CN111499207A - Glass powder, valve plate structure and preparation method - Google Patents
Glass powder, valve plate structure and preparation method Download PDFInfo
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- CN111499207A CN111499207A CN202010313132.5A CN202010313132A CN111499207A CN 111499207 A CN111499207 A CN 111499207A CN 202010313132 A CN202010313132 A CN 202010313132A CN 111499207 A CN111499207 A CN 111499207A
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- glass powder
- filler
- valve plate
- valve
- matrix
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- 239000011521 glass Substances 0.000 title claims abstract description 203
- 239000000843 powder Substances 0.000 title claims abstract description 143
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 66
- 239000000945 filler Substances 0.000 claims abstract description 64
- 239000000463 material Substances 0.000 claims abstract description 52
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 46
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000203 mixture Substances 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 37
- 238000002156 mixing Methods 0.000 claims abstract description 34
- 239000000155 melt Substances 0.000 claims abstract description 31
- 230000001105 regulatory effect Effects 0.000 claims abstract description 31
- 238000001816 cooling Methods 0.000 claims abstract description 24
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 86
- 239000011787 zinc oxide Substances 0.000 claims description 43
- 239000002002 slurry Substances 0.000 claims description 31
- 239000006185 dispersion Substances 0.000 claims description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000001856 Ethyl cellulose Substances 0.000 claims description 17
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 17
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 claims description 17
- 229920001249 ethyl cellulose Polymers 0.000 claims description 17
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 17
- 229910000174 eucryptite Inorganic materials 0.000 claims description 17
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 17
- 229910052845 zircon Inorganic materials 0.000 claims description 16
- 238000005507 spraying Methods 0.000 claims description 14
- 229910000505 Al2TiO5 Inorganic materials 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 11
- 229910052582 BN Inorganic materials 0.000 claims description 9
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 9
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 9
- 229910002113 barium titanate Inorganic materials 0.000 claims description 9
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 9
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 9
- 229910052878 cordierite Inorganic materials 0.000 claims description 9
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052907 leucite Inorganic materials 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 9
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 9
- 239000001040 synthetic pigment Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 9
- 230000007704 transition Effects 0.000 abstract description 6
- 229910052681 coesite Inorganic materials 0.000 abstract description 5
- 229910052593 corundum Inorganic materials 0.000 abstract description 5
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 5
- 229910052682 stishovite Inorganic materials 0.000 abstract description 5
- 229910052905 tridymite Inorganic materials 0.000 abstract description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 5
- 229910052573 porcelain Inorganic materials 0.000 description 24
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 15
- 238000000498 ball milling Methods 0.000 description 15
- 239000007788 liquid Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 8
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 8
- 238000005096 rolling process Methods 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 8
- 239000010935 stainless steel Substances 0.000 description 8
- 229910052726 zirconium Inorganic materials 0.000 description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 7
- 229910001928 zirconium oxide Inorganic materials 0.000 description 7
- 238000007789 sealing Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000003849 aromatic solvent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007590 electrostatic spraying Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray 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
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/07—Glass compositions containing silica with less than 40% silica by weight containing lead
- C03C3/072—Glass compositions containing silica with less than 40% silica by weight containing lead containing boron
- C03C3/074—Glass compositions containing silica with less than 40% silica by weight containing lead containing boron containing zinc
-
- 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
- C03C8/10—Frit compositions, i.e. in a powdered or comminuted form containing lead
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
- H01C7/12—Overvoltage protection resistors
Abstract
The embodiment of the invention provides glass powder, a valve plate structure and a preparation method thereof, wherein the preparation method of the glass powder comprises the following steps: weighing raw materials and mixing to obtain a mixture; melting the mixture into a melt; cooling the melt and grinding to obtain matrix glass powder; adding a filler into the matrix glass powder and mixing to obtain glass powder; the raw materials comprise: 50% -70% of PbO; b is2O310％‑20％；ZnO 5％‑15％；SiO20.5‑10％；Al2O30 to 5 percent; 0-3% of regulating material, the regulating material comprises NiO and Co2O3、MnO2And CuO; the weight ratio of the matrix glass powder to the filler is (60-90): (10-40). The glass powder prepared by the method has good performance, when the glass powder is applied to the ZnO valve plate, the glass powder is easily matched with the thermal expansion coefficient of the valve plate, the moisture-proof effect is good, and because the components of the glass powder contain the components of the valve plate, a good transition layer is easily formed between the glass powder and the valve plate, so that the glass powder glaze layer is well combined with the valve plate.
