CN108585503B - Novel anti-static ceramic glaze and preparation method and application thereof - Google Patents
Novel anti-static ceramic glaze and preparation method and application thereof Download PDFInfo
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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
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- 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
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- C04B33/00—Clay-wares
- C04B33/32—Burning methods
- C04B33/34—Burning methods combined with glazing
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention discloses a novel antistatic ceramic glaze and a preparation method and application thereof, wherein common transparent ceramic glaze mainly made of mineral raw materials is subjected to microwave continuous synthesis under the condition of heat preservation at the temperature of 1100-1300 ℃ for 20-30 minutes, the common transparent ceramic glaze is directly poured into water for quenching after being melted, then the prepared frit is put into a ball milling tank for grinding, a 400-mesh sieve is sieved to obtain frit powder, the frit powder and aluminum-doped zinc oxide conductive powder which is sieved by a 150-200-mesh sieve are weighed and mixed according to the mass ratio of 20-30%, 60% deionized water is added for ball milling and mixing uniformly, sodium carboxymethylcellulose is added for adjusting the performance of glaze, thus glaze slurry is prepared, the prepared slurry is aged and then is applied to a dried ceramic biscuit by adopting a glaze dipping method, and the glaze soaking time is 3 seconds. And (3) drying the glazed ceramic blank in a drying box, and sintering by adopting a microwave continuous sintering process. The ceramic glaze obtained by the invention has smooth and flat glaze surface, no bubble, transparency, good chemical stability, no toxicity, environmental protection, low price and the like.
Description
Technical Field
The invention relates to the field of ceramics, in particular to a novel anti-static ceramic glaze and a preparation method and application thereof.
Background
From a microstructure point of view, conductive particles must be present in the vitreous phase of the glaze in order to make the glaze conductive, but if the conductive particles are dispersed among each other, a conductive path cannot be formed, the glaze is not conductive, and therefore it is critical that the conductive particles are connected to each other. The conductive particles are connected by first melting the glass phase of the glaze so that the molten glass phase melts a portion of the conductive particles to form a flowable conductive melt layer. At high temperature, the conductive melt layer diffuses and permeates along with the liquid glaze glass to connect isolated conductive particles around to form a conductive vein, and when the continuous and uninterrupted conductive veins are communicated in the three-dimensional direction, the glaze surface has electrical property, so that the antistatic effect is achieved.
Antistatic glazes are generally prepared by adding a certain amount of conductive metal, carbon and metal oxide series or compounds to a common glaze material, followed by sintering. The metal oxide conductive powder mainly contains Fe2O3、TiO2、SnO2ZnO, etc. In the production of antistatic glaze, because of Fe2O3、TiO2Unstable performance and deep color without mass popularization, and SnO2Belongs to scarce resources and is limited in application. The zinc oxide conductive powder has unique advantages as a conductive filler. The antistatic glaze mainly comprises a glass phase, a conductive melt layer and conductive particles, wherein the conductive melt layer connects the conductive particles through permeation and diffusion and penetrates through the glass matrix to form a continuous conductive network.
The transparent glaze contains silica glass network and boron-oxygen network. When the glaze contains boron, the network is compact, free electrons are difficult to pass through the network, and the resistance of the glass glaze is increased. Meanwhile, zinc oxide and boron oxide begin to react at about 500 ℃ to generate ZnB with low melting point2O4(zinc borate), which acts as an accelerator during melting. Therefore, the zinc oxide has strong fluxing action in the glaze containing boron, so the invention selects the glaze without boric acidThe glaze of salt serves as the base glaze. Meanwhile, considering the melting of zinc oxide in glaze components, the AZO conductive powder for preparing the antistatic glaze disclosed by the invention is sieved by a sieve of 150-200 meshes, and in addition, the zinc oxide starts to react with amorphous SiO in a glass phase from 750 DEG C2The reaction generates willemite, and when the silicon dioxide exists in the form of quartz, the initial temperature of the reaction is between 1000 and 1100 ℃, so in order to avoid the generation of a large amount of zinc silicate crystal phase, the glaze component of the invention takes mineral raw materials as main components. The microwave solid phase method is a novel synthesis mode, has the advantages of high synthesis speed, low temperature, energy conservation and environmental protection, and improves the yield after microwave serialization.
