CN111423127A - Preparation method of glass powder and glass powder - Google Patents
Preparation method of glass powder and glass powder Download PDFInfo
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- CN111423127A CN111423127A CN202010316166.XA CN202010316166A CN111423127A CN 111423127 A CN111423127 A CN 111423127A CN 202010316166 A CN202010316166 A CN 202010316166A CN 111423127 A CN111423127 A CN 111423127A
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- 239000011521 glass Substances 0.000 title claims abstract description 180
- 239000000843 powder Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000155 melt Substances 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims abstract description 41
- 238000000227 grinding Methods 0.000 claims abstract description 32
- 229910001634 calcium fluoride Inorganic materials 0.000 claims abstract description 28
- 238000002844 melting Methods 0.000 claims abstract description 20
- 230000008018 melting Effects 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 18
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 239000012634 fragment Substances 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000005347 annealed glass Substances 0.000 claims description 27
- 239000002002 slurry Substances 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 21
- 230000004907 flux Effects 0.000 claims description 14
- 238000010791 quenching Methods 0.000 claims description 10
- 230000000171 quenching effect Effects 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 6
- 239000006063 cullet Substances 0.000 claims description 6
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 15
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract description 15
- 239000003795 chemical substances by application Substances 0.000 abstract description 15
- 229910052593 corundum Inorganic materials 0.000 abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 15
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 15
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 abstract description 11
- 239000002253 acid Substances 0.000 abstract description 10
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 abstract description 7
- 239000013081 microcrystal Substances 0.000 abstract description 6
- 229910052793 cadmium Inorganic materials 0.000 abstract description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 4
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 4
- 238000000498 ball milling Methods 0.000 description 16
- XGCTUKUCGUNZDN-UHFFFAOYSA-N [B].O=O Chemical compound [B].O=O XGCTUKUCGUNZDN-UHFFFAOYSA-N 0.000 description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 11
- 229910052760 oxygen Inorganic materials 0.000 description 11
- 239000001301 oxygen Substances 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- 239000007788 liquid Substances 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- 239000007921 spray Substances 0.000 description 8
- 238000001694 spray drying Methods 0.000 description 8
- 238000003860 storage Methods 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- 239000005341 toughened glass Substances 0.000 description 7
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical group [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 230000005496 eutectics Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 239000001023 inorganic pigment Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
Images
Classifications
-
- 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
- C03C12/00—Powdered glass; Bead compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
Abstract
The embodiment of the invention provides a preparation method of glass powder and the glass powder, wherein the preparation method comprises the following steps: weighing raw materials and mixing to obtain a mixture; melting the mixture to obtain a melt; cooling the melt and grinding to obtain glass powder; the raw materials comprise: SiO 2240％‑50％；Bi2O317％‑28％；B2O310％‑14％；Al2O31％‑8％；ZrO20.5％‑3％；TiO21％‑3％；La2O30.1-2%, 4.1-14% of fluxing agent, L i2O、Na2O and CaF2. By adding a proper amount of fluxing agent into the components, the glass network connection is tighter, the softening and melting temperature of a glass system is reduced, a multiphase composite system of a microcrystal phase and a glass phase is easy to form, the network structure can be enhanced by the generation of the microcrystal, the acid resistance of the glass is improved, and the glass does not contain heavy metal elements such as lead, cadmium and the like.
Description
Technical Field
The invention relates to the technical field of glass powder, in particular to a preparation method of glass powder and the glass powder.
Background
The automobile toughened glass ink is glass ceramic slurry used at the peripheral edge of automobile toughened glass or on the surface of the whole windshield, and is mainly prepared by uniformly mixing and grinding low-melting-point glass powder, ink-regulating oil, inorganic pigment and an auxiliary agent. Generally, glass printing ink is printed on a glass substrate to be printed through screen printing, after drying and sintering, organic components in the printing ink are basically decomposed and volatilized, low-melting-point glass powder and inorganic pigment are melted and cover the surface of toughened glass, and a black or other dark glass glaze layer is formed. However, the existing glass powder contains heavy metal elements such as lead and cadmium, is easy to pollute the environment, has poor chemical stability, poor chemical corrosion resistance and high melting temperature, and limits the application in glass ink.
