CN109225780A - A kind of production method of antifog glass - Google Patents

A kind of production method of antifog glass Download PDF

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Publication number
CN109225780A
CN109225780A CN201811121218.7A CN201811121218A CN109225780A CN 109225780 A CN109225780 A CN 109225780A CN 201811121218 A CN201811121218 A CN 201811121218A CN 109225780 A CN109225780 A CN 109225780A
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China
Prior art keywords
glass
production method
metal
conductive
antifog
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CN201811121218.7A
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Chinese (zh)
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CN109225780B (en
Inventor
简明德
王乾廷
董俊豪
骆润松
沈茂田
宋耀东
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Fujian University of Technology
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Fujian University of Technology
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Publication of CN109225780A publication Critical patent/CN109225780A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/12Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain a coating with specific electrical properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00Processes for applying liquids or other fluent materials
    • B05D1/02Processes for applying liquids or other fluent materials performed by spraying
    • B05D1/04Processes for applying liquids or other fluent materials performed by spraying involving the use of an electrostatic field
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2203/00Other substrates
    • B05D2203/30Other inorganic substrates, e.g. ceramics, silicon
    • B05D2203/35Glass

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Glass Compositions (AREA)

Abstract

The present invention relates to a kind of production methods of antifog glass, including electric heating layer is arranged on the glass substrate, spray vehicle glass de-fog electrocondution slurry on the glass substrate by the way of electrostatic spraying, are formed by curing the electric heating layer.The present invention is by the way of electrostatic spraying, it is poor to can solve traditional silver powder dispersibility caused by existing silver powder reunion during silk-screen printing prepares electrocondution slurry, to reduce the defect of electric conductivity, film is made to have the characteristics that wearability is strong, anticorrosive, adhesive force is strong, uniform color by electrostatic spraying.The present invention can reduce nano-silver powder and reunite, and equably be adsorbed on by the surface of painting glass, heated to be formed by curing smooth, uniform, smooth coating, no pollution to the environment is realized, curing time is short, and adhesive force is strong, presentation quality is excellent, at low cost etc., provides better electric conductivity.

