CN109225780B - Manufacturing method of demisting glass - Google Patents

Manufacturing method of demisting glass Download PDF

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Publication number
CN109225780B
CN109225780B CN201811121218.7A CN201811121218A CN109225780B CN 109225780 B CN109225780 B CN 109225780B CN 201811121218 A CN201811121218 A CN 201811121218A CN 109225780 B CN109225780 B CN 109225780B
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glass
spraying
conductive
conductive phase
demisting
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CN109225780A (en
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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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    • 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)
  • Glass Compositions (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

The invention relates to a manufacturing method of demisting glass, which comprises the steps of arranging an electric heating layer on a glass substrate, spraying conductive slurry of a vehicle glass demisting line on the glass substrate in an electrostatic spraying mode, and curing to form the electric heating layer. The invention adopts the electrostatic spraying mode, can solve the defects of poor dispersity and reduced conductivity caused by silver powder agglomeration in the traditional process of preparing the conductive paste by screen printing of silver powder, and ensures that the coating has the characteristics of strong wear resistance, corrosion resistance, strong adhesive force, uniform color and the like by electrostatic spraying. The invention can reduce the agglomeration of the nano silver powder, uniformly adsorb the nano silver powder on the surface of the coated glass, and form a flat, uniform and smooth coating through heating and curing, thereby realizing no pollution to the environment, short curing time, strong adhesive force, excellent appearance quality, low cost and the like, and providing better conductivity.