Disclosure of Invention
In view of the above, the invention provides a preparation method of glass powder and the glass powder, which are used for solving the problems that the glass powder contains heavy metal elements such as lead and cadmium, is easy to pollute the environment, has poor chemical stability, poor chemical corrosion resistance and high melting temperature.
In order to solve the technical problems, the invention adopts the following technical scheme:
in a first aspect, a method for preparing glass frit according to an embodiment of the present invention includes:
weighing raw materials and mixing to obtain a mixture;
melting the mixture to obtain a melt;
cooling the melt and grinding to obtain the glass powder;
wherein the raw materials comprise:
4.1% -14% of fluxing agent, wherein the fluxing agent comprises L i2O、Na2O and CaF2。
Wherein the flux comprises:
Li2O 1％-5％；
Na2O 3％-7％；
CaF20.1％-2％。
wherein the step of melting the mixture to obtain a melt comprises:
and heating the mixture to 1100-1200 ℃ and preserving the heat for 90-100 min to obtain the melt.
Wherein the step of cooling and grinding the melt to obtain the glass powder comprises:
adding the melt into water for water quenching to obtain glass fragments;
and grinding the glass fragments to obtain the glass powder.
Wherein the step of grinding the glass cullet to obtain the glass powder comprises:
heating the glass fragment to 380-410 ℃, preserving the heat for 30-40 min, and cooling to obtain the annealed glass fragment;
and grinding the annealed glass fragments to obtain the glass powder.
Wherein the step of grinding the annealed glass cullet to obtain the glass powder comprises:
placing the annealed glass fragments in a grinding machine, and grinding and sieving by taking water as a grinding medium to obtain glass slurry;
and drying the glass slurry to obtain the glass powder.
Wherein the glass softening point of the glass powder is 450-480 ℃, and the thermal expansion coefficient of the glass powder is (70-80) × 10-7/℃。
In a second aspect, a glass frit according to an embodiment of the present invention, comprises the following components:
4.1% -14% of fluxing agent, wherein the fluxing agent comprises L i2O、Na2O and CaF2。
Wherein the flux comprises:
Li2O 1％-5％；
Na2O 3％-7％；
CaF20.1％-2％。
wherein the glass softening point of the glass powder is 450-480 ℃, and the thermal expansion coefficient of the glass powder is (70-80) × 10-7/℃。
The technical scheme of the invention has the following beneficial effects:
according to the preparation method of the glass powder, the raw materials are weighed and mixed to obtain a mixture; melting the mixture to obtain a melt; cooling the melt and grinding to obtain the glass powder; wherein the raw materials comprise: SiO 2240％-50％、Bi2O317％-28％、B2O310％-14％、Al2O31％-8％、ZrO20.5％-3％、TiO21％-3％、La2O30.1% -2% and 4.1% -14% of fluxing agent, wherein the fluxing agent comprises L i2O、Na2O and CaF2. By reasonably adjusting the dosage of the components and adding a proper amount of fluxing agent, enough free oxygen can be provided, so that part of boron oxygen trigonal [ BO ] in a glass system3]Boron-oriented oxygen tetrahedron [ BO4]The glass network is more closely connected, the structure is more compact and stable, the softening temperature and the melting temperature of a glass system can be reduced, and micro-pores are easy to formThe multi-phase composite system of the crystal phase and the glass phase has the advantages that the generation of the microcrystal can strengthen the network structure, the acid resistance of the glass is improved, the chemical stability is good, the heavy metal elements such as lead, cadmium and the like are not contained, and the environmental pollution is avoided.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention are clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention, are within the scope of the invention.
The method for preparing the glass frit according to the embodiment of the present invention is specifically described below.