The invention content is as follows:
the invention aims to overcome the defects of the prior art and provides a novel anti-static ceramic glaze as well as a preparation method and application thereof.
The invention adopts the following technical scheme:
a preparation method of a novel anti-static ceramic glaze is characterized by comprising the following steps:
(1) carrying out microwave continuous synthesis on a common ceramic transparent glaze sold in the market at the temperature of 1100-1300 ℃ for 20-30 minutes, directly pouring the molten common ceramic transparent glaze into water for quenching to obtain a fusion cake;
(2) grinding the prepared fusion cake in a ball milling tank, and sieving with a 300-plus-500-mesh sieve to obtain fusion cake powder;
(3) mixing with aluminum-doped zinc oxide conductive powder, adding deionized water into the mixed powder, and ball-milling and mixing uniformly;
(4) and adding sodium carboxymethylcellulose to prepare the novel antistatic ceramic glaze.
Preferably, the microwave continuous synthesis has the power of 3.0-5.0 kW.
Preferably, the aluminum-doped zinc oxide conductive powder is prepared by the following preparation method:
(1) adding ZnO and Al2O3Putting the powder into a ball milling tank, adding grinding balls and ethanol solution for dispersion according to the weight ratio of the powder, the grinding balls and the ethanol of 1 (1.6-2) to (0.5-1), and carrying out ball milling mixing on a ball mill for 10-15 h;
(2) mixing, drying at 100 deg.C in a drying oven;
(3) putting the dried mixed powder into an alumina crucible, and putting the crucible into a microwave continuous synthesis furnace for synthesis under the conditions of 1200-1300 ℃ and heat preservation for 0.5-1h to obtain conductive powder;
(4) putting the conductive powder synthesized by microwave into a ball milling tank, grinding in a ball mill according to the weight ratio of the conductive powder to a grinding ball of 1 (1.6-2), wherein the ball milling time is 1-3 hours, and sieving with a sieve of 150-200 meshes to obtain the aluminum-doped zinc oxide conductive powder.
More preferably, in the powder, Al2O3The powder content is 1.25-2.50 wt%.
Preferably, the dosage of the aluminum-doped zinc oxide conductive powder is 20-30% of the total amount of the powder.
Preferably, the raw materials for the synthesis of the commercially available common ceramic clear glaze do not contain borate.
A novel antistatic ceramic glaze is prepared by the preparation method according to any one of the above.
An application of a novel anti-static ceramic glaze for preparing anti-static ceramic tiles.
Preferably, the method specifically comprises the following steps:
(1) the novel anti-static ceramic glaze slurry is aged for 6-12 hours and is applied to a dry ceramic biscuit by a glaze dipping method, and the glaze dipping time is 3 seconds.
(2) And (3) drying the glazed ceramic blank in a drying box, and sintering by adopting a microwave continuous sintering process.
Further preferably, the sintering temperature of the microwave continuous sintering process adopted in the step (2) is 1050-; the power is 3.0-5.0 kW.
The invention adopts common transparent glaze sold in the market, adopts mineral raw materials, and prevents ZnO conductive powder from reacting with borate in the mineral raw materials to generate ZnB with low melting point2O4(Zinc borate, not conducive to electrical conduction), so the present invention uses borate-free glazes as the preferred base glazes.
The sodium carboxymethyl cellulose plays a role in adjusting the performance of the glaze, the glaze slip is different from the surface wetting condition of ceramic green bodies with different components, the rheological property of the glaze slip on the surfaces of the ceramic green bodies with different components is also different, the expansion and contraction conditions at high temperature are different, and the glaze can form patterns or even crack, so that the performance of the glaze can be adjusted by adding the sodium carboxymethyl cellulose in a proper amount according to the condition of the ceramic green bodies in practical application.
