CN110950537A - Preparation method of low-expansion low-temperature environment-friendly glass glaze - Google Patents
Preparation method of low-expansion low-temperature environment-friendly glass glaze Download PDFInfo
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- CN110950537A CN110950537A CN201811133894.6A CN201811133894A CN110950537A CN 110950537 A CN110950537 A CN 110950537A CN 201811133894 A CN201811133894 A CN 201811133894A CN 110950537 A CN110950537 A CN 110950537A
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- glaze
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- temperature environment
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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
- C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3644—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the metal being silver
-
- 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
Abstract
The invention discloses a preparation method of low-expansion low-temperature environment-friendly glass glaze, which comprises the following steps: preparing materials; mixing and grinding, and performing dry ball milling for 6H; sintering a frit, namely putting the ball-milled material in the step (2) into a frit furnace for melting, keeping the temperature for 20min at the melting temperature of 1000-1050 ℃, and performing water quenching; preparing glass powder and drying; preparing glaze, namely mixing 60wt% of the glass powder in the step (4) with 40wt% of an organic carrier, and then ball-milling the mixture of the glass powder and the organic carrier for 2H; printing; firing the glaze; and (6) detecting the appearance. The preparation method of the low-expansion low-temperature environment-friendly glass glaze ensures that the glass glaze is stably placed at a certain temperature, improves the overall stability of the glass glaze, is convenient for not polluting the environment in the preparation process of the glass glaze, improves the environmental protection performance of the glass glaze, further improves the quality of the whole glass glaze, is convenient for picking out unqualified glass glaze, reduces the defective rate of the whole glass glaze production, and has good market value.
Description
Technical Field
The invention relates to a preparation method of a low-expansion low-temperature environment-friendly glass glaze, in particular to a preparation method of a low-expansion low-temperature environment-friendly glass glaze, and belongs to the technical field of glass glaze processing and application.
Background
After the surface of the high borosilicate glass is metallized, a glass glaze layer is coated to protect the high borosilicate glass from metal oxidation. The high borosilicate glass has the 'double low' characteristics (the thermal expansion coefficient is 3.3 multiplied by 10 < -6 >, the heat-resisting temperature is 600 ℃) and puts severe requirements on the glass glaze.
Most of the existing low-temperature glaze formulas adopt potassium, albite, bismuth systems, lead systems and the like, but the thermal expansion coefficient of the glaze is often larger (more than or equal to 8 multiplied by 10 < -6 >) or does not meet the requirement of environmental protection; the formula with low expansion coefficient mostly adopts high silicon, high aluminum and the like, but the melting point is higher (more than or equal to 650 ℃), the heat-resistant temperature of the high borosilicate glass is exceeded, and the requirement of double low of the high borosilicate glass is difficult to meet. Therefore, a preparation method of the low-expansion low-temperature environment-friendly glass glaze is provided for solving the problems.
Disclosure of Invention
The invention aims to solve the problems and provide a preparation method of a low-expansion low-temperature environment-friendly glass glaze.
The invention realizes the aim through the following technical scheme, and provides a preparation method of a low-expansion low-temperature environment-friendly glass glaze, which comprises the following steps:
(1) preparing materials according to Bi2O 340 wt-50 wt%, SiO 25 wt-15 wt%, Al2O 30 wt-3 wt%, ZnO 5-10 wt%, B2O 310 wt-20 wt%, Li2O 3-10 wt%, MgO 0-5 wt%, CaO 0-5 wt% and BaO0 wt-5 wt%, wherein the granularity of each raw material is controlled to be less than 10 μm;
(2) mixing and grinding, namely putting the material in the step (1) into a ball mill, and performing dry ball milling for 6H;
(3) sintering a frit, namely putting the ball-milled material in the step (2) into a frit furnace for melting, keeping the temperature for 20min at the melting temperature of 1000-1050 ℃, and performing water quenching;
(4) preparing glass powder, namely performing ball milling on the fired frit in the step (3) by using a wet ball mill, controlling the particle size of the powder to be less than 3 mu m, and drying;
(5) preparing glaze, namely mixing 60wt% of the glass powder in the step (4) with 40wt% of an organic carrier, and then ball-milling the mixture of the glass powder and the organic carrier for 2H;
(6) printing, namely screen-printing on a metal silver surface (the silver surface is covered on the surface of a high borosilicate 3.3 glass substrate), wherein the thickness of a glaze layer is 20-30 mu m;
(7) firing glaze, wherein the firing glaze temperature is 550-580 ℃, preserving heat for 5min, and finally cooling the heat preserved glaze to below 100 ℃ along with a furnace, and then discharging the glaze from the furnace;
(8) and (5) detecting the appearance, observing cracks of the glaze surface through a 100X microscope, and removing the unqualified fired glaze.
