CN115448597B - Bonding glaze and preparation process and application thereof - Google Patents
Bonding glaze and preparation process and application thereof Download PDFInfo
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- CN115448597B CN115448597B CN202211051509.XA CN202211051509A CN115448597B CN 115448597 B CN115448597 B CN 115448597B CN 202211051509 A CN202211051509 A CN 202211051509A CN 115448597 B CN115448597 B CN 115448597B
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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
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- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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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
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- 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
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Abstract
The invention discloses an adhesive glaze, a preparation process and application thereof, and relates to the technical field of ceramic materials. The invention discloses a bonding glaze material, which consists of a basic glaze material, a modifier and a pigment, wherein the basic glaze material consists of the following raw materials: potassium feldspar powder, quartz powder, kaolin, micro aluminum powder, cooked talcum powder, uozhou soil, lawn field washing mud and wollastonite; the addition amount of the modifier is 1.6-2.5% of the total mass of the basic glaze, and the modifier is ZrSiO prepared by adopting a sol-gel method 4 ‑TiO 2 ‑GeO 2 A complex; the pigment is high-temperature pigment oxide. The bonding glaze provided by the invention has the advantages of easily available raw materials, low cost, good high-temperature fluidity, thinner glaze layer, good bonding effect, low porosity, difficult brittle fracture, bright glaze surface at the bonding position with the porcelain bushing, uniform color and no color difference; has excellent strength, toughness and weather resistance, also has excellent self-lubricating property, and prolongs the service life of porcelain bushing products.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a bonding glaze applicable to a porcelain bushing and a preparation process thereof.
Background
With the continuous increase of voltage level, the electric power and electric appliance industry requires more and more pollution-resistant large porcelain bushings with high voltage level. The higher the voltage level, the larger the geometric dimension of the porcelain bushing, and the more complex the structural shape. If the porcelain bushing product with higher voltage class (more than 500 kV) is manufactured as a whole conventionally, the molding process is complex, the difficulty is high, a large factory building, molding equipment and a professional firing kiln are needed, the electric porcelain belongs to brittle porcelain, the strength of the porcelain insulator serving as a blank is not high, the required product is up to a height of more than 3000mm, and the blank cannot be damaged due to the fact that the blank cannot bear dead weight, so that the porcelain insulator cannot be molded and fired for more than 3000mm in one step.
The porcelain insulator is formed by sintering the porcelain insulator and the porcelain insulator in a sectional mode, and then bonding and combining the sintered porcelain insulator, namely, the porcelain insulator is decomposed into single-section sintered porcelain and then bonded into a whole. The adhesive in the bonding process can be classified into inorganic bonding glaze and organic bonding glaze according to materials. The common organic bonding glaze is epoxy resin, phenolic resin and the like, and is widely applied due to good bonding property, simple bonding process and low price, so that most of domestic enterprises at present adopt the organic bonding glaze, but the organic bonding glaze is easy to flow when being solidified, is brittle, poor in elasticity, easy to age and general in electrical property, and is easy to cause the deterioration of strength, weather resistance and aging resistance of the bonded porcelain bushing, thereby influencing the service life of the porcelain bushing and bringing great hidden trouble to the normal operation of power equipment. The inorganic bonding glaze has excellent temperature resistance, oil resistance, good ageing resistance, high bonding strength and good electrical performance, but the inorganic bonding glaze can generate bubbles and is difficult to discharge in the sintering process, so that poor bonding quality is easily caused, and the bonding strength of bonding porcelain sleeves is affected; because the raw material components of the porcelain bushing and the inorganic bonding glaze are different, and the expansion coefficient of the bonding glaze is lower than that of the porcelain bushing, the bonding property of the bonding porcelain bushing is easy to be poor, the thermal stability is poor, the mechanical strength is lower, the later stage is easy to crack, the service life of the later stage product is influenced, and the safety accident is caused. Moreover, the research of inorganic bonding glaze by domestic researchers mainly focuses on bonding force and bonding strength, so that the glaze color of the bonding part of the porcelain sleeve is dull and not bright, and the appearance of the final product is affected.
Disclosure of Invention
The invention aims to provide the bonding glaze, which has the advantages of easily available raw materials, low cost, good high-temperature fluidity, thinner glaze layer, good bonding effect, high bonding strength, low porosity, difficult brittle failure, full and bright color, bright luster, uniform color and no color difference at the bonding position of the bonding glaze and the porcelain bushing; has excellent strength, toughness and weather resistance, also has excellent self-lubricating property and lower friction coefficient, and prolongs the service life of porcelain bushing products.
In order to achieve the aim of the invention, the invention provides a bonding glaze which consists of a basic glaze, a modifier and a pigment, wherein the basic glaze consists of the following raw materials in percentage by weight: 10 to 20 percent of potassium feldspar powder, 15 to 20 percent of quartz powder, 15 to 25 percent of kaolin, 3 to 5 percent of micro aluminum powder, 4 to 6 percent of cooked talcum powder, 5 to 10 percent of Uozhou soil, 10 to 20 percent of lawn field mud washing and 15 to 25 percent of wollastonite;
the addition amount of the modifier is 1.6-2.5% of the total mass of the basic glaze, and the modifier is ZrSiO 4 -TiO 2 -GeO 2 A complex;
the pigment is high-temperature pigment oxide.
Further, the particle diameter of the micro-aluminum powder is 1-20 mu m.