According to the main composition of the mineral raw material (SiO)2The content is 50-60 percent) and the average grain diameter (nanometer, submicron and micron), the heating rate is controlled by properly adjusting the power of the microwave (2-5kW is continuously adjustable), so as to better implement the microwave continuous synthesis of the common ceramic transparent glaze frit according to the actual situation.
The invention has the beneficial effects that: the ceramic glaze obtained by the invention has smooth and flat glaze surface, no bubble, transparency, good chemical stability, no toxicity, environmental protection, low price and the like, and the antistatic glaze surface has the resistance of 30-180 MOmega.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The common ceramic transparent glaze used in the examples had SiO as the main component2、Al2O3、Fe2O3、TiO2、CaO、MgO、K2O、Na2O、BaO。
Example 1:
preparing aluminum-doped zinc oxide conductive powder:
(1) adding ZnO and Al2O3Putting the powder into a ball milling tank, wherein Al is contained in the powder2O3The powder accounts for 2.5 percent of the total amount of the powder, then grinding balls and ethanol solution are added according to the weight ratio of 1:1.6:1 of the powder, the grinding balls and the ethanol solution for dispersion, and ball milling and mixing are carried out on a ball mill for 12 hours;
(2) mixing, drying at 100 deg.C in a drying oven;
(3) putting the dried mixed powder into an alumina crucible, and putting the crucible into a microwave continuous synthesis furnace for synthesis, wherein the microwave power is generally 5kW, the synthesis condition is 1250 ℃, and the heat preservation is carried out for 1h to obtain conductive powder;
(4) putting the conductive powder synthesized by microwave into a ball milling tank, grinding in a ball mill according to the weight ratio of the conductive powder to the grinding balls of 1:2, wherein the ball milling time is 3 hours, and sieving by a 180-mesh sieve to obtain the aluminum-doped zinc oxide conductive powder, wherein the resistivity of the conductive powder is 9.8k omega cm.
Preparing a novel antistatic ceramic glaze:
(1) carrying out microwave continuous synthesis on a common ceramic transparent glaze sold in the market at 1100 ℃ for 30 minutes with the power of 3.0kW, directly pouring the molten common ceramic transparent glaze into water for quenching to obtain a fusion cake;
(2) grinding the prepared fusion cake in a ball milling tank, and sieving with a 500-mesh sieve to obtain fusion cake powder;
(3) mixing the powder with aluminum-doped zinc oxide conductive powder, wherein the dosage of the aluminum-doped zinc oxide conductive powder is 20% of the total amount of the powder, adding 60% of deionized water into the mixed powder, and ball-milling and uniformly mixing;
(4) and adding sodium carboxymethylcellulose to prepare the novel antistatic ceramic glaze.
Example 2:
preparing aluminum-doped zinc oxide conductive powder:
(1) adding ZnO and Al2O3Putting the powder into a ball milling tank, wherein Al is contained in the powder2O3Adding grinding balls and ethanol solution into the powder which accounts for 1.25% of the total amount of the powder according to the weight ratio of the powder to the grinding balls to the ethanol of 1:2:0.5 for dispersion, and performing ball milling and mixing on a ball mill for 15 hours;
(2) mixing, drying at 100 deg.C in a drying oven;
(3) putting the dried mixed powder into an alumina crucible, and putting the crucible into a microwave continuous synthesis furnace for synthesis, wherein the microwave power is generally 3kW, the synthesis condition is 1300 ℃, and the heat preservation time is 0.5h, so as to obtain conductive powder;
(4) putting the conductive powder synthesized by microwave into a ball milling tank, grinding in a ball mill according to the weight ratio of the conductive powder to the grinding ball of 1:1.8, wherein the ball milling time is 2 hours, and sieving by a 200-mesh sieve to obtain the aluminum-doped zinc oxide conductive powder, wherein the resistivity of the conductive powder is 5.8k omega cm.