Description

A kind of production method of antifog glass
Technical field
The present invention relates to a kind of production methods of antifog glass.
Background technique
Electric slurry is a kind of electronic functional material of high-tech, mainly for the manufacture of thick film integrated circuit, solar-electricity Pond electrode, automobile back windshield etc..Electric slurry is made of conductive phase, glass powder and organic carrier.Currently, conductive phase mainly has Noble metal and its oxide conducting phase: mainly with noble metals and its oxygen such as golden (Au), silver-colored (Ag), palladium (Pd), platinum (Pt), ruthenium (Ru) Compound has many advantages, such as that high temperature resistant, corrosion-resistant, waterproof, dielectric strength are high, thermal conductivity is high as conductive phase.There are also carbon series conductives Phase: mainly using the carbon-based material of the low cost such as carbon black, graphite as conductive phase.Base metal and its oxide conducting phase: mainly with Copper, zinc, barium carbonate, strontium lanthanum manganese oxide, cobalt strontium lanthanum oxide etc. are used as conductive phase, cheap.
Heater wire on automobile back windshield is used to remove frost mist, it has also become one of essential device of automobile.Glass of automobile The heater wire effect of glass is to generate heat after being powered to the frost mist for eliminating glass surface, the vehicle glass with heating wires Very widely used, it keeps out the wind after being almost applied to all car glasses, in car glass art, is chiefly used in window driver and removes Mist.It is that dedicated conductive silver paste is printed onto the surface of glass by way of silk-screen printing to such heating wires, glass warp After tempering, conductive silver paste is sintered to glass surface, since it is with certain resistance, can generate heat after energization.This glass of automobile The screen painting of glass heater wire still has many deficiencies: 1) nanoparticle is easy to oxidize, and the binding force between particle is weak, causes Wearability is poor after sintering;2) it is not easy to form the graphical silver paste conductive layer of fine, the edge of conductive layer is unsmooth, has saw Dentation is unfavorable for preparing the conducting wire of low-resistivity;3) it in order to obtain low-resistance conductive silver paste, can all be used in ink big Silver powder is measured, nano-silver powder is easy to reunite, on the other hand be led due to the presence of glass powder so that the electric conductivity of conductive silver paste is poor Cause the phenomenon of generation demisting unevenness.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of production method of antifog glass.Pass through electrostatic spraying shape At the high and smooth coating of compactness, so that film has the characteristics that high rigidity, adhesive force are good, square resistance is low.
The present invention is implemented as follows:
The present invention provides a kind of production methods of antifog glass, including electric heating layer is arranged on the glass substrate, It sprays vehicle glass de-fog electrocondution slurry on the glass substrate by the way of electrostatic spraying, is formed by curing the electricity fever Layer.
Further, the condition of the electrostatic spraying are as follows: 60~90kV of spray voltage, 10~20uA of electric current, flow velocity pressure Power 0.3-0.45MPa spray time 20~50 seconds, 30~60 ㎜ of spray gun reciprocating speed/second, is sprayed 2~5cc/ of flow seconds, spray gun Mouth and workpiece distance 100mm-150mm, 70 °~90 ° of spray angle.Anode is connected substrate to be sprayed by the electrostatic spraying And be grounded, and cathode high pressure connects electrostatic gun, it muzzle and is sprayed-on substrate and forms a strong electric field region, compressed air when spraying By electrocondution slurry powder be pumped to electrostatic gun mouth atomization, under the action of electric field, fly to anode rapidly, be equably adsorbed on by Heated to be formed by curing electric heating layer on the surface for applying substrate, the coating surface is smooth, uniform, bubble-free, flawless.
Further, the vehicle glass de-fog electrocondution slurry, composed of the following components by mass percentage: carbon system leads Electric phase 10~15%, metal and metal conductive oxide phase 65~80%, organic binder 5%-15%, glass powder 5%- 15%, above-mentioned each component mass percent summation is 100%.
Further, the metal and metal conductive oxide phase, the oxide including following metal and metal: gold Au, silver Ag, palladium Pd, platinum Pt, ruthenium Ru, copper, zinc, barium carbonate, strontium lanthanum manganese oxide, cobalt strontium lanthanum oxide, partial size 100-200nm;It is described Carbon series conductive mutually includes carbon black, graphite, partial size 100um-500um.
Further, the organic binder be selected from polyethylene glycol, diethylene glycol methyl ether, terpinol, glycol monoethyl ether, Ethylene glycol monoethyl ether, N-Methyl pyrrolidone, N-N dimethyl acetamide, Sodium Polyacrylate, polyvinylpyrrolidone, polyphenyl sulphur Sour sodium, polyimides, low molecule pa resin, acrylic acid modified alkyd resin, styrenated alkyd, ureaformaldehyde tree Rouge;Its viscosity is 50dPas-300dPas.
Further, the glass powder selects Bi-Si-B-Zn, Bi-Si-Al-Mg-Zn, P-Zn-Sn or B-Zn-V body System.
Further, the preparation method of the vehicle glass de-fog electrocondution slurry, specifically includes the following steps:
Step 1) mixes carbon series conductive phase, metal and metal conductive oxide uniformly, and moisture removal is removed in drying;Then It is put into grinding device and grinds repeatedly, glass powder is added, continue milled processed, obtain composite powder;
Organic binder is added in the composite powder in step 2), stirs evenly, mixture is ultrasonically treated, and is obtained To composite diffusion object;
The composite diffusion object is heated to 35~40 DEG C by step 3), is dispersed with stirring uniformly, is obtained vehicle glass de-fog Electrocondution slurry.
By the above-mentioned glass de-fog electrocondution slurry modulated, the mode being electrostatically sprayed spray on the glass substrate, to 10-20min is dried after its levelling in 100-150 DEG C of thermostatic drying chamber, it is cured to form the electric heating layer, then again in ladder It is sintered in degree furnace, forms conductive film.