As shown in fig. 1, the method for preparing glass frit according to an embodiment of the present invention includes:
step S1, weighing the raw materials and mixing to obtain a mixture;
step S2, melting the mixture to obtain a melt;
step S3, cooling the melt and grinding to obtain the glass powder;
wherein the raw materials comprise: SiO 2240％-50％、Bi2O317％-28％、B2O310％-14％、Al2O31％-8％、ZrO20.5％-3％、TiO21％-3％、La2O30.1% -2% and 4.1% -14% of fluxing agent, wherein the fluxing agent comprises L i2O、Na2O and CaF2。
In the preparation process of the glass powder, the raw materials are weighed according to the mixture ratio of different components, the weighed raw materials are uniformly mixed to obtain a mixture, the mixture is melted to obtain a melt, the melt is cooled and then ground, and the cooled melt can be ground and ground in a planetary ball millThe flux may comprise L i2O、Na2O and CaF2，Li2O、Na2O and CaF2The specific weight ratio of (A) can be adjusted according to actual needs, for example, the fluxing agent can comprise L i2O 1％-5％、Na2O3% -7% and CaF20.1％-2％。
In the above preparation process, in SiO2、B2O3、Bi2O3、TiO2、ZrO2、Al2O3And L a2O3In (1), adding an appropriate amount of L i2O、Na2O、CaF2As a flux, it is possible to supply sufficient free oxygen to partially form boron-oxygen trigonal [ BO ] in the glass system3]Boron-oriented oxygen tetrahedron [ BO4]The transformation, so that the glass network is connected more closely, the structure is more compact and stable, the thermal expansion coefficient of a glass system can be reduced, and the acid and alkali resistance is improved at L i2O、Na2O、Ca F2In a built fluxing system, L i2O can increase the amount of oxygen in the glass system, break the silicon-oxygen bond, generate non-bridge oxygen, and destroy three-dimensional structure L i+The glass has a small radius, has the greatest bonding strength with oxygen, easily enters the gaps of basic structural units of silicon-oxygen tetrahedrons, boron-oxygen triangles and boron-oxygen tetrahedrons, is easy to move, and contributes to lowering the softening temperature and melting temperature of the glass system. Na (Na)2In addition to breaking the silicon-oxygen bonds and facilitating access to the voids where silicon-oxygen tetrahedra, boron-oxygen trigones, and boron-oxygen tetrahedra are the basic structural elements, O can also form eutectics with other oxides, thereby lowering the softening and melting temperatures of the glass system. CaF2Can form eutectic with other oxides, especially promote SiO2To break the silica bonds to lower the melting point of the glass frit; in addition, a small amount of CaF2With Al2O3、SiO2The oxides can form small amount of microcrystalline glass-like micro crystals to form a multiphase composite system of microcrystalline phase and glass phase, and the thermal expansion coefficient of the glass system is stably controlled within a proper range so as to be matched with a toughened glass substrate(ii) a Meanwhile, the generation of the microcrystal can strengthen the network structure of the glass, improve the acid resistance of the glass and obtain a proper amount of ZrO2And L a2O3The glass network can be reinforced to link broken chains in the network, thereby further enhancing the acid resistance of the glass. The glass powder has good particle size distribution, sintering property and acid and alkali resistance, and is suitable for preparing the automobile toughened glass ink.
In some embodiments of the present invention, the step of melting the mix to obtain a melt may comprise:
heating the mixture to 1100-1200 ℃ and preserving heat for 90-100 min to obtain the melt, for example, heating the mixture to 1100 ℃ and preserving heat for 100min to obtain the melt.
In an embodiment of the present invention, the step of cooling the melt and then grinding to obtain the glass frit may include:
adding the melt into water for water quenching to obtain glass fragments so as to crush the melt while rapidly cooling the melt;
grinding the glass fragments to obtain the glass powder; grinding the melt after pulverizing can improve grinding efficiency and quality.
In some embodiments of the present invention, the step of grinding the glass cullet to obtain the glass powder may include: heating the glass fragment to 380-410 ℃, preserving the heat for 30-40 min, and cooling to obtain the annealed glass fragment; and grinding the annealed glass fragments to obtain the glass powder. The glass fragments are annealed after heat preservation, so that the hardness and the residual stress can be reduced, the size is stabilized, and the deformation and the cracks are reduced.
In an embodiment of the present invention, the step of grinding the annealed glass cullet to obtain the glass powder includes: placing the annealed glass fragments in a grinding machine, and grinding and sieving by taking water as a grinding medium to obtain glass slurry; and drying the glass slurry to obtain the glass powder. For example, the annealed glass fragments are placed in a planetary ball mill, water is used as a ball milling medium, ball milling is carried out for 10h-13h at the rotating speed of 400-450rap/min, then a 200-mesh screen is passed to remove porcelain balls to obtain glass slurry, the glass slurry can be poured into a liquid storage tank of a spray granulator to carry out spray drying, so as to obtain glass powder, the glass powder can be ground into glass powder with different particle sizes according to requirements, for example, the particle size D50 can be 1um-2 um.
