CN104402226A - Zirconium based high temperature resistant composite ceramic coating preparation method - Google Patents
Zirconium based high temperature resistant composite ceramic coating preparation method Download PDFInfo
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- CN104402226A CN104402226A CN201410609096.1A CN201410609096A CN104402226A CN 104402226 A CN104402226 A CN 104402226A CN 201410609096 A CN201410609096 A CN 201410609096A CN 104402226 A CN104402226 A CN 104402226A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2207/00—Compositions specially applicable for the manufacture of vitreous enamels
- C03C2207/04—Compositions specially applicable for the manufacture of vitreous enamels for steel
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Abstract
The invention relates to a zirconium based high temperature resistant composite ceramic coating preparation method including modified fluoro silicone solvent preparation, paint powder preparation and preparation of a zirconium based high temperature resistant composite ceramic coating by mixing of the modified fluoro silicone solvent and the paint powder. The beneficial effects of the zirconium based high temperature resistant composite ceramic coating preparation method are that: the process is simple, the prepared zirconium based high temperature resistant composite ceramic coating can form a dense nano ceramic glaze layer, has good impact resistance and wear resistance, can be used for a long term in high temperature environment below 1350 DEG C, and has the characteristics of high temperature resistance, good acid and alkali corrosion resistance, long one-time spraying and use cycle, no pollution to environment, and the like. The composite ceramic paint can be resistant to general acid and alkaline etching, waterproof and moistureproof, can prevent organic compound corrosion, and has excellent protection effect on parts working in high temperature environment, acid and alkali environment and other perishable environment.
Description
Technical field
The present invention relates to technical field of coatings, is a kind of preparation method of zirconium based high-temp-resistant composite ceramics coating specifically.
Background technology
At present, market is sold high temperature resistant paint vehicle and mostly be organic high temperature-resistant paint vehicle, also have small part inorganic high-temperature resistant paint vehicle, all in all, organic high temperature-resistant paint vehicle occupies the market of industry 85%.Mainly use client as heat resistance paint, have also been made investigation in many ways fastidious simultaneously, find the heat resistance paint ubiquity heatproof insufficient strength that existing market exists, the shortcomings such as enamelled coating easily comes off under the high temperature conditions, and solidity to corrosion is poor, and life cycle is short.For the above problem that heat resistance paint exists, through repeatedly probing into, develop zirconium based high-temp-resistant composite ceramics paint vehicle, to solve original paint vehicle Problems existing.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of energy is high temperature resistant, the preparation method of the zirconium based high-temp-resistant composite ceramics coating of acid and alkali-resistance, long service life.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for zirconium based high-temp-resistant composite ceramics coating, comprising:
By elemental silicon and fluorine source by 1: 1 ~ 1: 5 weight ratio be added to the water, heated and stirred reaction 60 ~ 90min, Heating temperature is 90 ~ 100 DEG C, and stir speed (S.S.) is 450 ~ 800 turns/min, obtains modified fluoro-silicone solvent;
By lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide mix after under isolated air or inert atmosphere roasting 110 ~ 120min, maturing temperature is 1720 ~ 1750 DEG C, obtains paint vehicle powder; The blending ratio controlling lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide makes the composition of described paint vehicle powder and content control: lanthanide rare compound 4.5 ~ 6.5wt%, aluminum oxide 21.5 ~ 24.5wt%, silicon carbide 12 ~ 17wt%, all the other are zirconium white and inevitable impurity, and zirconia content is greater than 35wt%;
By described modified fluoro-silicone solvent and paint vehicle powder by 1: 1.15 ~ 1: 1.45 weight ratio mix, obtain zirconium based high-temp-resistant composite ceramics coating;
Wherein, described fluorine source is selected from the one in fluorine gas, hydrogen fluoride, nonmetal fluorochemical and Neutral ammonium fluoride.
Beneficial effect of the present invention is: technical process is simple, obtained zirconium based high-temp-resistant composite ceramics coating can form the nano ceramics glaze paint of one deck densification in high temperature environments, there is stronger wear resistant and impact resistant, can use for a long time in hot environment below 1350 DEG C, have high temperature resistant, acid-alkali-corrosive-resisting good, disposable spray finishing life cycle is long, to features such as environment are nuisanceless.This kind of composite ceramics paint vehicle under the high temperature conditions can resistance to live the etch of general soda acid, waterproof and dampproof, the corrosion of organic compound can be prevented simultaneously, to the parts of various hot environment, acid or alkali environment and other perishable environmental work, there is fabulous provide protection.