Further, the condition of the step 2) ultrasonic treatment are as follows: supersonic frequency is 5~20kHz, peak power output For 2000W, ultrasonic treatment time 30-50min.Keep the dispersibility of conductive phase in electrocondution slurry more preferable using ultrasonic treatment, Be conducive to improve conductive phase.
Electrostatic spraying of the present invention is a kind of spraying technology according to electrostatic field to the action principle of charge, is being carried out Anode connection is generallyd use in spraying to be sprayed-on on substrate and be grounded, and cathode high pressure connects electrostatic gun, muzzle is equipped with tip Spray point, when voltage is sufficiently high, electric discharge needle-discharging makes the air of spray gun near zone generate strong corona, forms gas ion Region, coating is pumped to the atomization of electrostatic gun mouth by compressed air when spraying, forms coating particle, and pass through ion range band Charge, electrically charged coating particle can be broken into smaller droplet under the action of electric field, fly to anode rapidly, equably adsorb On by the surface of painting substrate, smooth, uniform, smooth, plentiful coating is formed.
The present invention has the advantage that the present invention by the way of electrostatic spraying, can solve traditional silver powder in screen printing The existing caused dispersibility of silver powder reunion is poor during brush prepares electrocondution slurry, to reduce the defect of electric conductivity.Using Electrostatic absorption principle can reduce nano-silver powder and reunite, and equably be adsorbed on by the surface of painting glass, heated solidification shape At smooth, uniform, smooth coating, realize no pollution to the environment, curing time is short, and adhesive force is strong, presentation quality is excellent, at This is low, provides better electric conductivity.
Specific embodiment
In order to which the preparation method to vehicle glass de-fog electrocondution slurry of the present invention carries out further illustrating explanation, application People illustrates following several embodiments, and in no specified otherwise, and the percentage in the present invention is mass percent.
Embodiment 1
(1) vehicle glass de-fog electrocondution slurry is prepared, for use;The electrocondution slurry is by mass percentage by following raw material Composition: carbon system powder 10%, metal and metal oxide powder 75%, organic binder 10%, glass powder 5%, and the metal And the component of metal oxide powder is as follows: Ag 80-90wt%, Pd 5-10wt%, RuO25-10wt%, above-mentioned each group sub-prime Measuring percentage summation is 100%;Carbon system powder uses graphene;
(2) it uses electrostatic painting process to spray above-mentioned resulting coating to remove on vehicle glass surface to form vehicle glass Mist line electrocondution slurry dope layer;Wherein, electrostatic painting process parameter are as follows: spray voltage 60kV, 10 μ A of electric current, velocity pressure 0.3MPa, spray time 20 seconds, 30 ㎜ of spray gun reciprocating speed/second, spray flow 2cc/ second, 20 μm of dusty spray, gun slot and Workpiece distance 100mm, then solidifies, is sintered, obtain dope layer by 70 ° of spray angle, wherein cured baking time 20min, dries Roasting 100 degree of temperature.
Embodiment 2
Vehicle glass de-fog electrocondution slurry is prepared, for use;Electrocondution slurry formula is the same as embodiment 1;
Electrostatic painting process is used to spray above-mentioned resulting coating on vehicle glass surface to form vehicle glass demisting Line electrocondution slurry dope layer;Wherein, electrostatic painting process parameter are as follows: spray voltage 75kV, electric current 15uA, velocity pressure 0.4MPa, spray time 35 seconds, 45 ㎜ of spray gun reciprocating speed/second, spray flow 4cc/ second, 100 μm of dusty spray, gun slot and Workpiece distance 125mm, then solidifies, is sintered, obtain dope layer by 80 ° of spray angle, wherein cured baking time 35min, dries Roasting 130 degree of temperature.
Embodiment 3
Vehicle glass de-fog electrocondution slurry is prepared, for use;Electrocondution slurry formula is the same as embodiment 1;
Electrostatic painting process is used to spray above-mentioned resulting coating on vehicle glass surface to form vehicle glass demisting Line electrocondution slurry dope layer;Wherein, electrostatic painting process parameter are as follows: spray voltage 90kV, electric current 20uA, velocity pressure 0.45MPa, spray time 50 seconds, 60 ㎜ of spray gun reciprocating speed/second, spraying flow 5cc/ seconds, 200 μm of dusty spray, gun slot With workpiece distance 150mm, 90 ° of spray angle, then solidifies, is sintered, obtain dope layer, wherein cured baking time 50min, 150 degree of baking temperature.
In order to verify the performance of vehicle glass de-fog electrocondution slurry dope layer made from preparation method of the present invention, to above-mentioned Dope layer in each embodiment carries out durability performance test, and the results are shown in Table 1.
Comparative example
The vehicle glass de-fog electrocondution slurry of embodiment 1 is printed onto the table of glass using prior art (silk-screen printing) Then face solidifies, is sintered.The performance of obtained dope layer is as shown in table 1.
Table 1 is using the present invention and the performance of the conductive film of prior art preparation
As known from Table 1, the vehicle glass de-fog dope layer that the present invention and prior art obtain, from hardness, adhesive force, side Block resistance, acid resistance are tested for the property comparison in terms of planarization, and vehicle glass demisting film of the invention is uniform, bubble-free, nothing Compactness height is split, there is high rigidity, compactness height, wearability strong, anticorrosive, adhesive force strong, uniform color, low square resistance etc. Feature.
Although specific embodiments of the present invention have been described above, those familiar with the art should be managed Solution, we are merely exemplary described specific embodiment, rather than for the restriction to the scope of the present invention, it is familiar with this The technical staff in field should be covered of the invention according to modification and variation equivalent made by spirit of the invention In scope of the claimed protection.