Description

Manufacturing method of demisting glass
Technical Field
The invention relates to a manufacturing method of demisting glass.
Background
The electronic paste is a high-technology electronic functional material and is mainly used for manufacturing thick film integrated circuits, solar cell electrodes, automobile rear windshield glass and the like. The electronic paste consists of a conductive phase, glass powder and an organic carrier. At present, the conductive phase mainly comprises noble metal and oxide conductive phases thereof: the conductive phase is mainly noble metal such as gold (Au), silver (Ag), palladium (Pd), platinum (Pt), ruthenium (Ru) and the like and oxides thereof, and has the advantages of high temperature resistance, corrosion resistance, water resistance, high insulating strength, high thermal conductivity and the like. And a carbon-based conductive phase: carbon-based materials such as carbon black and graphite, which are low in cost, are mainly used as the conductive phase. Base metal and its oxide conductive phase: mainly uses copper, zinc, barium carbonate, strontium lanthanum manganate, strontium lanthanum cobaltate and the like as conductive phases, and has low price.
The use of heating wires on the rear glass of a vehicle for defrosting fog has become one of the indispensable devices for vehicles. The heating wire of the automobile glass can generate heat after being electrified so as to eliminate frost on the surface of the glass, the automobile glass with the heating wire is widely applied, and the heating wire is almost applied to the rear windshield of all car glass and is mostly used for demisting the driver window in the field of passenger car glass. The heating wire is characterized in that special conductive silver paste is printed on the surface of glass in a screen printing mode, the conductive silver paste is sintered on the surface of the glass after the glass is tempered, and the heating wire can generate heat after being electrified due to certain resistance of the heating wire. The screen printing of the automobile glass heating wire still has a plurality of defects: 1) the nano particles are easy to oxidize, and the bonding force between the particles is weak, so that the wear resistance after sintering is poor; 2) a high-precision patterned silver paste conducting layer is not easy to form, the edge of the conducting layer is not smooth, and a sawtooth shape exists, so that the preparation of a conducting circuit with low resistivity is not facilitated; 3) in order to obtain the low-resistance conductive silver paste, a large amount of silver powder is used in the printing ink, the nano silver powder is easy to agglomerate, and on the other hand, due to the existence of the glass powder, the conductivity of the conductive silver paste is poor, so that the phenomenon of non-uniform demisting is caused.
Disclosure of Invention
The invention aims to solve the technical problem of providing a manufacturing method of demisting glass. The coating with high compactness and smoothness is formed by electrostatic spraying, so that the coating has the characteristics of high hardness, good adhesive force, low square resistance and the like.
The invention is realized by the following steps:
the invention provides a manufacturing method of demisting glass, which comprises the steps of arranging an electric heating layer on a glass substrate, spraying conductive slurry of a vehicle glass demisting line on the glass substrate in an electrostatic spraying mode, and curing to form the electric heating layer.
Further, the electrostatic spraying conditions are as follows: the spraying voltage is 60-90 kV, the current is 10-20 uA, the flow rate and pressure are 0.3-0.45MPa, the spraying time is 20-50 seconds, the reciprocating speed of a spray gun is 30-60 mm/second, the spraying flow is 2-5 cc/second, the distance between the mouth of the spray gun and a workpiece is 100-150 mm, and the spraying angle is 70-90 degrees. The electrostatic spraying is characterized in that the positive electrode is connected with a substrate to be sprayed and grounded, the negative electrode is connected with an electrostatic spray gun at high voltage, a gun nozzle and the substrate to be sprayed form a strong electric field area, the conductive slurry powder is sucked to the nozzle of the electrostatic spray gun to be atomized by compressed air during spraying, rapidly flies to the positive electrode under the action of an electric field and is uniformly adsorbed on the surface of the substrate to be coated, and an electric heating layer is formed by heating and curing, and the surface of the coating is smooth, flat, uniform, bubble-free and crack-free.
Further, the conductive paste for the vehicle glass demisting line comprises the following components in percentage by mass: 10-15% of carbon-based conductive phase, 65-80% of metal and metal oxide conductive phase, 5-15% of organic binder and 5-15% of glass powder, wherein the sum of the mass percentages of the components is 100%.
Further, the metal and metal oxide conductive phase comprises the following metals and metal oxides: gold Au, silver Ag, palladium Pd, platinum Pt, ruthenium Ru, copper, zinc, barium carbonate, lanthanum strontium manganate and lanthanum strontium cobaltate, wherein the particle size is 100-200 nm; the carbon conductive phase comprises carbon black and graphite, and the particle size of the carbon conductive phase is 100-500 um.
Still further, the organic binder is selected from the group consisting of polyethylene glycol, diethylene glycol methyl ether, terpineol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, N-methylpyrrolidone, N-N dimethylacetamide, sodium polyacrylate, polyvinylpyrrolidone, sodium polysulfonate, polyimide, low molecular polyamide resin, acrylic acid-modified alkyd resin, styrene-modified alkyd resin, urea resin; the viscosity is 50 dPas-300 dPas.
Furthermore, the glass powder is selected from a Bi-Si-B-Zn system, a Bi-Si-Al-Mg-Zn system, a P-Zn-Sn system or a B-Zn-V system.
Furthermore, the preparation method of the conductive paste for the vehicle glass demisting line comprises the following steps:
step 1), uniformly mixing a carbon conductive phase, a metal conductive phase and a metal oxide conductive phase, and drying to remove moisture; then, repeatedly grinding the mixture in a grinding device, adding glass powder, and continuously grinding the mixture to obtain composite powder;
step 2), adding an organic binder into the composite powder, uniformly stirring, and carrying out ultrasonic treatment on the mixture to obtain a composite dispersion;
and 3) heating the composite dispersion to 35-40 ℃, and uniformly stirring and dispersing to obtain the conductive slurry for the vehicle glass demisting line.
And spraying the prepared glass defogging line conductive paste on a glass substrate in an electrostatic spraying manner, drying the glass substrate in a constant-temperature drying box at the temperature of 100-150 ℃ for 10-20min after the glass substrate is leveled, curing to form the electric heating layer, and sintering in a gradient furnace to form the conductive film.