Preferably, the mixed milling in the step (2) is performed by using a dry ball mill, and the mixed milling time is 6H.
Preferably, the particle size of the glass powder in the step (4) is less than 3 μm.
Preferably, in the step (5), 60wt% of the glass powder and 40wt% of the organic vehicle are stirred uniformly by a known stirring device, and then glaze preparation is performed.
Preferably, in the step (3), the clinker is quenched by using water as a quenching agent, and the clinker is put into water, then is heated by burning, and then is put into water, and the above steps are repeated, so that the rigidity is improved.
Preferably, the powder material ball-milled in the step (4) is placed into a special dryer for glass powder to be dried.
The invention has the beneficial effects that: the preparation method of the low-expansion low-temperature environment-friendly glass glaze ensures that the glass glaze is stably placed at a certain temperature, improves the overall stability of the glass glaze, is convenient for not polluting the environment in the preparation process of the glass glaze, improves the environmental protection performance of the glass glaze, further improves the quality of the whole glass glaze, is convenient for picking out unqualified glass glaze, reduces the defective rate of the whole glass glaze production, and has good market value.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a preparation method of a low-expansion low-temperature environment-friendly glass glaze comprises the following steps:
(1) preparing materials according to Bi2O 345 wt-50 wt%, SiO 27 wt-15 wt%, Al2O 31 wt-3 wt%, ZnO 2-10 wt%, B2O 312 wt-20 wt%, Li2O 4-10 wt%, MgO 1-5 wt%, CaO 1-5 wt% and BaO1 wt-5 wt%, wherein the granularity of each raw material is controlled to be less than 10 mu m;
(2) mixing and grinding, namely putting the material in the step (1) into a ball mill, and performing dry ball milling for 6H;
(3) sintering a frit, namely putting the ball-milled material in the step (2) into a frit furnace for melting, keeping the temperature for 20min at the melting temperature of 1010-1050 ℃, and performing water quenching;
(4) preparing glass powder, namely performing ball milling on the fired frit in the step (3) by using a wet ball mill, controlling the particle size of the powder to be less than 3 mu m, and drying;
(5) preparing glaze, namely mixing 60wt% of the glass powder in the step (4) with 40wt% of an organic carrier, and then ball-milling the mixture of the glass powder and the organic carrier for 2H;
(6) printing, namely screen-printing on a metal silver surface (the silver surface is covered on the surface of a high borosilicate 3.3 glass substrate), wherein the thickness of a glaze layer is 25-30 mu m;
(7) firing glaze, wherein the firing glaze temperature is 560-580 ℃, preserving heat for 5min, and finally cooling the preserved glaze to below 100 ℃ along with a furnace, and then discharging the glaze from the furnace;
(8) and (5) detecting the appearance, observing cracks of the glaze surface through a 100X microscope, and removing the unqualified fired glaze.
Preferably, the mixed milling in the step (2) is performed by using a dry ball mill, and the mixed milling time is 6H.
Preferably, the particle size of the glass powder in the step (4) is less than 3 μm.
Preferably, in the step (5), 60wt% of the glass powder and 40wt% of the organic vehicle are stirred uniformly by a known stirring device, and then glaze preparation is performed.
Preferably, in the step (3), the clinker is quenched by using water as a quenching agent, and the clinker is put into water, then is heated by burning, and then is put into water, and the above steps are repeated, so that the rigidity is improved.
Preferably, the powder material ball-milled in the step (4) is placed into a special dryer for glass powder to be dried.
The preparation method of the low-expansion low-temperature environment-friendly glass glaze is suitable for manufacturing large-batch glass glaze
Example two:
a preparation method of a low-expansion low-temperature environment-friendly glass glaze comprises the following steps:
(1) preparing materials according to Bi2O 340 wt-45 wt%, SiO 25 wt-10 wt%, Al2O 30 wt-1 wt%, ZnO 5-2 wt%, B2O 310 wt-15 wt%, Li2O 3-4 wt%, MgO 0-1 wt%, CaO 0-1 wt% and BaO 0-1 wt%, wherein the particle size of each raw material is controlled to be less than 10 mu m;
(2) mixing and grinding, namely putting the material in the step (1) into a ball mill, and performing dry ball milling for 6H;
(3) sintering a frit, namely putting the ball-milled material in the step (2) into a frit furnace for melting, keeping the temperature for 20min at the melting temperature of 1000-1010 ℃, and performing water quenching;
(4) preparing glass powder, namely performing ball milling on the fired frit in the step (3) by using a wet ball mill, controlling the particle size of the powder to be less than 3 mu m, and drying;
(5) preparing glaze, namely mixing 60wt% of the glass powder in the step (4) with 40wt% of an organic carrier, and then ball-milling the mixture of the glass powder and the organic carrier for 2H;
(6) printing, namely screen-printing on a metal silver surface (the silver surface is covered on the surface of a high borosilicate 3.3 glass substrate), wherein the thickness of a glaze layer is 20-25 mu m;
(7) firing glaze, wherein the firing glaze temperature is 550-560 ℃, preserving heat for 5min, and finally cooling the preserved glaze to below 100 ℃ along with a furnace, and then discharging the glaze from the furnace;
(8) and (5) detecting the appearance, observing cracks of the glaze surface through a 100X microscope, and removing the unqualified fired glaze.