Embodiment
By describing technology contents of the present invention in detail, being realized object and effect, be explained below in conjunction with embodiment.
The design of most critical of the present invention is: using silicon-fluorochemical as modification solvent, the powder simultaneously obtained using lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide for raw material high-temperature roasting is as paint vehicle powder, can be obtained by mixed and modified solvent and paint vehicle powder there is stronger wear resistant and impact resistant, high temperature resistant, acid-alkali-corrosive-resisting good, disposable spray finishing life cycle is long, zirconium based high-temp-resistant composite ceramics coating to features such as environment are nuisanceless, technical process is simple.
Concrete, the preparation method of zirconium based high-temp-resistant composite ceramics coating provided by the invention, comprising:
By elemental silicon and fluorine source by 1: 1 ~ 1: 5 weight ratio be added to the water, heated and stirred reaction 60 ~ 90min, Heating temperature is 90 ~ 100 DEG C, and stir speed (S.S.) is 450 ~ 800 turns/min, obtains modified fluoro-silicone solvent;
By lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide mix after under isolated air or inert atmosphere roasting 110 ~ 120min, maturing temperature is 1720 ~ 1750 DEG C, obtains paint vehicle powder; The blending ratio controlling lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide makes the composition of described paint vehicle powder and content control: lanthanide rare compound 4.5 ~ 6.5wt%, aluminum oxide 21.5 ~ 24.5wt%, silicon carbide 12 ~ 17wt%, all the other are zirconium white and inevitable impurity, and zirconia content is greater than 35wt%;
By described modified fluoro-silicone solvent and paint vehicle powder by 1: 1.15 ~ 1: 1.45 weight ratio mix, obtain zirconium based high-temp-resistant composite ceramics coating;
Wherein, described fluorine source is selected from the one in fluorine gas, hydrogen fluoride, nonmetal fluorochemical and Neutral ammonium fluoride.
From foregoing description, beneficial effect of the present invention is: technical process is simple, obtained zirconium based high-temp-resistant composite ceramics coating can form the nano ceramics glaze paint of one deck densification in high temperature environments, there is stronger wear resistant and impact resistant, can use for a long time in hot environment below 1350 DEG C, have high temperature resistant, acid-alkali-corrosive-resisting good, disposable spray finishing life cycle is long, to features such as environment are nuisanceless.This kind of composite ceramics paint vehicle under the high temperature conditions can resistance to live the etch of general soda acid, waterproof and dampproof, the corrosion of organic compound can be prevented simultaneously, to the parts of various hot environment, acid or alkali environment and other perishable environmental work, there is fabulous provide protection.
Further, the mode of described heating is heating in water bath.
Further, described elemental silicon and fluorine source after heated and stirred reaction 60 ~ 90min, then are incubated 100 ~ 120min, then naturally cool to room temperature, obtain modified fluoro-silicone solvent.
Further, in described nanoscale zirconia ceramic, oxidation of impurities iron <0.025wt%, oxidation of impurities titanium <0.06wt%, impurity oxygen SiClx <0.12wt%.
Further, the purity of described alumina in Nano level ceramic is more than 99.8%.
Further, the purity of described lanthanide rare micro mist and silicon carbide is more than 99.5%.
Further, described inert atmosphere is helium, neon or argon atmosphere, is preferably argon atmosphere.
Embodiment 1
1, prepare modified fluoro-silicone solvent: elemental silicon, fluorine gas are evenly slowly added to the water by the weight ratio of 1: 1, heating in water bath is to 90 DEG C, and strong stirring 60min under 450 ~ 800 turns/min, obtains modified fluoro-silicone solvent;
2, prepare paint vehicle powder: by lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide mix after under isolated air ambient roasting 120min, maturing temperature is 1740 DEG C, obtains paint vehicle powder; The blending ratio controlling lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide makes the composition of described paint vehicle powder and content control: lanthanide rare compound 5.5wt%, aluminum oxide 21.5wt%, silicon carbide 12wt%, all the other are zirconium white and some inevitable impurity, and zirconia content is greater than 35wt%.
Oxidation of impurities iron <0.02wt% in described nanoscale zirconia ceramic, oxidation of impurities titanium <0.05wt%, impurity oxygen SiClx <0.05wt%.The purity of alumina in Nano level ceramic is more than 99.8%, and other material purity controls more than 99.5%.