Claims (8)

1. a kind of production method of antifog glass, including electric heating layer is set on the glass substrate, it is characterised in that: it uses The mode of electrostatic spraying sprays vehicle glass de-fog electrocondution slurry on the glass substrate, cured to form the electric heating layer.
2. the production method of antifog glass according to claim 1, it is characterised in that: the vehicle glass de-fog is conductive Slurry, composed of the following components by mass percentage: carbon series conductive phase 10~15%, metal and metal conductive oxide phase 65~ 80%, organic binder 5%-15%, glass powder 5%-15%, above-mentioned each component mass percent summation are 100%.
3. the production method of antifog glass according to claim 2, it is characterised in that: the metal and metal oxide are led Electric phase, the oxide including following metal and metal: golden Au, palladium Pd, silver Ag, platinum Pt, ruthenium Ru, copper, zinc, barium carbonate, strontium manganate Lanthanum, cobalt strontium lanthanum oxide, partial size 100-200nm;The carbon series conductive mutually includes carbon black, graphite, partial size 100um- 500um。
4. the production method of antifog glass according to claim 2, it is characterised in that: the organic binder is selected from poly- second Glycol, diethylene glycol methyl ether, terpinol, glycol monoethyl ether, ethylene glycol monoethyl ether, N-Methyl pyrrolidone, N-N dimethylacetamide It is amine, Sodium Polyacrylate, polyvinylpyrrolidone, polyphenyl sodium sulfonate, polyimides, low molecule pa resin, acrylic acid modified Alkyd resin, styrenated alkyd, Lauxite;Its viscosity is 50dPas-300dPas.
5. the production method of antifog glass according to claim 2, it is characterised in that: the glass powder selects Bi-Si-B- Zn, Bi-Si-Al-Mg-Zn, P-Zn-Sn or B-Zn-V system.
6. the production method of antifog glass according to claim 1, it is characterised in that: the condition of the electrostatic spraying Are as follows: 60~90kV of spray voltage, 10~20uA of electric current, velocity pressure 0.3-0.45MPa, spray time 20~50 seconds, spray gun was past 30~60 ㎜ of complex velocity/second are sprayed 2~5cc/ of flow seconds, gun slot and workpiece distance 100mm-150mm, and 70 ° of spray angle~ 90°。
7. the production method of antifog glass according to claim 2, it is characterised in that: the vehicle glass de-fog is conductive The preparation method of slurry, specifically includes the following steps:
Step 1) mixes carbon series conductive phase, metal and metal conductive oxide uniformly, and moisture removal is removed in drying;It is then placed in It is ground repeatedly in grinding device, glass powder is added, continued milled processed, obtain composite powder;
Organic binder is added in the composite powder in step 2), stirs evenly, mixture is ultrasonically treated, and is answered Close dispersion;
The composite diffusion object is heated to 35~40 DEG C by step 3), is dispersed with stirring uniformly, and it is conductive to obtain vehicle glass de-fog Slurry.
8. the production method of antifog glass according to claim 7, it is characterised in that: the item of the step 2) ultrasonic treatment Part are as follows: supersonic frequency is 5~20kHz, peak power output 2000W, ultrasonic treatment time 30-50min.
CN201811121218.7A 2018-09-26 2018-09-26 Manufacturing method of demisting glass Expired - Fee Related CN109225780B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109485271A (en) * 2019-01-22 2019-03-19 福建工程学院 Anti-radiation, antistatic, heat-insulated coated glass of one kind and preparation method thereof
CN110232987A (en) * 2019-06-28 2019-09-13 智玻蓝新科技(武汉)有限公司 A kind of dedicated electrocondution slurry of glass base circuit board
CN110381614A (en) * 2019-06-24 2019-10-25 东莞市中科智恒新材料有限公司 Far infrared heating material, the preparation method of far infrared heater and far infrared heater
CN112309606A (en) * 2019-07-31 2021-02-02 湖北中烟工业有限责任公司 Composite metal slurry composition and preparation method and application thereof
CN114749346A (en) * 2022-04-08 2022-07-15 百为智能科技(广州)有限公司 Preparation method based on large-size glass substrate circuit and display device

