CN108793752B - Microwave medium glaze water and preparation method thereof - Google Patents
Microwave medium glaze water and preparation method thereof Download PDFInfo
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- CN108793752B CN108793752B CN201810709946.3A CN201810709946A CN108793752B CN 108793752 B CN108793752 B CN 108793752B CN 201810709946 A CN201810709946 A CN 201810709946A CN 108793752 B CN108793752 B CN 108793752B
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- water
- glaze water
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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
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
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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
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/20—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
Abstract
The invention provides microwave medium glaze water and a preparation method thereof, wherein the preparation method comprises the following steps: preparing materials, preparing a frit, roughly adjusting glaze water, preparing a graphene oxide dispersion liquid, preparing tungsten zirconate powder, preparing a mixed liquid, finely adjusting glaze water, adjusting the pH value, and forming the glaze water. The microwave medium glaze water disclosed by the invention is strong in stability, has a more stable temperature coefficient, is simple in preparation process, is pollution-free in process, has partial characteristics of graphene and better strength and conductivity, and is capable of reducing graphene oxide into graphene under the catalysis of far infrared rays, so that the graphene is gradually combined with zirconium tungstate in the process, and the graphene can be combined with the zirconium tungstate more tightly and uniformly, has a very important effect on improving the final quality of the glaze water, improves the quality of a ceramic product, has a low-expansion characteristic, and has an important industrial application value.
Description
Technical Field
The invention belongs to the technical field of glaze water preparation, and particularly relates to microwave medium glaze water and a preparation method thereof.
Background
The ceramic is one of the most common appliances in daily life, has wide application, various ceramics on the market and different functions, and has a plurality of new ceramic varieties in the last hundred years along with the development of modern science and technology. They no longer use or rarely use traditional ceramic raw materials such as clay, feldspar, quartz, etc., but use other special raw materials, even expand to the range of non-silicate, non-oxide, and have appeared many new processes.
The microwave dielectric ceramic is a ceramic which is used as a dielectric material and completes one or more functions in a microwave frequency band (mainly UHF, SHF frequency band, 300MHz-300GHz) circuit, is a hot direction in the microwave dielectric material research field at home and abroad in recent years, is mainly used as a resonator, a filter, a dielectric antenna, a dielectric guided wave loop and other microwave components, can be used in the aspects of mobile communication, satellite communication, military radar and the like, and along with the development of scientific technology, the rapid increase of communication information quantity and the requirement of people on wireless communication, a microwave communication system using satellite communication, satellite direct broadcast television and the like becomes a necessary trend of the development of the current communication technology, and the microwave dielectric ceramic is used for widely manufacturing a microwave dielectric filter and a resonator in the aspects of portable mobile phones, automobile phones, cordless phones, television satellite receivers, military radars and the like, plays an increasingly important role in the miniaturization and integration of modern communication tools.
The glaze layer of the ceramic is one of the quality indexes of the ceramic, and the improvement of the quality and the performance of the glaze layer has important significance for improving the quality of the ceramic product.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides microwave medium glaze water and a preparation method thereof, wherein the glaze water has strong stability and more stable temperature coefficient, and can improve the quality and performance of ceramic products.
In order to achieve the purpose, the invention is realized by the following technical scheme: a microwave medium glaze water and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
the method comprises the following steps: preparing materials; taking 55.17% of barium carbonate, 25.46% of niobium oxide, 4.25% of cobalt oxide, 2.12% of zinc oxide, 0.17% of gallium oxide, 4.81% of graphene oxide, 2.83% of magnesium oxide and 5.19% of zirconium tungstate, and removing impurities from the raw materials;
step two: preparing a frit; mixing barium carbonate, niobium oxide, cobalt oxide, zinc oxide and magnesium oxide according to the raw material ratio, grinding for 8-10h by using a ball mill, then putting into a kiln to be melted into blocks, preserving heat for 2h, then water quenching, and grinding for later use after water quenching;
step three: coarse adjustment of glaze water; taking gallium oxide with corresponding weight according to the proportion of the raw materials, grinding, putting the frit powder obtained in the step two into a proper container, adding gallium oxide powder, mixing uniformly, adding water, and diluting to prepare glaze slurry;
step four: preparing a graphene oxide dispersion liquid; taking a proper amount of graphene oxide powder according to the raw material ratio, placing the graphene oxide powder into a proper container, adding a macromolecular dispersing agent, uniformly mixing, and then carrying out ultrasonic oscillation for 12 hours;
step five: preparing tungsten zirconate powder; slowly adding a zirconium-containing solution and a tungsten-containing solution of 0.5mol/L into water at room temperature under stirring, wherein the ratio of the water to the zirconium-containing solution to the tungsten-containing solution is 0.25:0.5:1, continuously stirring for 10h, then adding hydrochloric acid of 6mol/L, fractionating the mixture for 2 days, standing for 3 weeks after fractionation to gelatinize the mixture, then pouring out a supernatant, filtering, washing, drying in an oven at 353K, heating for 10h at 873K, and then grinding for later use;
step six: preparing a mixed solution; adding a proper amount of tungsten zirconate powder into the graphene oxide dispersion liquid in the step four according to the raw material ratio, uniformly mixing, fully irradiating the mixed liquid for 24 hours by using far infrared rays, reducing the graphene oxide into graphene, and fully combining the graphene oxide with the tungsten zirconate powder;
step seven: finely adjusting glaze water; fully stirring and mixing the glaze slurry in the third step and the mixed liquid in the sixth step to prepare glaze water, and adjusting the water content of the glaze water to 28-32%;
step eight: adjusting the pH value; detecting the pH value of the glaze water, and properly adjusting;
step nine: molding glaze water; standing the glaze water for a period of time, and then reserving for later use.
