CN107056066A - A kind of preparation method of crystallite thick film dielectric coating - Google Patents

A kind of preparation method of crystallite thick film dielectric coating Download PDF

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Publication number
CN107056066A
CN107056066A CN201611172313.0A CN201611172313A CN107056066A CN 107056066 A CN107056066 A CN 107056066A CN 201611172313 A CN201611172313 A CN 201611172313A CN 107056066 A CN107056066 A CN 107056066A
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powder
crystallite
thick film
film dielectric
metal base
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颜宏志
张源锋
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/20Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23DENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
    • C23D5/00Coating with enamels or vitreous layers
    • C23D5/04Coating with enamels or vitreous layers by dry methods

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a kind of preparation method of crystallite thick film dielectric coating, this method is into molten condition first by inorganic oxide high melt;Then melt is fabricated to devitrified glass disintegrating slag by water quenching;Then devitrified glass most ground-slag is broken into by powder, and admixed with additives in the powder by pulverizer, is sufficiently stirred for obtaining micro-crystalline ceramic powder;Followed by by the micro-crystalline ceramic powder coating of making in metallic substrate surface by the way of electrostatic powder coating;Finally, metal base is sintered, so as to make formation crystallite thick film dielectric coating on metal base.Powder spray on the surface of metal base, while can adjust the coating layer thickness in metallic substrate surface according to the size of regulation electrostatic, once can just be completed coating operations, substantially increase production efficiency by the mode that the present invention is sprayed using electrostatic ceramic.Meanwhile, the present invention is not after adopting the above technical scheme, because it is by the way of electrostatic spraying, having any limitation to the moulding of metal base, going on the metal base of different shaping.