In the embodiment of the invention, the glass softening point of the glass powder is 450-480 ℃, and the thermal expansion coefficient of the glass powder is (70-80) × 10-7The glass powder has the transition temperature of 380-405 deg.c, high chemical stability, low heat expansion coefficient and low smelting temperature.
The embodiment of the invention provides glass powder, and the glass powder in the embodiment of the invention can be prepared by the preparation method of the glass powder in the embodiment.
The glass powder comprises the following components: SiO 2240％-50％、Bi2O317％-28％、B2O310％-14％、Al2O31％-8％、ZrO20.5％-3％、TiO21％-3％、La2O30.1% -2% and 4.1% -14% of fluxing agent, wherein the fluxing agent comprises L i2O、Na2O and CaF2，Li2O、Na2O and CaF2The specific weight ratio of (A) can be adjusted according to actual needs, for example, the fluxing agent can comprise L i2O 1％-5％、Na2O3% -7% and CaF20.1％-2％。
In the above glass frit, in SiO2、B2O3、Bi2O3、TiO2、ZrO2、Al2O3And L a2O3In (1), adding an appropriate amount of L i2O、Na2O、CaF2As a flux, it is possible to supply sufficient free oxygen to partially form boron-oxygen trigonal [ BO ] in the glass system3]Boron-oriented oxygen tetrahedron [ BO4]The transformation, so that the glass network is connected more closely, the structure is more compact and stable, the thermal expansion coefficient of a glass system can be reduced, and the acid and alkali resistance is improved at L i2O、Na2O、Ca F2In a built fluxing system, L i2O can increase the amount of oxygen in the glass system, break the silicon-oxygen bond, and generate non-bridge oxygenL i, destroying three-dimensional structure+The glass has a small radius, has the greatest bonding strength with oxygen, easily enters the gaps of basic structural units of silicon-oxygen tetrahedrons, boron-oxygen triangles and boron-oxygen tetrahedrons, is easy to move, and contributes to lowering the softening temperature and melting temperature of the glass system. Na (Na)2In addition to breaking the silicon-oxygen bonds and facilitating access to the voids where silicon-oxygen tetrahedra, boron-oxygen trigones, and boron-oxygen tetrahedra are the basic structural elements, O can also form eutectics with other oxides, thereby lowering the softening and melting temperatures of the glass system. CaF2Can form eutectic with other oxides, especially promote SiO2To break the silica bonds to lower the melting point of the glass frit; in addition, a small amount of CaF2With Al2O3、SiO2The oxides can form a small amount of microcrystalline glass-like tiny crystals to form a multiphase composite system of a microcrystalline phase and a glass phase, and the thermal expansion coefficient of the glass system is stably controlled within a proper range so as to be matched with the toughened glass substrate; meanwhile, the generation of the microcrystal can strengthen the network structure of the glass, improve the acid resistance of the glass and obtain a proper amount of ZrO2And L a2O3The glass network can be reinforced to link broken chains in the network, thereby further enhancing the acid resistance of the glass. The glass powder has good particle size distribution, sintering property and acid and alkali resistance, and is suitable for preparing the automobile toughened glass ink.
In the embodiment of the invention, the glass softening point of the glass powder is 450-480 ℃, and the thermal expansion coefficient of the glass powder is (70-80) × 10-7The glass powder has the transition temperature of 380-405 deg.c, high chemical stability, low heat expansion coefficient and low smelting temperature.
The invention is further illustrated by the following specific examples.
Example 1
Weighing the components according to the weight ratio, and fully mixing to obtain a mixture;
wherein, the raw materials include: SiO 2240％、Bi2O328％、B2O314％、Al2O38％、ZrO23％、TiO21％、La2O30.1% and 5.9% of flux, including L i2O 2.8％、Na2O3% and CaF20.1％；
Heating the mixture to 1200 ℃, preserving heat for 100min to fully melt the mixture to obtain a melt, and then pouring the melt into water for water quenching to obtain glass fragments;
heating the glass fragments to 410 ℃, preserving the heat for 40min, and cooling to room temperature to obtain annealed glass fragments;
placing the annealed glass fragments in a planetary ball mill, ball-milling for 13h at the rotating speed of 450rap/min by using water as a ball-milling medium, then passing through a 200-mesh screen to remove ceramic balls to obtain glass slurry, and pouring the glass slurry into a liquid storage tank of a spray granulator for spray drying to obtain glass powder.