Further, the ultrasonic treatment conditions in step 2) are as follows: the ultrasonic frequency is 5-20 kHz, the maximum output power is 2000W, and the ultrasonic treatment time is 30-50 min. The ultrasonic treatment is adopted to ensure that the dispersibility of the conductive phase in the conductive slurry is better, which is beneficial to improving the conductive phase.
The electrostatic spraying is a spraying technology based on the action principle of electrostatic field on electric charge, in the course of spraying, it usually adopts positive electrode connected to the substrate to be sprayed and grounded, and negative electrode connected with electrostatic spray gun at high voltage, and its gun mouth is equipped with tip discharge needle, when the voltage is high enough, the discharge needle can discharge to make the air near the spray gun produce strong corona to form gas ion region, and when the coating is sprayed, the compressed air can be used for sucking coating material into the nozzle of electrostatic spray gun and atomizing to form coating material particles, and the coating material particles can be charged by means of ion region, and under the action of electric field the charged coating material particles can be broken into smaller fog drops, and quickly flying toward positive electrode, and can be uniformly adsorbed on the surface of the substrate to be coated so as to form flat, uniform, smooth and full coating layer.
The invention has the following advantages: the invention adopts an electrostatic spraying mode, and can solve the defects of poor dispersibility and reduced conductivity caused by silver powder agglomeration in the traditional process of preparing the conductive paste by screen printing of silver powder. By adopting the electrostatic adsorption principle, the nano silver powder can be reduced to agglomerate and be uniformly adsorbed on the surface of the coated glass, and a flat, uniform and smooth coating is formed by heating and curing, so that the nano silver powder coating has the advantages of no environmental pollution, short curing time, strong adhesive force, excellent appearance quality, low cost and the like, and provides better conductivity.
Detailed Description
In order to further illustrate the preparation method of the conductive paste for a defogging line of a vehicle glass according to the present invention, the applicant exemplifies several examples as follows, and the percentages in the present invention are percentages by mass without specific description.
Example 1
(1) Preparing conductive slurry for the vehicle glass demisting line for later use; the conductive slurry is prepared from the following raw materials in percentage by mass: 10% of carbon powder, 75% of metal and metal oxide powder, 10% of organic binder and 5% of glass powder, wherein the metal and metal oxide powder comprises the following components: 80-90 wt% of Ag, 5-10 wt% of Pd, and RuO25-10 wt%, wherein the sum of the mass percentages of the components is 100%; the carbon-series powder adopts graphene;
(2) spraying the obtained paint on the surface of the vehicle glass by adopting an electrostatic spraying process to form a conductive paste paint layer of the vehicle glass demisting line; wherein, the electrostatic spraying process parameters are as follows: spraying voltage of 60kV, current of 10 mu A, flow rate and pressure of 0.3MPa, spraying time of 20 seconds, reciprocating speed of a spray gun of 30 mm/second, spraying flow of 2 cc/second, spraying powder of 20 mu m, distance between a spray gun opening and a workpiece of 100mm, and spraying angle of 70 degrees, and then curing and sintering to obtain a coating layer, wherein the curing baking time is 20min, and the baking temperature is 100 ℃.
Example 2
Preparing conductive slurry for the vehicle glass demisting line for later use; the formulation of the conductive paste was the same as in example 1;
spraying the obtained paint on the surface of the vehicle glass by adopting an electrostatic spraying process to form a conductive paste paint layer of the vehicle glass demisting line; wherein, the electrostatic spraying process parameters are as follows: the spraying voltage is 75kV, the current is 15uA, the flow rate and pressure are 0.4MPa, the spraying time is 35 seconds, the reciprocating speed of a spray gun is 45 mm/second, the spraying flow is 4 cc/second, the spraying powder is 100 micrometers, the distance between a spray gun opening and a workpiece is 125mm, the spraying angle is 80 degrees, then the curing and sintering are carried out, and a coating layer is obtained, wherein the curing baking time is 35min, and the baking temperature is 130 degrees.
Example 3
Preparing conductive slurry for the vehicle glass demisting line for later use; the formulation of the conductive paste was the same as in example 1;
spraying the obtained paint on the surface of the vehicle glass by adopting an electrostatic spraying process to form a conductive paste paint layer of the vehicle glass demisting line; wherein, the electrostatic spraying process parameters are as follows: spraying voltage of 90kV, current of 20uA, flow rate and pressure of 0.45MPa, spraying time of 50 seconds, reciprocating speed of a spray gun of 60 mm/second, spraying flow of 5 cc/second, spraying powder of 200 mu m, distance between a spray gun opening and a workpiece of 150mm, and spraying angle of 90 degrees, and then curing and sintering to obtain a coating layer, wherein the curing baking time is 50min, and the baking temperature is 150 degrees.
In order to verify the performance of the conductive paste coating layer for the vehicle glass demisting line prepared by the preparation method of the invention, the coating layer in each example was subjected to a performance test, and the results are shown in table 1.
Comparative examples
The conductive paste for the automotive glass defogging line in the example 1 is printed on the surface of glass by adopting the prior art (screen printing), and then is cured and sintered. The properties of the resulting coating layer are shown in table 1.
TABLE 1 Properties of conductive films prepared using the present invention and prior art processes
Figure BDA0001811249820000051
Figure BDA0001811249820000061
As can be seen from Table 1, compared with the automotive glass demisting line coating layer obtained by the prior art, the automotive glass demisting line coating layer is subjected to performance test comparison in the aspects of hardness, adhesive force, square resistance, acid resistance and flatness, and the automotive glass demisting film has the characteristics of uniformity, no bubbles, no cracks, high compactness, high hardness, high compactness, strong wear resistance, corrosion resistance, strong adhesive force, uniform color, low square resistance and the like.
Although specific embodiments of the invention have been described above, it will be understood by those skilled in the art that the specific embodiments described are illustrative only and are not limiting upon the scope of the invention, and that equivalent modifications and variations can be made by those skilled in the art without departing from the spirit of the invention, which is to be limited only by the appended claims.