Description

A kind of preparation method of crystallite thick film dielectric coating
Technical field
The present invention relates to the preparation method technical field of coating for metal surfaces, and in particular to a kind of crystallite thick film dielectric coating Preparation method.
Background technology
In order to prevent the corrosion and oxidation of metal material, it will usually be coated with dielectric coated in metallic surface.Dielectric coated Used material has a lot, and du pont company develops a kind of crystallite thick film dielectric coating, and its micro-crystalline ceramic used is made For dielectric coated, the corrosion and oxidation of metal material not only can be effectively prevented, and it has higher hardness, can be to metal Surface forms good protective layer, while the texture of metal material can also be improved.The making of this crystallite thick film dielectric coating Method is as follows:
1st, by a variety of different metal oxides materials (being used for the raw material for making glass ceramics such as calcium oxide, aluminum oxide) Mixed sintering, and after water quenching, being crushed to 1000-1500 mesh, that powder stock is made is standby.
2nd, it is mixed into using terpinol, ATBC, ethyl cellulose, 1-4 butyrolactone, rilanit special organic molten Agent.
3rd, by powder stock with mailing solvent using weight ratio as:75%:The mixing of 25% ratio is mixed thoroughly, is then ground with three rods Machine is fully pressed, and slurry is made.
4th, by way of screen printing, by slurry coating on a metal plate, then again with 850 degree of high temperature sinterings.
Due to by way of screen printing, the thickness only 20um thickness per secondary coating.And the dielectric coated typically required Need to reach the standard of 100um thickness, so using the above method, screen printing coating operations must be just repeated 5 times, and it is each Screen printing coating operations will take a substantial amount of time, and cause production efficiency low.In addition, this crystallite thick film dielectric coating Preparation method there is another problem that it carries out material coating by the mode for then passing through screen printing, so it is only Flat metal material is only used for, is that can not use this kind of method for some curved surfaces or irregular metal product It is coated.Finally, at present in this preparation method, used slurry, the profit after organic solvent volatilization in presswork With rate only 75%, unnecessary waste and environmental problem are caused.
For problem above, the present inventor proposes solution below by continuous research..
The content of the invention
The technical problems to be solved by the invention, which are that, overcomes the preparation method of existing crystallite thick film dielectric coating not Foot is simple there is provided a kind of technique, and the preparation method of the crystallite thick film dielectric coating of efficiency high.
In order to solve the above technical problems, present invention employs following technical scheme:The making of the crystallite thick film dielectric coating Method is into molten condition first by inorganic oxide high melt;Then melt is fabricated to devitrified glass by water quenching broken Slag;Then devitrified glass most ground-slag is broken into by powder, and admixed with additives in the powder by pulverizer, is sufficiently stirred for obtaining micro- Brilliant ceramic powders;Followed by by the micro-crystalline ceramic powder coating of making in metal base table by the way of electrostatic powder coating Face;Finally, metal base is sintered, so as to make formation crystallite thick film dielectric coating on metal base.
Furthermore, in above-mentioned technical proposal, specifically, this method comprises the following steps:The first step, by inorganic oxide Thing is put into smelting furnace and heated, and is smelted into molten condition;Second step, will be heated into the melt of molten condition by way of water quenching It is fabricated to devitrified glass disintegrating slag;3rd step, obtained devitrified glass disintegrating slag is put into airslide disintegrating mill and is ground into powder, powder Granularity in 300-800 mesh;4th step, adulterate organic additive in the powder, and the weight ratio of the additive and powder is: 0.1-3%, and make additive be sufficiently mixed uniformly with powder by mixer;5th step, by the way of electrostatic powder coating By the micro-crystalline ceramic powder coating of making in metallic substrate surface, the thickness of application is not less than 100 microns, and by adjusting electrostatic Voltage adjusts the application thickness of micro-crystalline ceramic powder, and the 6th step burnt the metal base for being coated with micro-crystalline ceramic powder Knot, so as to make formation crystallite thick film dielectric coating on metal base.
Furthermore, in above-mentioned technical proposal, the expansion ratio of the crystallite thick film dielectric coating and metal base it is swollen Swollen ratio correspondence.
Furthermore, in above-mentioned technical proposal, inorganic oxides different according to the coefficient of expansion of metal base, described Using following different scheme:Scheme one uses calcium based material for primary raw material, i.e., using calcium oxide as main raw material, and Other inorganic oxides are added, the weight accounting of wherein calcium oxide is:35-50%;Scheme two uses barium based material to be main former Material, i.e., using barium monoxide as main raw material, and add other inorganic oxides, the weight accounting of wherein barium monoxide is:40- 60%;
Furthermore, in above-mentioned technical proposal, in described scheme one, the part by weight of various composition is in raw material: Calcium oxide 40-50%, silica 1 5-30%, titanium dioxide 5-15%, aluminum oxide 5-10%, boron oxide 5-10%, cobalt oxide 2-5%, zirconium oxide 2-5%.
Furthermore, in above-mentioned technical proposal, in described scheme two, the part by weight of various composition is oxygen in raw material Change barium 45-60%, silica 1 0-25%, titanium dioxide 5-15%, aluminum oxide 2-10%, boron oxide 3-10%, cobalt oxide 2- 5%th, zirconium oxide 2-5%.
Furthermore, in above-mentioned technical proposal, described additive is:Water-soluble organic cellulose.
Furthermore, in above-mentioned technical proposal, described sintering temperature is 750-900 degrees Celsius, and the time is:5-30 points Clock.
The present invention after adopting the above technical scheme, the mode sprayed using electrostatic ceramic by powder spray in metal base Surface, while can adjust the coating layer thickness in metallic substrate surface according to the size of regulation electrostatic, once can just complete to apply Cloth operation, is finally sintered.Meanwhile, the present invention is after adopting the above technical scheme, the side for using electrostatic spraying due to it Formula, does not have any limitation to the moulding of metal base, goes on the metal base of different shaping, including:Curved surface and The metal base of irregular moulding.