3, batch mixing: by modified fluoro-silicone solvent and paint vehicle powder by 1: 1.15 weight ratio mix, under 450 ~ 800 turns/min after strong stirring 60min, obtain zirconium based high-temp-resistant composite ceramics coating.
Dewater by the zirconium based high-temp-resistant composite ceramics paint spay-coating obtained by aforesaid method through seasoning behind stainless steel cylinder surface, spraying like this 3 times, through High Temperature Furnaces Heating Apparatus under 1350 DEG C of heating, roasting 72 hours under the flue gas condition such as acid, alkaline, zirconium based high-temp-resistant composite ceramics dope layer is observed after naturally cooling, circulation like this does not find that its top layer is damaged for 10 times, high temperature resistant, acid-alkali-corrosive-resisting is good.
Embodiment 2
1, prepare modified fluoro-silicone solvent: the weight ratio of elemental silicon, ammonium acid fluoride 1: 1.35 be evenly slowly added to the water, heating in water bath is to 100 DEG C, and strong stirring 90min under 450 ~ 800 turns/min, obtains modified fluoro-silicone solvent;
2, prepare paint vehicle powder: by lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide mix after under argon atmosphere roasting 115min, maturing temperature is 1720 DEG C, obtains paint vehicle powder; The blending ratio controlling lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide makes the composition of described paint vehicle powder and content control: lanthanide rare compound 4.5wt%, aluminum oxide 22wt%, silicon carbide 13wt%, all the other are zirconium white and some inevitable impurity, and zirconia content is greater than 35wt%.
Oxidation of impurities iron <0.025wt% in described nanoscale zirconia ceramic, oxidation of impurities titanium <0.05wt%, impurity oxygen SiClx <0.05wt%.The purity of alumina in Nano level ceramic is more than 99.8%, and other material purity controls more than 99.5%.
3, batch mixing: by modified fluoro-silicone solvent and paint vehicle powder by 1: 1.25 weight ratio mix, under 450 ~ 800 turns/min after strong stirring 50min, obtain zirconium based high-temp-resistant composite ceramics coating.
Dewater by the zirconium based high-temp-resistant composite ceramics paint spay-coating obtained by aforesaid method through seasoning behind stainless steel cylinder surface, spraying like this 3 times, through High Temperature Furnaces Heating Apparatus under 1350 DEG C of heating, roasting 72 hours under the flue gas condition such as acid, alkaline, zirconium based high-temp-resistant composite ceramics dope layer is observed after naturally cooling, circulation like this does not find that its top layer is damaged for 10 times, high temperature resistant, acid-alkali-corrosive-resisting is good.
Embodiment 3
1, prepare modified fluoro-silicone solvent: elemental silicon, Neutral ammonium fluoride are evenly slowly added to the water by the weight ratio of 1: 5, heating in water bath is to 90 DEG C, and strong stirring 90min under 450 ~ 800 turns/min, obtains modified fluoro-silicone solvent;
2, prepare paint vehicle powder: by lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide mix after under argon shield atmosphere roasting 110min, maturing temperature is 1750 DEG C, obtains paint vehicle powder; The blending ratio controlling lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide makes the composition of described paint vehicle powder and content control: lanthanide rare compound 6.5wt%, aluminum oxide 24.5wt%, silicon carbide 17wt%, all the other are zirconium white and some inevitable impurity, and zirconia content is greater than 35wt%.
Oxidation of impurities iron <0.025wt% in described nanoscale zirconia ceramic, oxidation of impurities titanium <0.05wt%, impurity oxygen SiClx <0.12wt%.The purity of alumina in Nano level ceramic is more than 99.8%, and other material purity controls more than 99.5%.
3, batch mixing: by modified fluoro-silicone solvent and paint vehicle powder by 1: 1.45 weight ratio mix, under 450 ~ 800 turns/min after strong stirring 45min, obtain zirconium based high-temp-resistant composite ceramics coating.
Dewater by the zirconium based high-temp-resistant composite ceramics paint spay-coating obtained by aforesaid method through seasoning behind stainless steel cylinder surface, spraying like this 3 times, through High Temperature Furnaces Heating Apparatus under 1350 DEG C of heating, roasting 72 hours under the flue gas condition such as acid, alkaline, zirconium based high-temp-resistant composite ceramics dope layer is observed after naturally cooling, circulation like this does not find that its top layer is damaged for 10 times, high temperature resistant, acid-alkali-corrosive-resisting is good.