Claims (5)

1. The manufacturing method of the defogging glass comprises the steps of arranging the electric heating layer on the glass substrate, and is characterized in that: spraying conductive slurry of the glass demisting line for the vehicle on the glass substrate in an electrostatic spraying mode, and forming the electric heating layer after curing;
the conductive paste for the automobile glass demisting line comprises the following components in percentage by mass: 10-15% of carbon-based conductive phase, 65-80% of metal and metal oxide conductive phase, 5-15% of organic binder and 5-15% of glass powder, wherein the sum of the mass percentages of the components is 100%;
the metal and metal oxide conductive phase comprises the following metals and metal oxides: gold Au, palladium Pd, silver Ag, platinum Pt, ruthenium Ru, copper, zinc, barium carbonate, lanthanum strontium manganate and lanthanum strontium cobaltate, the particle size of which is 100-200 nm; the carbon conductive phase comprises carbon black and graphite, and the particle size of the carbon conductive phase is 100-500 um;
the electrostatic spraying conditions are as follows: the spraying voltage is 60-90 kV, the current is 10-20 uA, the flow rate and pressure are 0.3-0.45MPa, the spraying time is 20-50 seconds, the reciprocating speed of a spray gun is 30-60 mm/second, the spraying flow is 2-5 cc/second, the distance between the mouth of the spray gun and a workpiece is 100-150 mm, and the spraying angle is 70-90 degrees.
2. A method of manufacturing a defogging glass according to claim 1, wherein: the organic binder is selected from polyethylene glycol, sodium polyacrylate, polyvinylpyrrolidone, sodium polystyrene sulfonate, polyimide, low molecular polyamide resin, acrylic acid modified alkyd resin, styrene modified alkyd resin and urea resin; the viscosity is 50 dPas-300 dPas.
3. A method of manufacturing a defogging glass according to claim 1, wherein: the glass powder is Bi-Si-B-Zn, Bi-Si-Al-Mg-Zn, P-Zn-Sn or B-Zn-V system.
4. A method of manufacturing a defogging glass according to claim 1, wherein: the preparation method of the conductive paste for the vehicle glass demisting line comprises the following steps:
step 1), uniformly mixing a carbon conductive phase, a metal conductive phase and a metal oxide conductive phase, and drying to remove moisture; then, repeatedly grinding the mixture in a grinding device, adding glass powder, and continuously grinding the mixture to obtain composite powder;
step 2), adding an organic binder into the composite powder, uniformly stirring, and carrying out ultrasonic treatment on the mixture to obtain a composite dispersion;
and 3) heating the composite dispersion to 35-40 ℃, and uniformly stirring and dispersing to obtain the conductive slurry for the vehicle glass demisting line.
5. The method for producing a defogging glass according to claim 4, wherein: the ultrasonic treatment conditions in the step 2) are as follows: the ultrasonic frequency is 5-20 kHz, the maximum output power is 2000W, and the ultrasonic treatment time is 30-50 min.
CN201811121218.7A 2018-09-26 2018-09-26 Manufacturing method of demisting glass Expired - Fee Related CN109225780B (en)

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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
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
CN110232987B (en) * 2019-06-28 2020-03-31 智玻蓝新科技(武汉)有限公司 Special conductive paste for glass-based 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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