In a preferred embodiment of the present invention, the step two of grinding is performed by coarse grinding and then grinding into powder by using a ball mill.
In a preferred embodiment of the present invention, the water content of the glaze slurry diluted by adding water in the third step is 23 to 33%.
In a preferred embodiment of the present invention, the pH value after the adjustment in step eight should be about 8.6.
As a preferable mode of the invention, all equipment is cleaned before the glaze water is prepared, so that the influence on the quality of finished products caused by impurities mixed in raw materials is avoided.
As a preferred mode of the invention, the calcination temperature in the second step is 1020-1150K.
The invention has the beneficial effects that:
1. the microwave medium glaze water provided by the invention has the advantages of strong stability, more stable temperature coefficient, simple preparation process, no pollution in the process, partial characteristics of graphene, and better strength and conductivity.
2. Meanwhile, far infrared ray catalysis is adopted in the glaze water preparation process to reduce graphene oxide into graphene, so that the graphene is gradually combined with zirconium tungstate powder in the process, the graphene can be combined with the zirconium tungstate powder more tightly and uniformly, the final quality of the glaze water is improved, and the ceramic product quality is improved.
3. The microwave medium glaze water has the characteristic of low expansion, so that the microwave medium glaze water has important industrial application value, and the microwave medium glaze water has simple steps, is convenient and controllable to prepare, improves the preparation efficiency of the glaze water, and has wide adaptability.
Drawings
FIG. 1 is a flow chart of a microwave medium glaze water and a preparation method thereof;
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Referring to fig. 1, the present invention provides a technical solution: a microwave medium glaze water and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
the method comprises the following steps: preparing materials; taking 55.17% of barium carbonate, 25.46% of niobium oxide, 4.25% of cobalt oxide, 2.12% of zinc oxide, 0.17% of gallium oxide, 4.81% of graphene oxide, 2.83% of magnesium oxide and 5.19% of zirconium tungstate, and removing impurities from the raw materials;
step two: preparing a frit; mixing barium carbonate, niobium oxide, cobalt oxide, zinc oxide and magnesium oxide according to the raw material ratio, grinding for 8-10h by using a ball mill, then putting into a kiln to be melted into blocks, preserving heat for 2h, then water quenching, and grinding for later use after water quenching;
step three: coarse adjustment of glaze water; taking gallium oxide with corresponding weight according to the proportion of the raw materials, grinding, putting the frit powder obtained in the step two into a proper container, adding gallium oxide powder, mixing uniformly, adding water, and diluting to prepare glaze slurry;
step four: preparing a graphene oxide dispersion liquid; taking a proper amount of graphene oxide powder according to the raw material ratio, placing the graphene oxide powder into a proper container, adding a macromolecular dispersing agent, uniformly mixing, and then carrying out ultrasonic oscillation for 12 hours;
step five: preparing tungsten zirconate powder; slowly adding a zirconium-containing solution and a tungsten-containing solution of 0.5mol/L into water at room temperature under stirring, wherein the ratio of the water to the zirconium-containing solution to the tungsten-containing solution is 0.25:0.5:1, continuously stirring for 10h, then adding hydrochloric acid of 6mol/L, fractionating the mixture for 2 days, standing for 3 weeks after fractionation to gelatinize the mixture, then pouring out a supernatant, filtering, washing, drying in an oven at 353K, heating for 10h at 873K, and then grinding for later use;
step six: preparing a mixed solution; adding a proper amount of tungsten zirconate powder into the graphene oxide dispersion liquid in the step four according to the raw material ratio, uniformly mixing, fully irradiating the mixed liquid for 24 hours by using far infrared rays, reducing the graphene oxide into graphene, and fully combining the graphene oxide with the tungsten zirconate powder;
step seven: finely adjusting glaze water; fully stirring and mixing the glaze slurry in the third step and the mixed liquid in the sixth step to prepare glaze water, and adjusting the water content of the glaze water to 28-32%;
step eight: adjusting the pH value; detecting the pH value of the glaze water, and properly adjusting;
step nine: molding glaze water; standing the glaze water for a period of time, and then reserving for later use.
In a preferred embodiment of the present invention, the step two of grinding is performed by coarse grinding and then grinding into powder by using a ball mill.
In a preferred embodiment of the present invention, the water content of the glaze slurry diluted by adding water in the third step is 23 to 33%.