Embodiment 4
1, modified fluoro-silicone solvent is prepared: elemental silicon, fluorine gas are evenly slowly added to the water by the weight ratio of 1: 1, heating in water bath to 90 DEG C, strong stirring 60min under 450 ~ 800 turns/min, then be incubated 100 ~ 120min, then room temperature is naturally cooled to, obtained modified fluoro-silicone solvent;
2, prepare paint vehicle powder: by lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide mix after under argon atmosphere roasting 120min, maturing temperature is 1740 DEG C, obtains paint vehicle powder; The blending ratio controlling lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide makes the composition of described paint vehicle powder and content control: lanthanide rare compound 5.5wt%, aluminum oxide 21.5wt%, silicon carbide 12wt%, all the other are zirconium white and some inevitable impurity, and zirconia content is greater than 35wt%.
Oxidation of impurities iron <0.025wt% in described nanoscale zirconia ceramic, oxidation of impurities titanium <0.05wt%, impurity oxygen SiClx <0.05wt%.The purity of alumina in Nano level ceramic is more than 99.8%, and other material purity controls more than 99.5%.
3, batch mixing: by modified fluoro-silicone solvent and paint vehicle powder by 1: 1.25 weight ratio mix, under 450 ~ 800 turns/min after strong stirring 60min, obtain zirconium based high-temp-resistant composite ceramics coating.
Dewater by the zirconium based high-temp-resistant composite ceramics paint spay-coating obtained by aforesaid method through seasoning behind stainless steel cylinder surface, spraying like this 3 times, through High Temperature Furnaces Heating Apparatus under 1350 DEG C of heating, roasting 72 hours under the flue gas condition such as acid, alkaline, zirconium based high-temp-resistant composite ceramics dope layer is observed after naturally cooling, circulation like this does not find that its top layer is damaged for 10 times, high temperature resistant, acid-alkali-corrosive-resisting is good.
Comparative example 1
Except maturing temperature is 1650 DEG C, other are identical with embodiment 1.
Dewater by the zirconium based high-temp-resistant composite ceramics paint spay-coating obtained by aforesaid method through seasoning behind stainless steel cylinder surface, spraying like this 3 times, through High Temperature Furnaces Heating Apparatus under 1350 DEG C of heating, roasting 72 hours under the flue gas condition such as acid, alkaline, zirconium based high-temp-resistant composite ceramics dope layer is observed after naturally cooling, circulation like this finds that tiny crack appears in its top layer for 5 times, and because maturing temperature is inadequate, its high-temperature behavior is deteriorated.
Comparative example 2
Except the oxidation of impurities iron in nanoscale zirconia ceramic is 0.14wt%>0.025wt%, oxidation of impurities titanium is 0.115wt%>0.05wt%, impurity oxygen SiClx is beyond 0.20wt%>0.12wt%, and other are identical with embodiment 1.
Dewater through seasoning after being sprayed on stainless steel cylinder surface by the high temperature resistant paint vehicle obtained by aforesaid method, spraying like this 2-3 time, through High Temperature Furnaces Heating Apparatus under 1300 DEG C of heating, roasting 72 hours under the flue gas condition such as acid, alkaline, zirconium based high-temp-resistant composite ceramics dope layer is observed after naturally cooling, circulation like this 4 its top layer badly brokens, because foreign matter content is too high in zirconia powder, its high-temperature behavior is deteriorated.
Comparative example 3
Except maturing temperature is 1780 DEG C, other are identical with embodiment 1.
Dewater through seasoning after being sprayed on stainless steel cylinder surface by the high temperature resistant paint vehicle obtained by aforesaid method, spraying like this 3 times, through High Temperature Furnaces Heating Apparatus under 1350 DEG C of heating, roasting 72 hours under the flue gas condition such as acid, alkaline, zirconium based high-temp-resistant composite ceramics dope layer is observed after naturally cooling, there is tiny crack in circulation like this 6 its top layers, because of ceramic powder burning, its high-temperature behavior is deteriorated.
Comparative example 4
Except the alumina content in paint vehicle powder is 58.5wt%, other are identical with embodiment 1.