Description
Technical Field
The invention relates to the technical field of glass materials, in particular to glass powder, a valve plate structure and a preparation method.
Background
The metal oxide arrester (ZnO arrester) is a latest power transmission line protection product, and can protect the normal operation of a line in thunderstorm weather and reduce economic loss. However, the ZnO arrester valve plate has the defects of rough side surface, easy moisture absorption, oil stain resistance and the like, and the normal operation of the arrester can be seriously influenced after the side surface is in flashover in thunderstorm weather or under high pressure, so that the side surface needs to be covered and protected. At present, the side face of a valve plate of a lightning arrester is protected by a glaze layer, the existing glaze is easy to absorb water, the valve plate is not well wetted, the thermal expansion coefficient of the valve plate is greatly different from that of the valve plate, so that the valve plate is poor in stability when being subjected to thermal shock, cracks are generated on the side face, the valve plate is aged, the performance is poor, the protective effect cannot be achieved, the temperature resistance is poor, and the strength is low.
Disclosure of Invention
In view of the above, the invention provides a glass powder, a valve plate structure and a preparation method thereof, which are used for solving the problems that the existing glaze is easy to absorb water, has poor wettability to a valve plate, has large difference between the thermal expansion coefficient and the valve plate, causes poor stability when the valve plate is subjected to thermal shock, generates cracks on the side surface, is aged, has poor performance, cannot play a role in protection, has poor temperature resistance and is low in strength.
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 mixed material into a melt;
cooling the melt and grinding to obtain matrix glass powder;
adding a filler into the matrix glass powder and mixing to obtain the glass powder;
wherein the raw materials comprise:
0-3% of regulating material, wherein the regulating material comprises NiO and Co2O3、MnO2And CuO;
the weight ratio of the matrix glass powder to the filler is (60-90): (10-40).
Wherein the filler comprises:
aluminum titanate, lead titanate, barium titanate, boron nitride, aluminum nitride, silicon nitride, β -eucryptite, leucite, cordierite, zircon, a synthetic pigment of zircon, silica, alumina, titania, zinc oxide, magnesium oxide.
Wherein the step of melting the mixture into a melt comprises:
and melting the mixture for 1h-3h at 1100-1300 ℃ to obtain the melt.
In a second aspect, a glass frit according to an embodiment of the present invention includes a matrix glass frit and a filler, and the matrix glass frit includes:
0-3% of regulating material, wherein the regulating material comprises NiO and Co2O3、MnO2And CuO;
the weight ratio of the matrix glass powder to the filler is (60-90): (10-40).
Wherein the filler comprises:
aluminum titanate, lead titanate, barium titanate, boron nitride, aluminum nitride, silicon nitride, β -eucryptite, leucite, cordierite, zircon, a synthetic pigment of zircon, silica, alumina, titania, zinc oxide, magnesium oxide.
In a third aspect, the preparation method of the valve sheet structure according to the embodiment of the invention comprises the following steps:
mixing the glass powder and the dispersion liquid to form slurry;
spraying the slurry on the side surface of an unannealed valve block blank, wherein the valve block blank is a zinc oxide material piece;
and sintering the sprayed valve sheet blank to obtain the valve sheet structure with the glass glaze layer.
The step of sintering the sprayed valve element blank to obtain the valve plate structure with the glass glaze layer comprises the following steps:
heating the sprayed valve element blank to 480-580 ℃ and preserving heat at 480-580 ℃;
and cooling the sprayed valve element blank from 480-580 ℃ to obtain the valve plate structure with the glass glaze layer.
Wherein the dispersion comprises ethyl cellulose and a solvent.
In a fourth aspect, a valve sheet structure according to an embodiment of the present invention includes:
the valve plate is made of zinc oxide material;
the glass glaze layer is coated on the surface of the valve plate;
wherein the glass glaze layer comprises matrix glass powder and a filler, and the matrix glass powder comprises:
0-3% of regulating material, wherein the regulating material comprises NiO and Co2O3、MnO2And CuO;
the weight ratio of the matrix glass powder to the filler is (60-90): (10-40).