Example 2
Weighing the components according to the weight ratio, and fully mixing to obtain a mixture;
wherein, the raw materials include: SiO 2250％、Bi2O321％、B2O310％、Al2O31％、ZrO20.5％、TiO21.5％、La2O32% and 14% flux, including L i2O 5％、Na2O7% and CaF22％；
Heating the mixture to 1100 ℃, preserving heat for 90min to fully melt the mixture to obtain a melt, and then pouring the melt into water for water quenching to obtain glass fragments;
heating the glass fragments to 380 ℃, preserving the temperature for 30min, and cooling to room temperature to obtain annealed glass fragments;
placing the annealed glass fragments in a planetary ball mill, ball-milling for 10 hours at the rotating speed of 450rap/min by using water as a ball-milling medium, then passing through a 200-mesh screen to remove ceramic balls to obtain glass slurry, and pouring the glass slurry into a liquid storage tank of a spray granulator for spray drying to obtain glass powder.
Example 3
Weighing the components according to the weight ratio, and fully mixing to obtain a mixture;
whereinThe raw materials comprise: SiO 2250％、Bi2O317％、B2O314％、Al2O38％、ZrO23％、TiO23％、La2O30.9% and 4.1% flux including L i2O 1％、Na2O3% and CaF20.1％；
Heating the mixture to 1100 ℃, preserving the temperature for 100min to fully melt the mixture to obtain a melt, and then pouring the melt into water for water quenching to obtain glass fragments;
heating the glass fragments to 400 ℃, preserving the heat for 30min, and cooling to room temperature to obtain annealed glass fragments;
placing the annealed glass fragments in a planetary ball mill, ball-milling for 11h at the rotating speed of 400rap/min by using water as a ball-milling medium, then passing through a 200-mesh screen to remove ceramic balls to obtain glass slurry, and pouring the glass slurry into a liquid storage tank of a spray granulator for spray drying to obtain glass powder.
Example 4
Weighing the components according to the weight ratio, and fully mixing to obtain a mixture;
wherein, the raw materials include: SiO 2245％、Bi2O328％、B2O37％、Al2O35％、ZrO22％、TiO22％、La2O32% and 9% of flux, including L i2O 1％、Na2O7% and CaF21％；
Heating the mixture to 1200 ℃, preserving heat for 100min to fully melt the mixture to obtain a melt, and then pouring the melt into water for water quenching to obtain glass fragments;
heating the glass fragments to 410 ℃, preserving the heat for 40min, and cooling to room temperature to obtain annealed glass fragments;
placing the annealed glass fragments in a planetary ball mill, ball-milling for 13h at the rotating speed of 450rap/min by using water as a ball-milling medium, then passing through a 200-mesh screen to remove ceramic balls to obtain glass slurry, and pouring the glass slurry into a liquid storage tank of a spray granulator for spray drying to obtain glass powder.
Example 5
Weighing the components according to the weight ratio, and fully mixing to obtain a mixture;
wherein, the raw materials include: SiO 2248％、Bi2O324％、B2O313.5％、Al2O32％、ZrO22％、TiO21％、La2O31.5% and 8% of flux, including L i2O 3％、Na2O4% and CaF21％；
Heating the mixture to 1200 ℃, preserving heat for 100min to fully melt the mixture to obtain a melt, and then pouring the melt into water for water quenching to obtain glass fragments;
heating the glass fragments to 410 ℃, preserving the heat for 40min, and cooling to room temperature to obtain annealed glass fragments;
placing the annealed glass fragments in a planetary ball mill, ball-milling for 13h at the rotating speed of 450rap/min by using water as a ball-milling medium, then passing through a 200-mesh screen to remove ceramic balls to obtain glass slurry, and pouring the glass slurry into a liquid storage tank of a spray granulator for spray drying to obtain glass powder.
Example 6
Weighing the components according to the weight ratio, and fully mixing to obtain a mixture;
wherein, the raw materials include: SiO 2242％、Bi2O323％、B2O313％、Al2O35.5％、ZrO22.5％、TiO21.5％、La2O31.5% and 11% flux, including L i2O 3.5％、Na2O6% and CaF21.5％；
Heating the mixture to 1100 ℃, preserving heat for 90min to fully melt the mixture to obtain a melt, and then pouring the melt into water for water quenching to obtain glass fragments;
heating the glass fragments to 410 ℃, preserving the heat for 40min, and cooling to room temperature to obtain annealed glass fragments;
placing the annealed glass fragments in a planetary ball mill, ball-milling for 13h at the rotating speed of 440rap/min by taking water as a ball-milling medium, then passing through a 200-mesh screen to remove ceramic balls to obtain glass slurry, and pouring the glass slurry into a liquid storage tank of a spray granulator for spray drying to obtain glass powder.