Further, the ZrSiO 4 -TiO 2 -GeO 2 The compound is prepared by adopting a sol-gel method.
Further, the ZrSiO 4 -TiO 2 -GeO 2 The preparation method of the compound specifically comprises the following steps:
(1) Adding a certain amount of tetraethoxysilane into 40wt% ethanol solution, adding 2mol/L hydrochloric acid, stirring for 0.5h, adding zirconium n-butoxide and lithium chloride, stirring for 1h, heating to 60-70 ℃ and stirring for reaction for 10-20 min to form transparent sol, cooling to room temperature, and continuing stirring for 1h to form zirconium silicate precursor gel;
(2) Adding 3-trichlorogermanopropionic acid and tetrabutyl orthotitanate into 30wt% ethanol solution, stirring uniformly, adding the mixture into the zirconium silicate precursor gel, adding a surfactant, mixing uniformly, and stirring at 80-90 ℃ for 1-2h to obtain a gel mixture;
(3) Stirring the gel mixture at 130-140 ℃ for reaction for 4-6 hours, cooling to room temperature, then washing with absolute ethyl alcohol, and then preserving heat for 4 hours at 700 ℃ to obtain ZrSiO 4 -TiO 2 -GeO 2 A complex.
Further, in the step (1), the molar ratio of Si to Zr in the tetraethoxysilane and the zirconium n-butoxide is (1.5 to 1.8): 1, wherein the molar ratio of Li to Zr in the lithium chloride to the zirconium n-butoxide is (0.05-0.08): 1, the ratio of Si in the ethyl orthosilicate to 40wt% ethanol solution is 0.8mol/L, and the volume ratio of the 40wt% ethanol solution to the hydrochloric acid is 3:1.
further, in the step (2), the molar ratio of Ge in the 3-trichlorogermanopropionic acid to Zr in the zirconium silicate precursor gel is (0.3 to 0.35): 1, a step of; the molar ratio of Ti in the tetrabutyl orthotitanate to Zr in the zirconium silicate precursor gel is (0.2-0.26): 1, a step of; the addition amount of the 30wt% ethanol solution is 2 times of the total mass of the 3-trichlorogermanium propionic acid and tetrabutyl orthotitanate.
Further, the surfactant is polyvinylpyrrolidone.
The invention also provides a preparation process of the bonding glaze, which specifically comprises the following steps:
s1, weighing a basic glaze according to the requirement, uniformly mixing, placing in a smelting furnace, heating to 1300-1350 ℃, preserving heat for 2-3h, and then performing water quenching to obtain a basic frit glaze;
s2, weighing the modifier and the pigment according to the requirements, then adding the modifier and the pigment into the basic frit glaze, uniformly mixing to obtain a glaze mixture, and then mixing the glaze mixture, the ball stone and water according to the mass ratio of 1:1:0.8 is put into a ball mill, and ball milling is carried out for 30-35 hours;
and S3, deironing the glaze slurry of the ball mill by using an iron removing machine, sieving the glaze slurry by using a 250-mesh sieve, ageing the glaze slurry for 72 hours, adjusting the moisture (25+/-0.5)%, and measuring the fluidity by using a viscometer for 58+/-2 seconds to obtain the bonding glaze.
The invention provides an application method of bonding glaze, which comprises the following specific steps:
p1, coating the bonding glaze on the connecting end surfaces of the upper and lower porcelain bushing blanks, wherein the coating thickness of the bonding glaze is 0.5-1.0 mm, and removing the redundant bonding glaze extruded from the connecting end surfaces;
p2, loading the bonded porcelain bushing blank into a kiln, heating the kiln to 300-400 ℃ from room temperature at a speed of 5 ℃/min, and then keeping the temperature for 2 hours; heating to 700-800 ℃ at the speed of 0.5 ℃/min, and then keeping the temperature for 2-3 hours; heating to 1120-1200 deg.c at the speed of 10 deg.c/min, maintaining for 5-7 hr, and naturally cooling to room temperature.
Further, the porcelain bushing blank body is composed of the following raw materials in percentage by mass: 20-30% of calcined bauxite, 25-35% of kaolin, 10-15% of method mud, 5-10% of bentonite, 5-8% of talcum powder, 2-3% of magnesium oxide, 3-5% of titanium dioxide, 4-7% of yttrium oxide and 6-10% of zirconium oxide;
the preparation method of the porcelain bushing blank comprises the following steps: weighing the raw materials of the porcelain bushing blank, uniformly mixing, and then mixing the mixture, the ball stone and water according to the mass ratio of 1:3:2, placing the mixture in a ball mill according to the mass ratio, ball milling for 40 hours, and sieving to remove iron to prepare slurry; removing water in the slurry to 10-15% by using a filter press, aging for 48 hours, and then extruding and forming to obtain a blank; naturally drying in shade for 48h, then placing in a sintering furnace for presintering, heating to 600-700 ℃ at the normal temperature at the speed of 10 ℃/min, and preserving heat for 3-4 h to obtain the porcelain bushing blank.