Wherein the filler comprises:
aluminum titanate, lead titanate, barium titanate, boron nitride, aluminum nitride, silicon nitride, β -eucryptite, leucite, cordierite, zircon, a synthetic pigment of zircon, silica, alumina, titania, zinc oxide, magnesium oxide.
The technical scheme of the invention has the following beneficial effects:
according to the preparation method of the glass powder, raw materials are weighed and mixed to form a mixture, the mixture is melted to form a melt, the melt is cooled and ground to obtain matrix glass powder, a filler is added into the matrix glass powder to be mixed to obtain the glass powder, and the raw materials comprise 50% -70% of PbO and B2O310％-20％、ZnO 5％-15％、SiO20.5％-10％、Al2O30-5% of regulating material and 0-3% of regulating material, the regulating material includes NiO and Co2O3、MnO2And CuO, the weight ratio of the matrix glass powder to the filler is (60-90): (10-40). The glass powder prepared by the method has the advantages of good performance, good temperature resistance, high strength, difficult water absorption, good wettability to the valve plate, small difference between the thermal expansion coefficient of the glass powder and the valve plate, capability of avoiding the problem of poor stability when the glass powder is subjected to thermal shock, stable performance and protective effect; when the glass powder is applied to the ZnO valve plate, the thermal expansion coefficient of the glass powder is matched with that of the valve plate, the moisture-proof effect is good, and the glass powder glaze layer is well combined with the valve plate because the components of the valve plate contain the components of the valve plate and a good transition layer is easily formed between the glass powder glaze layer and the valve plate.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing glass frit according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a valve plate structure according to an embodiment of the invention.
Reference numerals
A valve plate 10; a glass glaze layer 11.
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 raw materials and mixing the raw materials into a mixture;
step S2, melting the mixture into a melt;
step S3, cooling the melt and grinding to obtain matrix glass powder;
step S4, adding filler into the matrix glass powder and mixing to obtain the glass powder;
wherein the raw materials comprise: 50% -70% of PbO, B2O310％-20％、ZnO 5％-15％、SiO20.5％-10％、Al2O30-5% of regulating material, 0-3% of matrix glass powder and filler in a weight ratio of (60-90): (10-40), the modifier comprises NiO and Co2O3、MnO2And CuO.
That is, in the preparation process, the raw material components are weighed according to the weight proportion, different components are uniformly mixed to form a mixture, for example, the raw materials can be put into a zirconia bottle and ball-milled by using zirconium balls, and the mixture is prepared after the raw materials are fully mixed for 1 hour by a planetary ball mill; the mixture can be melted into a melt at a certain temperature, for example, the mixture is melted at 1100-1300 ℃ for 1-3 h to obtainMelting the mixture in a silicon-carbon rod resistance furnace, cooling the melt, grinding to obtain matrix glass powder, wherein the raw material components have the same content as the matrix glass powder, for example, pouring the melt on a stainless steel mill, rolling into glass sheets, putting the glass sheets into an alumina porcelain bottle, putting high-alumina balls into the alumina porcelain bottle, putting the alumina porcelain bottle on a roller bottle mill, performing ball milling for 24 hours, grinding the glass sheets to obtain matrix glass powder, and crushing the matrix glass powder to a particle size D50 of 10 μm, wherein the glass transition temperature of the matrix glass powder is 350-390 ℃, the softening temperature is 400-440 ℃, and the thermal expansion coefficient of the matrix glass powder is 60 × 10-300 DEG C-7/℃-90×10-7V. C. The filler can be added into the matrix glass powder to be mixed to obtain the glass powder, and the filler can be added into the matrix glass powder according to different thermal expansion coefficients and sintering temperatures of the ZnO valve plates to meet the thermal expansion coefficient matching sealing requirements of the valve plates with different formulas.
