by liquid in the cyclic use process of the basket.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (8)
1. The lyophobic coating is used for a flower basket and is characterized by comprising the following raw materials: silicone resin, micro-nano particles, a modifier, a cross-linking agent and a solvent;
wherein the silicon resin is fluorine silicon copolymer resin and/or epoxy silicon resin,
the micro-nano particles are made of silicon nitride and/or polyether-ether-ketone, and the particle size of the micro-nano particles is 0.1-50 mu m;
the cross-linking agent is a platinum catalyst and/or ethyl orthosilicate;
the modifier is vinyl silicone oil;
100-120 parts of silicone resin, 30-50 parts of micro-nano particles, 10-20 parts of modifier, 0.08-0.15 part of cross-linking agent and 300-400 parts of solvent.
2. The lyophobic coating according to claim 1, wherein the ratio of the particle size of the micro-nano particles to the thickness of the lyophobic coating is 0.4-1; and/or the weight ratio of the modifier to the silicone is greater than 0.15.
3. The lyophobic coating according to claim 1, wherein the silicone resin is 110 parts, the micro-nano particles are 35 parts, the modifier is 20 parts, the cross-linking agent is 0.15 parts, and the solvent is 350 parts; the ratio of the particle size of the micro-nano particles to the thickness of the lyophobic coating is 0.4-1.
4. The lyophobic coating according to claim 1, wherein the lyophobic coating has a thickness of 10-100 μm; and/or the solvent is toluene and/or ethyl acetate.
5. The preparation method of the lyophobic coating is characterized by comprising the following steps of:
respectively weighing the silicon resin, the micro-nano particles, the modifier, the cross-linking agent and the solvent according to the formula amount; the formula comprises the following components in percentage by weight: 100-120 parts of silicone resin, 30-50 parts of micro-nano particles, 10-20 parts of modifier, 0.08-0.15 part of cross-linking agent and 300-400 parts of solvent;
mixing the solvent, the silicone resin and the modifier, adding the cross-linking agent after stirring for a first time, continuously stirring for a second time, adding the micro-nano particles, and standing for a third time after stirring to obtain a mixed solution;
applying the mixed solution to the surface of a workpiece, and then solidifying; the workpiece is a flower basket;
wherein the silicon resin is fluorine silicon copolymer resin and/or epoxy silicon resin,
the micro-nano particles are made of silicon nitride and/or polyether-ether-ketone, and the particle size of the micro-nano particles is 0.1-50 mu m;
the cross-linking agent is a platinum catalyst and/or ethyl orthosilicate;
the modifier is vinyl silicone oil.
6. The method of preparing a lyophobic coating according to claim 5, wherein the first time is 30 to 60min, the second time is 15 to 30min, and the third time is 50 to 70min;
the temperature of the curing step is 150-180 ℃ and the curing time is 30-50 min.
7. A flower basket coated with a lyophobic coating on its surface, said lyophobic coating being according to any one of claims 1 to 4 or prepared by the method of claim 5 or 6.
8. The basket according to claim 7, wherein the lyophobic coating has a thickness of 10-100 μm.
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| CN101962514B (en) * | 2010-09-27 | 2013-07-10 | 复旦大学 | High-durability super-hydrophobic self-cleaning coating material and preparation method thereof |
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