The invention has the following beneficial effects:
1. the modifier is ZrSiO compounded by ethyl orthosilicate, zirconium n-butoxide, 3-trichlorogermanium propionic acid and tetrabutyl orthotitanate by adopting a sol-gel method 4 -TiO 2 -GeO 2 The compound reduces the sintering temperature of the bonding glaze, ensures that the bonding glaze has good high-temperature fluidity, precipitates crystals in the bonding sintering process, improves the strength of the bonding glaze, thereby improving the bonding strength between porcelain sleeves, and also ensures that the surface of the bonding glaze has uniform color, no chromatic aberration, bright color and bright luster and improves the weather resistance of the invention; the invention adopts sol-gel method to make ZrSiO 4 、TiO 2 And GeO 2 The cost is reduced by compounding, and the particle size of the modifier is smaller and can reach below micron level by adding the surfactant polyvinylpyrrolidone while controlling the uniform compounding of three substances; the addition of lithium chloride greatly reduces the crystallization temperature of zirconium silicate, so that ZrSiO 4 -TiO 2 -GeO 2 The compound can obtain a crystalline phase compound at a lower sintering temperature; the invention uses ZrSiO 4 、TiO 2 And GeO 2 Three substances passing through organic matterThe three substances can be added into the bonding glaze simultaneously by adopting a sol-gel method to synthesize the three substances, so that the three substances can be dispersed in the bonding glaze more conveniently and uniformly, bubbles are avoided at high temperature, the porosity is reduced, and the strength and toughness of the bonding glaze are further improved.
2. The bonding glaze and the modifier are matched to ensure that the expansion coefficient of the bonding glaze is similar to that of the porcelain bushing blank in the invention, and residual stress is avoided, so that the bonding glaze is bonded with the high-strength porcelain bushing in high-temperature sintering, is more complete in mutual penetration and more firm in bonding, is more favorable for forming a porcelain glaze intermediate layer, and has stronger bonding strength and breaking strength.
3. The micro aluminum powder is added, so that the micro aluminum powder is melted into a liquid state in the high-temperature sintering process, namely at about 600 ℃, and air holes in the slurry are filled, and a dispersed crystalline phase is bonded, so that the bonding glaze is oxidized in the sintering process, the bonding glaze is more densified, and the strength of the bonding glaze is further enhanced; because the grain diameter of the micro aluminum powder is small and the melting point is low, the micro aluminum powder is easy to permeate into the porcelain bushing blank in the sintering process, and the bonding strength between the bonding glaze and the porcelain bushing is improved.
4. The invention adds the Uozhou soil, which has less impurity, soft quality, good plasticity, and is sintered at a lower temperature, does not affect the whiteness of the bonding glaze, and is added into the glaze according to a proper proportion, so that the bonding glaze can better present different colors, the whiteness of the sintered glaze is enhanced, the density is uniform, the color is bright, the surface is not easy to crack, and the bonding glaze has better bonding strength and bonding force.
5. The addition of wollastonite reduces the sintering temperature of the bonding glaze, reduces the cracks and warpage of the glaze, increases the glossiness of the glaze, improves the strength of the glaze, and ensures that the bonding glaze has better stain resistance and weather resistance.
6. The porcelain bushing is aluminum porcelain and has excellent mechanical strength, high and low temperature resistance, insulativity, weather resistance, ageing resistance and the like. The magnesia can generate liquid phase with alumina in the bonding glaze in the high-temperature sintering process, so that the bonding force and compactness of each component are enhanced, the mechanical strength and toughness of the bonding glaze are improved, the bonding glaze and the porcelain sleeve are tightly combined, and the bonding strength of the product is improved; the yttrium oxide is easy to form a liquid phase with silicon oxide in the high-temperature sintering process, so that the compactness of the porcelain bushing can be improved, the mechanical strength of the porcelain bushing can be improved, and the binding force with the bonding glaze component can be improved; in the sintering process of zirconia, the crystallization of the porcelain bushing is promoted, so that the strength of the porcelain bushing is improved; the addition of bentonite and method warehouse mud improves the bonding force of the porcelain bushing and the bonding glaze, so that the porcelain bushing and the bonding glaze are easy to combine in the bonding process, and the subsequent high-temperature sintering is convenient.
7. In the application process of the bonding glaze, the bonding glaze adopts a step heating sintering method, and is heated to 700-800 ℃ at a lower heating rate, so that the generation of air holes is reduced as much as possible, the gas of the product is discharged, the porosity of the glaze layer and the porcelain sleeve is reduced, and the bonding strength, the mechanical strength and the toughness of the product are improved; after the porcelain bushing blank body is presintered, the porcelain bushing blank body and the bonding glaze material are directly sintered together at high temperature, so that the cost is reduced, the contact area of the porcelain bushing blank body and the bonding glaze material at the bonding interface is increased, and the bonding effect of the product is further improved.
8. According to the invention, the raw materials such as potassium feldspar powder, quartz powder, kaolin, micro aluminum powder, cooked talcum powder, uozhou soil, lawn field mud washing and wollastonite are used as bonding glaze, so that the glaze has small thermal expansion coefficient and internal stress and good plasticity, so that the glaze has excellent mechanical strength, toughness and self-lubricity, and has excellent weather resistance and hydrophobicity; the invention is ZrSiO 4 -TiO 2 -GeO 2 The compound is matched with basic glaze for use, so that the glaze has bright color, high bonding strength and good mechanical property, and the service life of porcelain bushing products is prolonged. The invention has the advantages of easily available raw materials, simple process, lower cost and easy industrialized popularization.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The micro aluminum powder of the invention is from micro spherical aluminum powder JT-5 (1-2 μm) provided by Hunan today aluminum industry high tech Co.