In some embodiments, the glass frit may not have Al added thereto2O3The adjusting material can be selectively added according to actual needs, and the color of the glass powder glaze layer can be adjusted by adding the adjusting material. The glass powder prepared by the method has the advantages of good performance, good temperature resistance, high strength, difficult water absorption, good wettability to the valve plate, small difference between the thermal expansion coefficient of the glass powder and the valve plate, capability of avoiding the problem of poor stability when the glass powder is subjected to thermal shock, stable performance and protective effect; when the glass powder is applied to the ZnO valve plate, the glass powder can be matched with the thermal expansion coefficient of the valve plate, the moisture-proof effect is good, and the glass powder glaze layer is well combined with the valve plate because the component ZnO of the valve plate is contained in the component ZnO, so that a good transition layer is easily formed between the glass powder glaze layer and the valve plate.
In some embodiments of the present invention, the filler may include one or more of aluminum titanate, lead titanate, barium titanate, boron nitride, aluminum nitride, silicon nitride, β -eucryptite, leucite, cordierite, zircon, a synthetic pigment of zircon, silica, alumina, titania, zinc oxide, magnesium oxide, for example, the filler may include β -eucryptite and lead titanate, the filler may include β -eucryptite or lead titanateThe coefficient of thermal expansion of the material may be-120 × 10-7/℃-250×10-7The filler can be added into the matrix glass powder according to the different thermal expansion coefficients and sintering temperatures of the ZnO valve plates to meet the requirement of matching sealing of the thermal expansion coefficients of the valve plates with different formulas, and the glass powder obtained by adding the filler can be used for sealing and matching the thermal expansion coefficient of the valve plates with 0-150 × 10-7The material between/° c provides a sealed sample.
The embodiment of the invention provides glass powder, which comprises matrix glass powder and a filler, wherein the matrix glass powder comprises the following components: 50% -70% of PbO, B2O310％-20％、ZnO 5％-15％、SiO20.5％-10％、Al2O30-5% of regulating material, 0-3% of matrix glass powder and filler in a weight ratio of (60-90): (10-40), the modifier comprises NiO and Co2O3、MnO2And CuO, NiO, Co2O3、MnO2And CuO may be present in a weight ratio of 1: 1: 0.7: 0.3. in some embodiments, the glass frit may not have Al added thereto2O3The glass powder has good temperature resistance, high strength, difficult water absorption, good infiltration to a valve plate, small difference between the thermal expansion coefficient and the valve plate, stable performance and protection effect, can be matched with the thermal expansion coefficient of the valve plate when being applied to a ZnO valve plate, has good moisture-proof effect, can easily form a good transition layer with the valve plate due to the ZnO component in the components, and ensures that a glass powder glaze layer is well combined with the valve plate, the glass transition temperature of the matrix glass powder is between 350 and 390 ℃, the softening temperature is between 400 and 440 ℃, and the thermal expansion coefficient of the matrix glass powder is 60 × 10 between 25 and 300 DEG.-7/℃-90×10-7/℃。
Optionally, the filler comprises aluminum titanate, lead titanate, barium titanate, boron nitride, aluminum nitride, silicon nitride, β -eucryptite, leucite, cordierite, zirconite, a pigment synthesized from zirconiteOne or more of silica, alumina, titania, zinc oxide, magnesium oxide, for example, the filler may comprise β -eucryptite and lead titanate, the filler may comprise β -eucryptite or lead titanate the filler may have a coefficient of thermal expansion of-120 × 10-7/℃-250×10-7and/DEG C, according to the difference between the thermal expansion coefficient of the used ZnO valve plate and the sintering temperature, the filler can be added into the matrix glass powder so as to meet the requirement of matching and sealing the thermal expansion coefficients of the valve plates with different formulas.
The glass powder in the embodiment of the invention can be prepared by the preparation method of the glass powder, and the components in the glass powder can be correspondingly consistent with the raw material components added in the preparation method.
The embodiment of the invention provides a preparation method of a valve plate structure.
The preparation method of the valve plate structure provided by the embodiment of the invention comprises the following steps:
mixing the glass powder and the dispersion liquid to form slurry;
spraying the slurry on the side surface of an unannealed valve block blank, wherein the valve block blank is a zinc oxide material piece;
and sintering the sprayed valve sheet blank to obtain the valve sheet structure with the glass glaze layer.