Embodiment
Embodiment 1:
The present embodiment 1 is to use calcium based material for primary raw material, i.e., using calcium oxide as main raw material, and add it His inorganic oxide, the weight accounting of wherein calcium oxide is:35-50%.Its concrete scheme is as follows:
The first step, inorganic oxide is put into smelting furnace and heated, molten condition is smelted into.It is inorganic that the present embodiment is used Oxide raw material is as follows:The part by weight of various composition is in raw material:Calcium oxide 40-50%, silica 1 5-30%, dioxy Change titanium 5-15%, aluminum oxide 5-10%, boron oxide 5-10%, cobalt oxide 2-5%, zirconium oxide 2-5%.It is preferred that:Calcium oxide 45%, Silica 25%, aluminum oxide 8%, boron oxide 8%, cobalt oxide 3%, zirconium oxide 5%, titanium dioxide 6%.
Second step, devitrified glass disintegrating slag is fabricated to by the melt for being heated into molten condition by way of water quenching.
3rd step, obtained devitrified glass disintegrating slag is put into airslide disintegrating mill and is ground into powder, the granularity of powder exists 300-800 mesh;
4th step, adulterate organic additive in the powder, and the weight ratio of the additive and powder is:0.1-3%, and pass through Mixer makes additive be sufficiently mixed uniformly with powder;Described additive is:Water-soluble organic cellulose, for example:Methyl is fine Dimension element, propyl cellulose, or alkoxide organic material.These can reinforcing material electrostatic produce, be easy to follow-up electrostatic Apply, and will not can in the coating be remained completely by high-temperature gasification and cause stomata in subsequent high temperature sintering process.
5th step, by the micro-crystalline ceramic powder coating of making in metallic substrate surface by the way of electrostatic powder coating, The thickness of application is not less than 100 microns.It is quiet to metal base generation 60000v-12 0000v high pressure machine to be produced using electrostatic Electricity, micro-crystalline ceramic powder spray is in workpiece.By with electrostatic pressure adjustment attachment ceramic powder thickness.
6th step, the metal base for being coated with micro-crystalline ceramic powder is sintered, and forms micro- on metal base so as to make Brilliant thick film dielectric coating.Described sintering temperature is 750-900 degrees Celsius, and the time is:5-30 minutes.
Because the metal base coefficient of expansion of different materials is different, so needing selection for the metal base of different materials Different inorganic oxide raw materials.So as to make the last coefficient of expansion for sintering the dielectric coated formed and the expansion system of metal base Number is consistent, it is ensured that the situation that dielectric coated will not be cracked during subsequent use.
The invention provides two schemes, the scheme one used in above-described embodiment 1.
Scheme one uses calcium based material for primary raw material, i.e., using calcium oxide as main raw material, and adds other nothings The weight accounting of machine oxide, wherein calcium oxide is:35-50%.The applicable coefficient of expansion of scheme one is:11x10-6The gold of left and right Belong to material, for example:Stainless steel (SUS430).
Scheme two uses barium based material for primary raw material, i.e., using barium monoxide as main raw material, and adds other nothings The weight accounting of machine oxide, wherein barium monoxide is:40-60%.The applicable coefficient of expansion of scheme two is:18x10-6The gold of left and right Belong to material, for example:Stainless steel (SUS304).
Embodiment 2:
Embodiment 2 employs such scheme two as inorganic oxide raw material.It is specific as follows:
The first step, inorganic oxide is put into smelting furnace and heated, molten condition is smelted into.It is inorganic that the present embodiment is used Oxide raw material is as follows:The part by weight of various composition is barium monoxide 45-60%, silica 1 0-25%, titanium dioxide in raw material Titanium 5-15%, aluminum oxide 2-10%, boron oxide 3-10%, cobalt oxide 2-5%, zirconium oxide 2-5%.Preferential oxidation barium 50%, two Silica 20%, aluminum oxide 8%, boron oxide 8%, cobalt oxide 3%, zirconium oxide 3%, titanium dioxide 8%
Second step, devitrified glass disintegrating slag is fabricated to by the melt for being heated into molten condition by way of water quenching.
3rd step, obtained devitrified glass disintegrating slag is put into airslide disintegrating mill and is ground into powder, the granularity of powder exists Below 300-800 mesh;
4th step, adulterate organic additive in the powder, and the weight ratio of the additive and powder is:0.1-3%, and pass through Mixer makes additive be sufficiently mixed uniformly with powder;Described additive is:Water-soluble organic cellulose, for example:Methyl is fine Dimension element, propyl cellulose, or alkoxide organic material.
5th step, by the micro-crystalline ceramic powder coating of making in metallic substrate surface by the way of electrostatic powder coating, The thickness of application is not less than 100 microns.It is quiet to metal base generation 60000v-120000v high pressure machine to be produced using electrostatic Electricity, micro-crystalline ceramic powder spray is in workpiece.By with electrostatic pressure adjustment attachment ceramic powder thickness.
6th step, the metal base for being coated with micro-crystalline ceramic powder is sintered, and forms micro- on metal base so as to make Brilliant thick film dielectric coating.Described sintering temperature is 750-900 degrees Celsius, and the time is:5-30 minutes.
Entered test, crystallite thick film dielectric coating uniformity and adhesive force are obtained substantially due to traditional handicraft using this method Making coating, and efficiency improve more than 4 times.Simultaneously as it is by the way of electrostatic spraying, metal base is made Type does not have any limitation, goes on the metal base of different shaping, including:Curved surface and the Metal Substrate of irregular moulding Material.Finally, the present invention uses electrostatic spraying, so additive amount is few, it is to avoid wastes and volatilizees.
Certainly, the foregoing is only the specific embodiment of the present invention, not limit the scope of the present invention, it is all according to The equivalent change or modification that construction, feature and principle described in scope of the present invention patent are done, all should be included in Shen of the present invention Please be in the scope of the claims.