Preparing a novel antistatic ceramic glaze:
(1) carrying out microwave continuous synthesis on a common ceramic transparent glaze sold in the market at 1300 ℃ for 20 minutes with the power of 5.0kW, directly pouring the molten common ceramic transparent glaze into water for quenching to obtain a fusion cake;
(2) grinding the prepared fusion cake in a ball milling tank, and sieving with a 300-mesh sieve to obtain fusion cake powder;
(3) mixing the powder with aluminum-doped zinc oxide conductive powder, wherein the dosage of the aluminum-doped zinc oxide conductive powder is 30% of the total amount of the powder, adding the mixed powder into deionized water accounting for 60% of the system, and performing ball milling and mixing uniformly;
(4) and adding sodium carboxymethylcellulose to prepare the novel antistatic ceramic glaze.
Example 3:
preparing aluminum-doped zinc oxide conductive powder:
(1) adding ZnO and Al2O3Putting the powder into a ball milling tank, wherein Al is contained in the powder2O3The powder accounts for 2.0 percent of the total amount of the powder, then the grinding balls and ethanol solution are added according to the weight ratio of 1:1.8:0.8 of the powder to the grinding balls and the ethanol solution for dispersion, and the mixture is subjected to ball milling and mixing on a ball mill for 10 hours;
(2) mixing, drying at 100 deg.C in a drying oven;
(3) putting the dried mixed powder into an alumina crucible, and putting the crucible into a microwave continuous synthesis furnace for synthesis, wherein the microwave power is generally 1kW, the synthesis condition is 1200 ℃, and the heat preservation time is 0.8h, so as to obtain conductive powder;
(4) putting the conductive powder synthesized by microwave into a ball milling tank, grinding in a ball mill according to the weight ratio of the conductive powder to the grinding balls of 1:1.6, wherein the ball milling time is 1 hour, and sieving by a 150-mesh sieve to obtain the conductive powder doped with the aluminum zinc oxide, wherein the resistivity of the conductive powder is 3.0k omega cm.
Preparing a novel antistatic ceramic glaze:
(1) carrying out microwave continuous synthesis on a common ceramic transparent glaze sold in the market at 1200 ℃ for 25 minutes under the condition of heat preservation, wherein the power is 4.0kW, and directly pouring the molten common ceramic transparent glaze into water for quenching to obtain a fusion cake;
(2) grinding the prepared fusion cake in a ball milling tank, and sieving with a 400-mesh sieve to obtain fusion cake powder;
(3) mixing the powder with aluminum-doped zinc oxide conductive powder, wherein the dosage of the aluminum-doped zinc oxide conductive powder is 26 percent of the total amount of the powder, adding the mixed powder into deionized water accounting for 60 percent of the system, and ball-milling and uniformly mixing;
(4) and adding sodium carboxymethylcellulose to prepare the novel antistatic ceramic glaze.
Example 4:
application of the novel antistatic ceramic glaze prepared in example 1:
(1) the novel antistatic ceramic slurry prepared in example 1 was aged for 6 hours and applied to a dried ceramic biscuit by a glaze dipping method for 3 seconds.
(2) Drying the glazed ceramic blank in a drying oven, and sintering by adopting a microwave continuous sintering process at 1050 ℃ for 0.1 h; the power is 4.0 kW.
The obtained antistatic glaze has a resistance of 180M omega.
Example 5:
application of the novel antistatic ceramic glaze prepared in example 1:
(1) the novel antistatic ceramic slurry prepared in example 1 was aged for 10 hours and applied to a dried ceramic biscuit by a glaze dipping method for 3 seconds.
(2) Drying the glazed ceramic blank in a drying oven, and sintering by adopting a microwave continuous sintering process at 1150 ℃ for 0.15 h; the power is 3.0 kW.
The obtained antistatic glaze has a resistance of 90M omega.