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101978776A (en) * 2008-03-17 2011-02-16 Lg化学株式会社 Heating element and manufacturing method for same
US20120082806A1 (en) * 2010-10-04 2012-04-05 Kyle Ryan Kissell Heatable coating with nanomaterials
CN103985434A (en) * 2014-05-05 2014-08-13 清华大学深圳研究生院 Manufacturing method of transparent conducting film and transparent conducting film

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101978776A (en) * 2008-03-17 2011-02-16 Lg化学株式会社 Heating element and manufacturing method for same
US20120082806A1 (en) * 2010-10-04 2012-04-05 Kyle Ryan Kissell Heatable coating with nanomaterials
CN103985434A (en) * 2014-05-05 2014-08-13 清华大学深圳研究生院 Manufacturing method of transparent conducting film and transparent conducting film

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109485271A (en) * 2019-01-22 2019-03-19 福建工程学院 Anti-radiation, antistatic, heat-insulated coated glass of one kind and preparation method thereof
CN109485271B (en) * 2019-01-22 2022-02-15 福建工程学院 Anti-radiation, anti-static and heat-insulating coated glass and preparation method thereof
CN110381614A (en) * 2019-06-24 2019-10-25 东莞市中科智恒新材料有限公司 Far infrared heating material, the preparation method of far infrared heater and far infrared heater
CN110381614B (en) * 2019-06-24 2022-02-18 东莞市中科智恒新材料有限公司 Far infrared heating material, preparation method of far infrared heating body and far infrared heating body
CN110232987A (en) * 2019-06-28 2019-09-13 智玻蓝新科技(武汉)有限公司 A kind of dedicated electrocondution slurry of glass base circuit board
CN112309606A (en) * 2019-07-31 2021-02-02 湖北中烟工业有限责任公司 Composite metal slurry composition and preparation method and application thereof
CN114749346A (en) * 2022-04-08 2022-07-15 百为智能科技(广州)有限公司 Preparation method based on large-size glass substrate circuit and display device

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Granted publication date: 20211217