Example 7
Weighing the components according to the weight ratio, and fully mixing to obtain a mixture;
wherein, the raw materials include: SiO 2245％、Bi2O320％、B2O312％、Al2O35％、ZrO22％、TiO22.5％、La2O30.5% and 13% of flux, including L i2O 4％、Na2O7% and CaF22％；
Heating the mixture to 1150 ℃ and preserving heat for 90min to fully melt the mixture to obtain a melt, and then pouring the melt into water for water quenching to obtain glass fragments;
heating the glass fragments to 410 ℃, preserving the heat for 40min, and cooling to room temperature to obtain annealed glass fragments;
placing the annealed glass fragments in a planetary ball mill, ball-milling for 13h at the rotating speed of 450rap/min by using water as a ball-milling medium, then passing through a 200-mesh screen to remove ceramic balls to obtain glass slurry, and pouring the glass slurry into a liquid storage tank of a spray granulator for spray drying to obtain glass powder.
The glass powder in the above examples was subjected to a performance test:
testing the thermal expansion coefficient: a test method of linear expansion coefficient of the electric vacuum glass by using SJ 689-83;
glass transition temperature, softening temperature: testing by differential thermal analysis DTA;
and (3) water-resistant chemical stability: SJ 696-83 electric vacuum glass water-chemical resistance stability test formula;
the properties of the glass frit in the above examples are specifically shown in table 1 below.
TABLE 1 Properties of glass frits in different examples
As can be seen from table 1, the glass frit of the above examples has good properties, low expansion coefficient, low melting temperature, easy melting, low softening temperature and glass transition temperature, and good chemical stability.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for preparing glass powder is characterized by comprising the following steps:
weighing raw materials and mixing to obtain a mixture;
melting the mixture to obtain a melt;
cooling the melt and grinding to obtain the glass powder;
wherein the raw materials comprise:
2. the production method according to claim 1, characterized in that the flux comprises:
Li2O 1％-5％；
Na2O 3％-7％；
CaF20.1％-2％。
3. the method of claim 1, wherein the step of melting the mixture to obtain a melt comprises:
and heating the mixture to 1100-1200 ℃ and preserving the heat for 90-100 min to obtain the melt.
4. The method according to claim 1, wherein the step of cooling the melt and then grinding the melt to obtain the glass frit comprises:
adding the melt into water for water quenching to obtain glass fragments;
and grinding the glass fragments to obtain the glass powder.
5. The production method according to claim 4, wherein the step of grinding the glass cullet to obtain the glass powder comprises:
heating the glass fragment to 380-410 ℃, preserving the heat for 30-40 min, and cooling to obtain the annealed glass fragment;
and grinding the annealed glass fragments to obtain the glass powder.
6. The production method according to claim 5, wherein the step of grinding the annealed glass cullet to obtain the glass powder comprises:
placing the annealed glass fragments in a grinding machine, and grinding and sieving by taking water as a grinding medium to obtain glass slurry;
and drying the glass slurry to obtain the glass powder.
7. The method according to claim 1, wherein the glass frit has a glass softening point of 450 ℃ to 480 ℃ and a thermal expansion coefficient of (70 to 80) × 10-7/℃。
8. The glass powder is characterized by comprising the following components:
9. the glass frit of claim 8, wherein the flux comprises:
Li2O 1％-5％；
Na2O 3％-7％；
CaF20.1％-2％。
10. the glass frit according to claim 8, wherein the glass frit has a glass softening point of 450 ℃ to 480 ℃ and a thermal expansion coefficient of (70 to 80) × 10-7/℃。
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| CN113480169A (en) * | 2021-08-03 | 2021-10-08 | 四川虹科创新科技有限公司 | Acid-resistant alkali-resistant lithium-aluminum-silicate glass |
| CN115557706A (en) * | 2022-09-24 | 2023-01-03 | 江苏拜富科技股份有限公司 | Preparation process of high-performance glass powder |
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