The bonding glaze of the present invention will be described with reference to specific examples.
Example 1
The bonding glaze consists of a basic glaze, a modifier and a pigment, wherein the basic glaze consists of the following raw materials in percentage by weight: 10% of potassium feldspar powder, 15% of quartz powder, 25% of kaolin, 5% of micro aluminum powder, 5% of cooked talcum powder, 10% of Uozhou soil, 15% of lawn soil washing mud and 15% of wollastonite.
The modifier in this embodiment is ZrSiO 4 -TiO 2 -GeO 2 The preparation method of the compound comprises the following steps:
(1) 31.2 parts of tetraethoxysilane is added into 187.5ml of 40wt% ethanol solution, 62.5ml of 2mol/L hydrochloric acid is added, stirring is carried out for 0.5h, 38.4 parts of zirconium n-butoxide and 0.2 part of lithium chloride are added, stirring is carried out for 1h, heating is carried out to 70 ℃ and stirring reaction is carried out for 15min, transparent sol is formed, cooling is carried out to room temperature, stirring is carried out for 1h again, and zirconium silicate precursor gel is formed;
(2) Adding 7.5 parts of 3-trichlorogermanium propionic acid and 6.8 parts of tetrabutyl orthotitanate into 28.7 parts of 30wt% ethanol solution, uniformly stirring, adding the mixture into the zirconium silicate precursor gel, adding 1.4 parts of polyvinylpyrrolidone, uniformly mixing, and stirring at 85 ℃ for 2 hours to prepare a gel mixture;
(3) Stirring the gel mixture at 135 ℃ for reaction for 5 hours, cooling to room temperature, then washing with absolute ethyl alcohol, and then preserving heat for 4 hours at 700 ℃ to obtain ZrSiO 4 -TiO 2 -GeO 2 A complex. The ZrSiO 4 -TiO 2 -GeO 2 The addition amount of the compound is 2% of the total mass of the basic glaze.
In this example 1, the adhesive glaze is a gray blue glaze, and the color material has the following components in mass ratio of 1:1.8 lead oxide and cobalt oxide; the addition amount of the pigment is 2.8% of the total mass of the basic glaze.
The gray blue bonding glaze is used for bonding porcelain sleeves, and the preparation method specifically comprises the following steps:
s1, weighing the basic glaze, uniformly mixing, placing in a smelting furnace, heating to 1320 ℃, preserving heat for 3 hours, and then performing water quenching to obtain the basic glaze;
s2, weighing the modifier and the pigment according to the above, then adding the modifier and the pigment into the basic frit glaze, uniformly mixing to obtain a glaze mixture, and then mixing the glaze mixture, the ball stone and water according to the mass ratio of 1:1:0.8 is put into a ball mill for ball milling for 35 hours;
s3, deironing the glaze slurry of the ball mill by using an iron removing machine, sieving the glaze slurry by using a 250 mesh sieve, ageing the glaze slurry for 72 hours, adjusting the moisture (25+/-0.5)%, and measuring the fluidity by using a viscometer for 58+/-2 seconds to obtain a bonding glaze;
s4, coating bonding glaze on the connecting end faces of the upper and lower porcelain bushing blanks, wherein the coating thickness of the bonding glaze is 0.8mm, and removing redundant bonding glaze extruded from the connecting end faces;
s5, loading the bonded porcelain bushing blank into a kiln, heating the kiln to 400 ℃ from room temperature at a speed of 5 ℃/min, and then keeping the temperature for 2 hours; heating to 700 ℃ at a speed of 0.5 ℃/min, and then keeping the temperature for 3 hours; heating to 1150 ℃ at the speed of 10 ℃/min, keeping the temperature for 6 hours, and naturally cooling to room temperature.
The porcelain bushing blank consists of the following raw materials in percentage by mass: 20% of calcined bauxite, 35% of kaolin, 10% of Faku mud, 10% of bentonite, 5% of talcum powder, 2% of magnesium oxide, 5% of titanium dioxide, 7% of yttrium oxide and 6% of zirconium oxide, and the preparation method comprises the following steps:
weighing the raw materials of the porcelain bushing blank, uniformly mixing, and then mixing the mixture, the ball stone and water according to the mass ratio of 1:3:2, placing the mixture in a ball mill according to the mass ratio, ball milling for 40 hours, and sieving to remove iron to prepare slurry; removing water in the slurry to 10-15% by using a filter press, aging for 48 hours, and then extruding and forming to obtain a blank; naturally drying in the shade for 48 hours, then placing in a sintering furnace for presintering, heating to 700 ℃ at the speed of 10 ℃/min at normal temperature, and preserving heat for 4 hours to obtain the porcelain bushing blank.
Example 2
The bonding glaze consists of a basic glaze, a modifier and a pigment, wherein the basic glaze consists of the following raw materials in percentage by weight: 20% of potassium feldspar powder, 20% of quartz powder, 15% of kaolin, 3% of micro-aluminum powder, 6% of cooked talcum powder, 6% of Uozhou soil, 10% of lawn soil washing mud and 20% of wollastonite.