In a preferred embodiment of the present invention, the pH value after the adjustment in step eight should be about 8.6.
As a preferable mode of the invention, all equipment is cleaned before the glaze water is prepared, so that the influence on the quality of finished products caused by impurities mixed in raw materials is avoided.
As a preferred mode of the invention, the calcination temperature in the second step is 1020-1150K.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. The microwave medium glaze water and the preparation method thereof are characterized by comprising the following steps:
the method comprises the following steps: preparing materials; taking 55.17% of barium carbonate, 25.46% of niobium oxide, 4.25% of cobalt oxide, 2.12% of zinc oxide, 0.17% of gallium oxide, 4.81% of graphene oxide, 2.83% of magnesium oxide and 5.19% of zirconium tungstate, and removing impurities from the raw materials;
step two: preparing a frit; mixing barium carbonate, niobium oxide, cobalt oxide, zinc oxide and magnesium oxide according to the raw material ratio, grinding for 8-10h by using a ball mill, then putting into a kiln to be melted into blocks, preserving heat for 2h, then water quenching, and grinding for later use after water quenching;
step three: coarse adjustment of glaze water; taking gallium oxide with corresponding weight according to the proportion of the raw materials, grinding, putting the frit powder obtained in the step two into a proper container, adding gallium oxide powder, mixing uniformly, adding water, and diluting to prepare glaze slurry;
step four: preparing a graphene oxide dispersion liquid; taking a proper amount of graphene oxide powder according to the raw material ratio, placing the graphene oxide powder into a proper container, adding a macromolecular dispersing agent, uniformly mixing, and then carrying out ultrasonic oscillation for 12 hours;
step five: preparing tungsten zirconate powder; slowly adding a zirconium-containing solution and a tungsten-containing solution of 0.5mol/L into water at room temperature under stirring, wherein the ratio of the water to the zirconium-containing solution to the tungsten-containing solution is 0.25:0.5:1, continuously stirring for 10h, then adding hydrochloric acid of 6mol/L, fractionating the mixture for 2 days, standing for 3 weeks after fractionation to gelatinize the mixture, then pouring out a supernatant, filtering, washing, drying in an oven at 353K, heating for 10h at 873K, and then grinding for later use;
step six: preparing a mixed solution; adding a proper amount of tungsten zirconate powder into the graphene oxide dispersion liquid in the step four according to the raw material ratio, uniformly mixing, fully irradiating the mixed liquid for 24 hours by using far infrared rays, reducing the graphene oxide into graphene, and fully combining the graphene oxide with the tungsten zirconate powder;
step seven: finely adjusting glaze water; fully stirring and mixing the glaze slurry in the third step and the mixed liquid in the sixth step to prepare glaze water, and adjusting the water content of the glaze water to 28-32%;
step eight: adjusting the pH value; detecting the pH value of the glaze water, and properly adjusting;
step nine: molding glaze water; standing the glaze water for a period of time, and then reserving for later use.
2. The microwave medium glaze water as claimed in claim 1, wherein the grinding process in the second step is coarse grinding and then grinding into powder by using a ball mill.
3. The microwave medium glaze water as claimed in claim 1, wherein the water content of the glaze slurry diluted by adding water in the third step is 23-33%.
4. The microwave medium glaze water as claimed in claim 1, wherein the pH value after the adjustment in step eight is 8.6.
5. The microwave medium glaze water as claimed in claim 1, wherein all equipment is cleaned before the glaze water is prepared, so as to avoid impurities mixed in the raw materials from affecting the quality of the finished product.
6. The microwave medium glaze water as claimed in claim 1, wherein the calcination temperature in step two is 1020-1150K.
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Citations (5)
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CN102761994A (en) * | 2011-04-25 | 2012-10-31 | 艾尔莎光电科技股份有限公司 | Nanometer ceramic electric-heating coating device and manufacturing method thereof |
CN103147226A (en) * | 2013-02-07 | 2013-06-12 | 江西师范大学 | Method for preparing high dielectric constant polymer-based nano composite material |
CN105924167A (en) * | 2016-04-20 | 2016-09-07 | 苏州艾福电子通讯股份有限公司 | Microwave dielectric ceramic powder, preparation method thereof, microwave dielectric ceramic and microwave component |
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CN101982435A (en) * | 2010-11-05 | 2011-03-02 | 中材高新材料股份有限公司 | Method for preparing low-temperature lead-free near zero expansion microcrystalline ceramic coating |
WO2012064399A1 (en) * | 2010-11-08 | 2012-05-18 | Baker Hughes Incorporated | Polycrystalline compacts including nanoparticulate inclusions, cutting elements and earth-boring tools including such compacts, and methods of forming same |
CN102761994A (en) * | 2011-04-25 | 2012-10-31 | 艾尔莎光电科技股份有限公司 | Nanometer ceramic electric-heating coating device and manufacturing method thereof |
CN103147226A (en) * | 2013-02-07 | 2013-06-12 | 江西师范大学 | Method for preparing high dielectric constant polymer-based nano composite material |
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