Preferably, the mixed milling in the step (2) is performed by using a dry ball mill, and the mixed milling time is 6H.
Preferably, the particle size of the glass powder in the step (4) is less than 3 μm.
Preferably, in the step (5), 60wt% of the glass powder and 40wt% of the organic vehicle are stirred uniformly by a known stirring device, and then glaze preparation is performed.
Preferably, in the step (3), the clinker is quenched by using water as a quenching agent, and the clinker is put into water, then is heated by burning, and then is put into water, and the above steps are repeated, so that the rigidity is improved.
Preferably, the powder material ball-milled in the step (4) is placed into a special dryer for glass powder to be dried.
The preparation method of the low-expansion low-temperature environment-friendly glass glaze is suitable for the preparation of small batches of glass glaze, and greatly improves the quality of the whole glass glaze.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes 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. A preparation method of low-expansion low-temperature environment-friendly glass glaze is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) preparing materials according to Bi2O 340 wt-50 wt%, SiO 25 wt-15 wt%, Al2O 30 wt-3 wt%, ZnO 5-10 wt%, B2O 310 wt-20 wt%, Li2O 3-10 wt%, MgO 0-5 wt%, CaO 0-5 wt% and BaO0 wt-5 wt%, wherein the granularity of each raw material is controlled to be less than 10 μm;
(2) mixing and grinding, namely putting the material in the step (1) into a ball mill, and performing dry ball milling for 6H;
(3) sintering a frit, namely putting the ball-milled material in the step (2) into a frit furnace for melting, keeping the temperature for 20min at the melting temperature of 1000-1050 ℃, and performing water quenching;
(4) preparing glass powder, namely performing ball milling on the fired frit in the step (3) by using a wet ball mill, controlling the particle size of the powder to be less than 3 mu m, and drying;
(5) preparing glaze, namely mixing 60wt% of the glass powder in the step (4) with 40wt% of an organic carrier, and then ball-milling the mixture of the glass powder and the organic carrier for 2H;
(6) printing, namely screen-printing on a metal silver surface (the silver surface is covered on the surface of a high borosilicate 3.3 glass substrate), wherein the thickness of a glaze layer is 20-30 mu m;
(7) firing glaze, wherein the firing glaze temperature is 550-580 ℃, preserving heat for 5min, and finally cooling the heat preserved glaze to below 100 ℃ along with a furnace, and then discharging the glaze from the furnace;
(8) and (5) detecting the appearance, observing cracks of the glaze surface through a 100X microscope, and removing the unqualified fired glaze.
2. The preparation method of the low-expansion low-temperature environment-friendly glass glaze according to claim 1, characterized in that: and (3) carrying out mixed grinding by adopting a dry ball mill in the step (2), wherein the mixed grinding time is 6H.
3. The preparation method of the low-expansion low-temperature environment-friendly glass glaze according to claim 1, characterized in that: the granularity of the glass powder in the step (4) is less than 3 mu m.
4. The preparation method of the low-expansion low-temperature environment-friendly glass glaze according to claim 1, characterized in that: in the step (5), 60wt% of glass powder and 40wt% of organic carrier are stirred uniformly by a known stirring device to prepare the glaze.
5. The preparation method of the low-expansion low-temperature environment-friendly glass glaze according to claim 1, characterized in that: in the step (3), water is used as a quenching agent to quench the frits, the frits are put into the water, then are heated in a red state, and are put into the water again, and the steps are repeated, so that the rigidity can be improved.
6. The preparation method of the low-expansion low-temperature environment-friendly glass glaze according to claim 1, characterized in that: and (4) drying the powder subjected to ball milling in the step (4) in a special dryer for glass powder.
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| CN101066839A (en) * | 2007-06-05 | 2007-11-07 | 东华大学 | No-lead glass powder for electrode coating and its prepn process |
| CN101544470A (en) * | 2009-04-20 | 2009-09-30 | 贵阳晶华电子材料有限公司 | High-bismuth-oxide dielectric material for electrode coating |
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Application publication date: 20200403 |