Claims (8)

1. a kind of preparation method of crystallite thick film dielectric coating, it is characterised in that:This method is by inorganic oxide high temperature first It is smelted into molten condition;Then melt is fabricated to devitrified glass disintegrating slag by water quenching;Then by pulverizer by devitrified glass Most ground-slag is broken into powder, and admixed with additives in the powder, is sufficiently stirred for obtaining micro-crystalline ceramic powder;Followed by using electrostatic The mode of powder coating is by the micro-crystalline ceramic powder coating of making in metallic substrate surface;Finally, metal base is sintered, So as to make formation crystallite thick film dielectric coating on metal base.
2. a kind of preparation method of crystallite thick film dielectric coating according to claim 1, it is characterised in that:This method includes Following steps:
The first step, inorganic oxide is put into smelting furnace and heated, molten condition is smelted into;
Second step, devitrified glass disintegrating slag is fabricated to by the melt for being heated into molten condition by way of water quenching;
3rd step, obtained devitrified glass disintegrating slag is put into airslide disintegrating mill and is ground into powder, the granularity of powder is in 300- 800 mesh;
4th step, adulterate organic additive in the powder, and the weight ratio of the additive and powder is:0.1-3%, and pass through stirring Machine makes additive be sufficiently mixed uniformly with powder;
5th step, by the micro-crystalline ceramic powder coating of making in metallic substrate surface, application by the way of electrostatic powder coating Thickness be not less than 100 microns, and adjust by adjusting electrostatic potential the application thickness of micro-crystalline ceramic powder,
6th step, the metal base for being coated with micro-crystalline ceramic powder is sintered, and crystallite thickness is formed on metal base so as to make Film medium coating.
3. a kind of preparation method of crystallite thick film dielectric coating according to claim 1 or 2, it is characterised in that:It is described micro- The coefficient of expansion of brilliant thick film dielectric coating is matched with the coefficient of expansion of metal base.
4. a kind of preparation method of crystallite thick film dielectric coating according to claim 3, it is characterised in that:According to Metal Substrate The coefficient of expansion of material is different, and described inorganic oxide uses following different scheme:
Scheme one uses calcium based material for primary raw material, i.e., using calcium oxide as main raw material, and adds other inorganic oxygen The weight accounting of compound, wherein calcium oxide is:35-50%;
Scheme two uses barium based material for primary raw material, i.e., using barium monoxide as main raw material, and adds other inorganic oxygen The weight accounting of compound, wherein barium monoxide is:40-60%.
5. a kind of preparation method of crystallite thick film dielectric coating according to claim 4, it is characterised in that:Described scheme In one, the part by weight of various composition is in raw material:Calcium oxide 40-50%, silica 1 5-30%, titanium dioxide 5-15%, Aluminum oxide 5-10%, boron oxide 5-10%, cobalt oxide 2-5%, zirconium oxide 2-5%.
6. a kind of preparation method of crystallite thick film dielectric coating according to claim 4, it is characterised in that:Described scheme In two, in raw material the part by weight of various composition be barium monoxide 45-60%, silica 1 0-25%, titanium dioxide 5-15%, Aluminum oxide 2-10%, boron oxide 3-10%, cobalt oxide 2-5%, zirconium oxide 2-5%.
7. a kind of preparation method of crystallite thick film dielectric coating according to claim 2, it is characterised in that:Described addition Agent is:Water-soluble organic cellulose.
8. a kind of preparation method of crystallite thick film dielectric coating according to claim 2, it is characterised in that:Described sintering Temperature is 750-900 degrees Celsius, and the time is:5-30 minutes.
CN201611172313.0A 2016-12-17 2016-12-17 A kind of preparation method of crystallite thick film dielectric coating Pending CN107056066A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111499389A (en) * 2020-05-11 2020-08-07 陕西长石电子材料股份有限公司 Preparation method of ceramic powder for metal-based ceramic copper-clad plate

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JPS56106971A (en) * 1980-01-28 1981-08-25 Nippon Furitsuto Kk Frit composition for electrostatic coating, and preparation of enameled ware
CN2603735Y (en) * 2002-12-12 2004-02-18 武汉理工大学 Metal sheet coating with crystallite glass
CN105176103A (en) * 2015-06-17 2015-12-23 宁波职业技术学院 Thick film circuit insulating dielectric slurry for aluminum substrates, and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS56106971A (en) * 1980-01-28 1981-08-25 Nippon Furitsuto Kk Frit composition for electrostatic coating, and preparation of enameled ware
CN2603735Y (en) * 2002-12-12 2004-02-18 武汉理工大学 Metal sheet coating with crystallite glass
CN105176103A (en) * 2015-06-17 2015-12-23 宁波职业技术学院 Thick film circuit insulating dielectric slurry for aluminum substrates, and preparation method thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111499389A (en) * 2020-05-11 2020-08-07 陕西长石电子材料股份有限公司 Preparation method of ceramic powder for metal-based ceramic copper-clad plate

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Application publication date: 20170818