The modifier in this embodiment is ZrSiO 4 -TiO 2 -GeO 2 The preparation method of the compound comprises the following steps:
(1) Adding 37.5 parts of tetraethoxysilane into 225mL of 40wt% ethanol solution, adding 75mL of 2mol/L hydrochloric acid, stirring for 0.5h, adding 38.4 parts of zirconium n-butoxide and 0.3 part of lithium chloride, stirring for 1h, heating to 70 ℃ and stirring for reaction for 15min to form transparent sol, cooling to room temperature, and continuing stirring for 1h to form zirconium silicate precursor gel;
(2) Adding 6.5 parts of 3-trichlorogermanium propionic acid and 8.8 parts of tetrabutyl orthotitanate into 30.6 parts of 30wt% ethanol solution, uniformly stirring, adding the mixture into the zirconium silicate precursor gel, adding 1.5 parts of polyvinylpyrrolidone, uniformly mixing, and stirring at 85 ℃ for 2 hours to prepare a gel mixture;
(3) Stirring the gel mixture at 135 ℃ for reaction for 5 hours, cooling to room temperature, then washing with absolute ethyl alcohol, and then preserving heat for 4 hours at 700 ℃ to obtain ZrSiO 4 -TiO 2 -GeO 2 A complex. The ZrSiO 4 -TiO 2 -GeO 2 The addition amount of the compound is 2% of the total mass of the basic glaze.
In this example 1, the adhesive glaze is a gray blue glaze, and the color material has a mass ratio of 3:4 lead oxide and cobalt oxide; the addition amount of the pigment is 2.1% of the total mass of the basic glaze.
The gray blue bonding glaze is used for bonding porcelain sleeves, and the preparation method is the same as that in the embodiment 1, and the embodiment 1 is specifically referred to.
The porcelain bushing blank in the embodiment is composed of the following raw materials in percentage by mass: 30% of calcined bauxite, 25% of kaolin, 15% of process mud, 5% of bentonite, 7% of talcum powder, 3% of magnesium oxide, 3% of titanium dioxide, 4% of yttrium oxide and 8% of zirconium oxide, and the preparation method is the same as that in the example 1, and the specific reference is made to the example 1.
Example 3
The bonding glaze consists of a basic glaze, a modifier and a pigment, wherein the basic glaze consists of the following raw materials in percentage by weight: 15% of potassium feldspar powder, 15% of quartz powder, 16% of kaolin, 5% of micro aluminum powder, 4% of cooked talcum powder, 5% of Uozhou soil, 15% of lawn soil washing mud and 25% of wollastonite.
The modifier in this embodiment is ZrSiO 4 -TiO 2 -GeO 2 The preparation method of the compound comprises the following steps:
(1) Adding 33.3 parts of tetraethoxysilane into 200mL of 40wt% ethanol solution, adding 67mL of 2mol/L hydrochloric acid, stirring for 0.5h, adding 38.4 parts of zirconium n-butoxide and 0.3 part of lithium chloride, stirring for 1h, heating to 70 ℃ and stirring for reaction for 15min to form transparent sol, cooling to room temperature, and continuing stirring for 1h to form zirconium silicate precursor gel;
(2) Adding 6.9 parts of 3-trichlorogermanium propionic acid and 8.5 parts of tetrabutyl orthotitanate into 30.8 parts of 30wt% ethanol solution, uniformly stirring, adding the mixture into the zirconium silicate precursor gel, adding 1.5 parts of polyvinylpyrrolidone, uniformly mixing, and stirring at 85 ℃ for 2 hours to prepare a gel mixture;
(3) Stirring the gel mixture at 135 ℃ for reaction for 5 hours, cooling to room temperature, then washing with absolute ethyl alcohol, and then preserving heat for 4 hours at 700 ℃ to obtain ZrSiO 4 -TiO 2 -GeO 2 A complex. The ZrSiO 4 -TiO 2 -GeO 2 The addition amount of the compound is 2.5% of the total mass of the basic glaze.
In this example 1, the adhesive glaze is a gray blue glaze, and the color material has the following components in mass ratio of 1:1.5 lead oxide and cobalt oxide; the addition amount of the pigment is 2.5% of the total mass of the basic glaze.
The gray blue bonding glaze is used for bonding porcelain sleeves, and the preparation method is the same as that in the embodiment 1, and the embodiment 1 is specifically referred to.
The porcelain bushing blank in the embodiment is composed of the following raw materials in percentage by mass: 25% of calcined bauxite, 30% of kaolin, 12% of Faku mud, 8% of bentonite, 7% of talcum powder, 2% of magnesium oxide, 4% of titanium dioxide, 5% of yttrium oxide and 7% of zirconium oxide, and the preparation method is the same as that in the example 1, and the specific reference is to the example 1.
Example 4
The bonding glaze consists of a basic glaze, a modifier and a pigment, wherein the basic glaze consists of the following raw materials in percentage by weight: 18% of potassium feldspar powder, 17% of quartz powder, 20% of kaolin, 4% of micro-aluminum powder, 5% of cooked talcum powder, 5% of Uozhou soil, 15% of lawn soil washing mud and 16% of wollastonite.
The modifier in this embodiment is ZrSiO 4 -TiO 2 -GeO 2 The preparation method of the compound is the same as that in the example 3, and the specific reference is made to the example 3. The ZrSiO 4 -TiO 2 -GeO 2 The addition amount of the compound is 1.6% of the total mass of the basic glaze.
In this example 1, the adhesive glaze is a gray blue glaze, and the color material has the following components in mass ratio of 1:2 lead oxide and cobalt oxide; the addition amount of the pigment is 3% of the total mass of the basic glaze.