Dewater through seasoning after being sprayed on stainless steel cylinder surface by the high temperature resistant paint vehicle obtained by aforesaid method, spraying like this 3 times, through High Temperature Furnaces Heating Apparatus under 1350 DEG C of heating, roasting 72 hours under the flue gas condition such as acid, alkaline, observe zirconium based high-temp-resistant nano composite ceramic paint vehicle layer after naturally cooling, so there is tiny crack, because in ceramic powder raw material, alumina content is too high in circulation 3 its top layers, rare earth and zirconium white amount reduce, and cause its high-temperature behavior to be deteriorated.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalents utilizing description of the present invention to do, or be directly or indirectly used in relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (7)
1. a preparation method for zirconium based high-temp-resistant composite ceramics coating, is characterized in that, comprising:
By elemental silicon and fluorine source by 1: 1 ~ 1: 5 weight ratio be added to the water, heated and stirred reaction 60 ~ 90min, Heating temperature is 90 ~ 100 DEG C, and stir speed (S.S.) is 450 ~ 800 turns/min, obtains modified fluoro-silicone solvent;
By lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide mix after under isolated air or inert atmosphere roasting 110 ~ 120min, maturing temperature is 1720 ~ 1750 DEG C, obtains paint vehicle powder; The blending ratio controlling lanthanide rare micro mist, nanoscale zirconia ceramic, alumina in Nano level ceramic and silicon carbide makes the composition of described paint vehicle powder and content control: lanthanide rare compound 4.5 ~ 6.5wt%, aluminum oxide 21.5 ~ 24.5wt%, silicon carbide 12 ~ 17wt%, all the other are zirconium white and inevitable impurity, and zirconia content is greater than 35wt%;
By described modified fluoro-silicone solvent and paint vehicle powder by 1: 1.15 ~ 1: 1.45 weight ratio mix, obtain zirconium based high-temp-resistant composite ceramics coating;
Wherein, described fluorine source is selected from the one in fluorine gas, hydrogen fluoride, nonmetal fluorochemical and Neutral ammonium fluoride.
2. the preparation method of zirconium based high-temp-resistant composite ceramics coating according to claim 1, is characterized in that: the mode of described heating is heating in water bath.
3. the preparation method of zirconium based high-temp-resistant composite ceramics coating according to claim 1, it is characterized in that: described elemental silicon and fluorine source are after heated and stirred reaction 60 ~ 90min, be incubated 100 ~ 120min again, then naturally cool to room temperature, obtain modified fluoro-silicone solvent.
4. the preparation method of zirconium based high-temp-resistant composite ceramics coating according to claim 1, it is characterized in that: in described nanoscale zirconia ceramic, oxidation of impurities iron <0.025wt%, oxidation of impurities titanium <0.06wt%, impurity oxygen SiClx <0.12wt%.
5. the preparation method of zirconium based high-temp-resistant composite ceramics coating according to claim 1, is characterized in that: the purity of described alumina in Nano level ceramic is more than 99.8%.
6. the preparation method of zirconium based high-temp-resistant composite ceramics coating according to claim 1, is characterized in that: the purity of described lanthanide rare micro mist and silicon carbide is more than 99.5%.
7. the preparation method of zirconium based high-temp-resistant composite ceramics coating according to claim 1, is characterized in that: described inert atmosphere is argon atmosphere.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108840652A (en) * | 2018-07-18 | 2018-11-20 | 合肥峰腾节能科技有限公司 | A kind of ceramic coating and preparation method thereof |
| CN111777412A (en) * | 2020-07-14 | 2020-10-16 | 嘉兴饶稷科技有限公司 | 3D ceramic printing process for large-size model |
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| CN1328173A (en) * | 2001-06-08 | 2001-12-26 | 中国科学院兰州化学物理研究所 | Process for preparing zirconium oxide-base ceramic film |
| CN1562879A (en) * | 2004-03-31 | 2005-01-12 | 南京工业大学 | High-strength and high-toughness zirconia-based ceramic and preparation method thereof |
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| JP2000516905A (en) * | 1997-05-28 | 2000-12-19 | ツェルデック アクチェンゲゼルシャフト ケラーミッシェ ファルベン | Coating powders for electrostatic coating of glass and ceramic and metal substrates, their production and use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108840652A (en) * | 2018-07-18 | 2018-11-20 | 合肥峰腾节能科技有限公司 | A kind of ceramic coating and preparation method thereof |
| CN111777412A (en) * | 2020-07-14 | 2020-10-16 | 嘉兴饶稷科技有限公司 | 3D ceramic printing process for large-size model |
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| CN104402226B (en) | 2016-08-24 |
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