Example 6:
application of the novel antistatic ceramic glaze prepared in example 1:
(1) the novel antistatic ceramic slurry prepared in example 1 was aged for 12 hours and applied to a dried ceramic biscuit by a glaze dipping method for 3 seconds.
(2) Drying the glazed ceramic blank in a drying oven, and sintering by adopting a microwave continuous sintering process at 1100 ℃ for 0.25 h; the power is 5.0 kW.
The obtained antistatic glaze has a resistance of 30 MOmega.
The above embodiments are only for illustrating the technical solutions of the present invention and are not limited thereto, and any modification or equivalent replacement without departing from the spirit and scope of the present invention should be covered by the technical solutions of the present invention.
Claims (9)
1. A preparation method of a novel anti-static ceramic glaze is characterized by comprising the following steps:
(1) carrying out microwave continuous synthesis on a common ceramic transparent glaze sold in the market at the temperature of 1100-1300 ℃ for 20-30 minutes, directly pouring the molten common ceramic transparent glaze into water for quenching to obtain a fusion cake;
(2) grinding the prepared fusion cake in a ball milling tank, and sieving with a 300-plus-500-mesh sieve to obtain fusion cake powder;
(3) mixing with aluminum-doped zinc oxide conductive powder, adding deionized water into the mixed powder, and ball-milling and mixing uniformly;
(4) adding sodium carboxymethylcellulose to obtain the novel antistatic ceramic glaze,
the microwave continuous synthesis has the power of 3.0-5.0 kW.
2. The preparation method of the novel antistatic ceramic glaze according to claim 1, wherein the aluminum-doped zinc oxide conductive powder is prepared by the following preparation method:
(1) adding ZnO and Al2O3Putting the powder into a ball milling tank, adding grinding balls and ethanol solution for dispersion according to the weight ratio of the powder, the grinding balls and the ethanol of 1 (1.6-2) to (0.5-1), and carrying out ball milling mixing on a ball mill for 10-15 h;
(2) mixing, drying at 100 deg.C in a drying oven;
(3) putting the dried mixed powder into an alumina crucible, and putting the crucible into a microwave continuous synthesis furnace for synthesis under the conditions of 1200-1300 ℃ and heat preservation for 0.5-1h to obtain conductive powder;
(4) putting the conductive powder synthesized by microwave into a ball milling tank, grinding in a ball mill according to the weight ratio of the conductive powder to a grinding ball of 1 (1.6-2), wherein the ball milling time is 1-3 hours, and sieving with a sieve of 150-200 meshes to obtain the aluminum-doped zinc oxide conductive powder.
3. The method for preparing a novel antistatic ceramic glaze according to claim 2, wherein Al in the powder is2O3The powder content is 1.25-2.50 wt%.
4. The method for preparing a novel antistatic ceramic glaze according to claim 1, wherein the amount of the aluminum-doped zinc oxide conductive powder is 20-30% of the total amount of the powder.
5. The method for preparing a novel antistatic ceramic glaze according to claim 1, wherein the raw materials for synthesizing the common ceramic transparent glaze sold in the market do not contain borate.
6. A novel antistatic ceramic glaze, characterized in that it is prepared by the process according to any one of claims 1 to 3.
7. Use of the novel antistatic ceramic glaze according to claim 6 for the preparation of antistatic ceramic tiles.
8. The application of the novel antistatic ceramic glaze according to claim 7 is characterized in that the specific application method is as follows:
(1) the novel anti-static ceramic glaze slurry is aged for 6 to 12 hours and is applied to a dry ceramic biscuit by a glaze dipping method, and the glaze dipping time is 3 seconds;
(2) and (3) drying the glazed ceramic blank in a drying box, and sintering by adopting a microwave continuous sintering process.
9. The application of the novel antistatic ceramic glaze as claimed in claim 8, wherein the sintering temperature of the microwave continuous sintering process adopted in the step (2) is 1050-; the power is 3.0-5.0 kW.
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