The gray blue bonding glaze is used for bonding porcelain sleeves, and the preparation method is the same as that in the embodiment 1, and the embodiment 1 is specifically referred to.
The porcelain bushing blank in the embodiment is composed of the following raw materials in percentage by mass: 22% of calcined bauxite, 28% of kaolin, 15% of process mud, 7% of bentonite, 6% of talcum powder, 2% of magnesium oxide, 4% of titanium dioxide, 6% of yttrium oxide and 10% of zirconium oxide, and the preparation method is the same as that in the example 1, and the specific reference is made to the example 1.
Example 5
The bonding glaze consists of a basic glaze, a modifier and a pigment, wherein the basic glaze consists of the following raw materials in percentage by weight: 17% of potassium feldspar powder, 15% of quartz powder, 15% of kaolin, 4% of micro aluminum powder, 4% of cooked talcum powder, 10% of Uozhou soil, 20% of lawn soil washing mud and 15% of wollastonite.
The modifier in this embodiment is ZrSiO 4 -TiO 2 -GeO 2 The preparation method of the compound is the same as that in the example 3, and the specific reference is made to the example 3. The ZrSiO 4 -TiO 2 -GeO 2 The addition amount of the compound is 2.1 percent of the total mass of the basic glaze.
In this example 1, the adhesive glaze is a gray blue glaze, and the color material has a mass ratio of 3:7 lead oxide and cobalt oxide; the addition amount of the pigment is 3% of the total mass of the basic glaze.
The gray blue bonding glaze is used for bonding porcelain sleeves, and the preparation method is the same as that in the embodiment 1, and the embodiment 1 is specifically referred to.
The porcelain bushing blank in the embodiment is composed of the following raw materials in percentage by mass: 27% of calcined bauxite, 31% of kaolin, 13% of Faku mud, 5% of bentonite, 5% of talcum powder, 3% of magnesium oxide, 5% of titanium dioxide, 5% of yttrium oxide and 6% of zirconium oxide, and the preparation method is the same as that in the example 1, and the specific reference is made to the example 1.
Comparative example 1
The comparative example is a gray blue bonding glaze, the raw material components and the preparation method are the same as those in the example 4, and the preparation process of the gray blue bonding glaze for bonding the porcelain bushing is also the same as that in the example 4, and the specific reference is made to the example 4. In contrast, the modifier in comparative example 1 was ZrSiO 4 、TiO 2 And GeO 2 The mole ratio of Zr, ti and Ge in the modifier is 1:1:1, wherein the addition amount of the modifier mixture is 1.6% of the total mass of the basic glaze.
Comparative example 2
The comparative example is a gray blue bonding glaze, the raw material components and the preparation method are the same as those in the example 4, and the preparation process of the gray blue bonding glaze for bonding the porcelain bushing is also the same as that in the example 4, and the specific reference is made to the example 4. The difference is that the basic glaze of the comparative example 2 does not contain micro aluminum powder, namely the basic glaze consists of the following raw materials in percentage by weight: 18% of potassium feldspar powder, 17% of quartz powder, 24% of kaolin, 5% of cooked talcum powder, 5% of Unzhou soil, 15% of lawn soil washing mud and 16% of wollastonite.
Comparative example 3
The comparative example is a gray blue bonding glaze, the raw material components and the preparation method are the same as those in the example 4, and the preparation process of the gray blue bonding glaze for bonding the porcelain bushing is also the same as that in the example 4, and the specific reference is made to the example 4. The difference is that bentonite is not added into the porcelain bushing blank of the comparative example 3, and the porcelain bushing blank consists of the following raw materials in percentage by mass: 22% of calcined bauxite, 28% of kaolin, 22% of method mud, 6% of talcum powder, 2% of magnesium oxide, 4% of titanium dioxide, 6% of yttrium oxide and 10% of zirconium oxide.
Comparative example 4
The comparative example is a gray blue bonding glaze, the raw material components and the preparation method are the same as those in the example 4, and the preparation process of the gray blue bonding glaze for bonding the porcelain bushing is also the same as that in the example 4, and the specific reference is made to the example 4. The difference is that the preparation method of the porcelain bushing blank in the comparative example 4 is as follows: weighing the raw materials of the porcelain bushing blank, uniformly mixing, and then mixing the mixture, the ball stone and water according to the mass ratio of 1:3:2, placing the mixture in a ball mill according to the mass ratio, ball milling for 40 hours, and sieving to remove iron to prepare slurry; removing water in the slurry to 10-15% by using a filter press, aging for 48 hours, and then extruding and forming to obtain a blank; naturally drying in shade for 48h, then placing in a sintering furnace for presintering, heating to 1300 ℃ at the speed of 10 ℃/min at normal temperature, and preserving heat for 6h to obtain the porcelain bushing blank.
Comparative example 5
The comparative example is a gray blue bonding glaze, the raw material components and the preparation method are the same as those in the example 4, and the preparation process of the gray blue bonding glaze for bonding the porcelain bushing is also the same as that in the example 4, and the specific reference is made to the example 4.
The difference is that, in the preparation process of the gray blue bonding glaze for bonding the porcelain bushing in the comparative example 5, the step S5 is as follows: loading the bonded porcelain bushing blank into a kiln, heating from room temperature to 400 ℃ at a speed of 5 ℃/min, and keeping the temperature for 2 hours; heating to 700 ℃ at a speed of 5 ℃/min, and then keeping the temperature for 3 hours; heating to 1150 ℃ at the speed of 10 ℃/min, keeping the temperature for 6 hours, and naturally cooling to room temperature.
Comparative example 6
This comparative example is a porcelain bushing using no bonding glaze, the raw material composition of which is the same as in example 4, and specifically reference is made to example 4. The preparation method of the porcelain bushing in the comparative example 6 comprises the following steps:
(1) Weighing the raw materials of the porcelain bushing blank, uniformly mixing, and then mixing the mixture, the ball stone and water according to the mass ratio of 1:3:2, placing the mixture in a ball mill according to the mass ratio, ball milling for 40 hours, and sieving to remove iron to prepare slurry; removing water in the slurry to 10-15% by using a filter press, aging for 48 hours, and then extruding and forming to obtain a blank; naturally drying in the shade for 48 hours, then placing in a sintering furnace for presintering, heating to 700 ℃ at the speed of 10 ℃/min at normal temperature, and preserving heat for 4 hours to obtain the porcelain bushing blank.
(2) The porcelain bushing blank is put into a kiln, and is heated to 400 ℃ from room temperature at a speed of 5 ℃/min and then kept at the constant temperature for 2 hours; heating to 700 ℃ at a speed of 0.5 ℃/min, and then keeping the temperature for 3 hours; heating to 1150 ℃ at the speed of 10 ℃/min, keeping the temperature for 6 hours, and naturally cooling to room temperature.
The porcelain bushings in examples 1 to 5 and comparative examples 1 to 6 were made into electric porcelain strips for convenience in performance, i.e., the coating thickness of the bonding glaze was modified to 0.2mm, and the performance of bonding the electric porcelain strips and the electric porcelain strips was examined, and the examination results are shown in table 1 below.
TABLE 1 results of testing the properties of bonded electroceramics
Remarks: the average linear expansion coefficient and porosity of the bonding frit at 25℃to 400℃were measured in examples 1 to 5 and comparative examples 1, 2 and 5, and the average linear expansion coefficient and porosity of the porcelain bushing at 25℃to 400℃were measured in comparative examples 3, 4 and 6.
As can be seen from the results in Table 1, after the two sections of porcelain sleeves are bonded by the bonding glaze, the bonding glaze has full appearance, bright luster and uniform color, and the flexural strength of the bonding porcelain sleeve is improved by at least 15% compared with that of the bonding porcelain sleeve without bonding, which indicates that the bonding glaze has excellent mechanical strength and bonding effect. The bonding porcelain bushing has excellent fracture toughness and lower porosity, and the expansion coefficient of the bonding layer is similar to that of the porcelain bushing.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (7)
1. The bonding glaze consists of a basic glaze, a modifier and a pigment, and is characterized by comprising the following raw materials in percentage by weight: 10 to 20 percent of potassium feldspar powder, 15 to 20 percent of quartz powder, 15 to 25 percent of kaolin, 3 to 5 percent of micro aluminum powder, 4 to 6 percent of cooked talcum powder, 5 to 10 percent of Uozhou soil, 10 to 20 percent of lawn field mud washing and 15 to 25 percent of wollastonite;
the addition amount of the modifier is 1.6-2.5% of the total mass of the basic glaze, and the modifier is ZrSiO 4 -TiO 2 - GeO 2 A complex;
the ZrSiO 4 -TiO 2 - GeO 2 The preparation method of the compound specifically comprises the following steps:
(1) Adding a certain amount of tetraethoxysilane into 40wt% ethanol solution, adding 2mol/L hydrochloric acid, stirring for 0.5h, adding zirconium n-butoxide and lithium chloride, stirring for 1h, heating to 60-70 ℃ and stirring for reaction for 10-20 min to form transparent sol, cooling to room temperature, and continuing stirring for 1h to form zirconium silicate precursor gel;
(2) Adding 3-trichlorogermanopropionic acid and tetrabutyl orthotitanate into 30wt% ethanol solution, stirring uniformly, adding the mixture into the zirconium silicate precursor gel, adding a surfactant, mixing uniformly, and stirring at 80-90 ℃ for 1-2h to obtain a gel mixture;
(3) Stirring the gel mixture at 130-140 ℃ for reaction for 4-6 hours, cooling to room temperature, then washing with absolute ethyl alcohol, and then preserving heat for 4 hours at 700 ℃ to obtain ZrSiO 4 -TiO 2 - GeO 2 A complex;
the pigment is high-temperature pigment oxide.
2. The bonding glaze according to claim 1, wherein the particle diameter of the micro aluminum powder is 1 to 20 μm.
3. The bonding glaze according to claim 1, wherein in said step (1), the molar ratio of Si to Zr in said tetraethyl orthosilicate and said zirconium n-butoxide is (1.5 to 1.8): 1, wherein the molar ratio of Li to Zr in the lithium chloride to the zirconium n-butoxide is (0.05-0.08): 1, the ratio of Si in the ethyl orthosilicate to 40wt% ethanol solution is 0.8mol/L, and the volume ratio of the 40wt% ethanol solution to the hydrochloric acid is 3:1.
4. the bonding glaze according to claim 1, wherein in said step (2), the molar ratio of Ge in said 3-trichlorogermanopropionic acid to Zr in said zirconium silicate precursor gel is (0.3-0.35): 1, a step of; the molar ratio of Ti in the tetrabutyl orthotitanate to Zr in the zirconium silicate precursor gel is (0.2-0.26): 1, a step of; the addition amount of the 30wt% ethanol solution is 2 times of the total mass of the 3-trichlorogermanium propionic acid and tetrabutyl orthotitanate.
5. The bonding frit according to claim 1, wherein the surfactant is polyvinylpyrrolidone.
6. A process for preparing a bonding glaze according to any one of claims 1 to 5, comprising the steps of:
s1, weighing a basic glaze according to the requirement, uniformly mixing, placing in a smelting furnace, heating to 1300-1350 ℃, preserving heat for 2-3h, and then performing water quenching to obtain a basic frit glaze;
s2, weighing the modifier and the pigment according to the requirements, then adding the modifier and the pigment into the basic frit glaze, uniformly mixing to obtain a glaze mixture, and then mixing the glaze mixture, the ball stone and water according to the mass ratio of 1:1:0.8 is put into a ball mill, and ball milling is carried out for 30-35 hours;
and S3, deironing the glaze slurry of the ball mill by using an iron removing machine, sieving the glaze slurry by using a 250 mesh sieve, ageing the glaze slurry for 72 hours, adjusting the moisture of the glaze slurry to be 25+/-0.5%, and measuring the fluidity by using a viscometer for 58+/-2 seconds to obtain the bonding glaze.
7. The method for producing a bonding glaze according to claim 6, comprising the steps of:
p1, coating the bonding glaze on the connecting end surfaces of the upper and lower porcelain bushing blanks, wherein the coating thickness of the bonding glaze is 0.5-1.0 mm, and removing the redundant bonding glaze extruded from the connecting end surfaces;
p2, loading the bonded porcelain bushing blank into a kiln, heating the kiln to 300-400 ℃ from room temperature at a speed of 5 ℃/min, and then keeping the temperature for 2 hours; heating to 700-800 ℃ at the speed of 0.5 ℃/min, and then keeping the temperature for 2-3 hours; heating to 1120-1200 ℃ at a speed of 10 ℃/min, keeping the temperature for 5-7 hours, and naturally cooling to room temperature;
the porcelain bushing blank body is composed of the following raw materials in percentage by mass: 20-30% of calcined bauxite, 25-35% of kaolin, 10-15% of method mud, 5-10% of bentonite, 5-8% of talcum powder, 2-3% of magnesium oxide, 3-5% of titanium dioxide, 4-7% of yttrium oxide and 6-10% of zirconium oxide;
the preparation method of the porcelain bushing blank comprises the following steps: weighing the raw materials of the porcelain bushing blank, uniformly mixing, and then mixing the mixture, the ball stone and water according to the mass ratio of 1:3:2, placing the mixture in a ball mill according to the mass ratio, ball milling for 40 hours, and sieving to remove iron to prepare slurry; removing water in the slurry to 10-15% by using a filter press, aging for 48 hours, and then extruding and forming to obtain a blank; naturally drying in shade for 48h, then placing in a sintering furnace for presintering, heating to 600-700 ℃ at the normal temperature at the speed of 10 ℃/min, and preserving heat for 3-4 h to obtain the porcelain bushing blank.
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| DE2065262A1 (en) * | 1969-10-11 | 1973-07-05 | Ngk Insulators Ltd | SEMI-CONDUCTIVE GLAZING MIXTURE AND PROCESS FOR THE PREPARATION |
| CN107129151A (en) * | 2017-07-06 | 2017-09-05 | 高慧芹 | Anion function ceramic tile glaze and preparation method thereof |
| CN108658466A (en) * | 2018-05-24 | 2018-10-16 | 醴陵华鑫电瓷科技股份有限公司 | A kind of inorganic adhesive glaze and the insulator sleeve adhesion method using the glaze |
| CN110357434A (en) * | 2019-08-09 | 2019-10-22 | 西安西电高压电瓷有限责任公司 | A kind of dusty blue inorganic adhesive glaze and the preparation method and application thereof |
| CN114804634A (en) * | 2022-03-04 | 2022-07-29 | 醴陵市东方电瓷电器有限公司 | Colored glaze for porcelain insulator and preparation method thereof |
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- 2022-08-31 CN CN202211051509.XA patent/CN115448597B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2065262A1 (en) * | 1969-10-11 | 1973-07-05 | Ngk Insulators Ltd | SEMI-CONDUCTIVE GLAZING MIXTURE AND PROCESS FOR THE PREPARATION |
| CN107129151A (en) * | 2017-07-06 | 2017-09-05 | 高慧芹 | Anion function ceramic tile glaze and preparation method thereof |
| CN108658466A (en) * | 2018-05-24 | 2018-10-16 | 醴陵华鑫电瓷科技股份有限公司 | A kind of inorganic adhesive glaze and the insulator sleeve adhesion method using the glaze |
| CN110357434A (en) * | 2019-08-09 | 2019-10-22 | 西安西电高压电瓷有限责任公司 | A kind of dusty blue inorganic adhesive glaze and the preparation method and application thereof |
| CN114804634A (en) * | 2022-03-04 | 2022-07-29 | 醴陵市东方电瓷电器有限公司 | Colored glaze for porcelain insulator and preparation method thereof |
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