That is, the glass powder is added into the dispersion liquid for uniform dispersion, and the slurry is obtained after uniform mixing, for example, the glass powder and the dispersion liquid are mixed according to a certain proportion and then are put into a horizontal grinding machine for mixing for 4 hours to obtain uniform slurry, and the solid content of the slurry can be 20-50%; then spraying the slurry on the side surface of the unannealed valve block blank, wherein the valve block blank can be cylindrical, and can be sprayed by using a spraying method such as manual brush coating, spray gun spraying, electrostatic spraying and the like, and the spraying thickness can be about 0.2mm and can also be selected according to needs; and finally, sintering the sprayed valve sheet element blank to obtain a valve sheet structure with a glass glaze layer, so that the outer layer of the valve sheet structure is coated with the glass powder glaze layer, and a good transition layer is easily formed between the glass powder glaze layer and the valve sheet because the component ZnO of the valve sheet is contained in the component of the glass powder glaze layer.
In some embodiments of the present invention, the step of sintering the sprayed valve element blank to obtain the valve element structure with the glass glaze layer may include:
heating the sprayed valve element blank to 480-580 ℃, preserving heat at 480-580 ℃, and cooling the sprayed valve element blank from 480-580 ℃ to obtain the valve plate structure. For example, the valve element blank can be heated to 480-580 ℃ (working temperature) after 6 hours, dispersion in the slurry is removed through heating, then heat preservation is carried out for 0.5 hour at 480-580 ℃, glass powder is vitrified through heat preservation, finally the temperature is reduced to 320 ℃ from 480-580 ℃ after 3 hours, stress between the glass powder glaze layer and the valve element can be reduced through slow cooling, then furnace cooling is carried out to room temperature, the valve element structure with the glass powder glaze layer is obtained, and different adjusting materials can be added according to needs to obtain the inorganic glass powder glaze layer with smooth surface, such as grayish yellow, grayish green or bluish black and the like. In addition, during testing, aluminum layers can be sprayed on the upper surface and the lower surface of the valve plate respectively.
In an embodiment of the present invention, the dispersion may include ethyl cellulose and a solvent, the solvent may be an alcohol (such as methanol, ethanol, etc.), the solvent may be butyl diglycol and/or ethanol, and the solvent may also be an aromatic solvent.
The embodiment of the invention provides a valve plate structure.
As shown in fig. 2, the valve sheet structure of the embodiment of the invention includes a valve sheet 10 and a glass glaze layer 11, the valve sheet 10 is a zinc oxide material, the valve sheet can be cylindrical, and the glass glaze layer 11 is coated on the side surface of the valve sheet 10; wherein, glass glaze layer 11 includes matrix glass powder and filler, and the matrix glass powder includes: 50% -70% of PbO, B2O310％-20％、ZnO 5％-15％、SiO20.5％-10％、Al2O30-5% of regulating material, 0-3% of matrix glass powder and filler in a weight ratio of (60-90): (10-40), the modifier comprises NiO and Co2O3、MnO2And CuO, NiO, Co2O3、MnO2And CuO may be present in a weight ratio of 1: 1: 0.7: 0.3. in addition, in-situ measurementWhen the valve plate is used in a trial mode, the upper surface and the lower surface of the valve plate can be respectively sprayed with aluminum layers.
In some embodiments, no Al may be added to glaze layer 112O3The regulating material can be selectively added according to actual requirements, and different regulating materials can be added according to requirements to obtain the inorganic glass powder glaze layer with smooth surface, such as grey yellow, grey green or blue black. The glass powder in the embodiment is used for coating the glass glaze layer 11 on the side face of the valve plate, so that a good protection effect can be generated on the side face of the valve plate 10, the glass glaze layer 11 is good in temperature resistance, high in strength, good in wettability to the valve plate, capable of being matched with the thermal expansion coefficient of the valve plate and good in moisture-proof effect, and a good transition layer is easily formed between the glass powder glaze layer and the valve plate due to the fact that the component ZnO of the valve plate is contained in the component ZnO, so that the glass powder glaze layer and the valve plate are well combined.
Alternatively, the filler may include one or more of aluminum titanate, lead titanate, barium titanate, boron nitride, aluminum nitride, silicon nitride, β -eucryptite, leucite, cordierite, zircon, a zircon-derived pigment, silica, alumina, titania, zinc oxide, magnesium oxide, for example, the filler may include β -eucryptite and lead titanate the filler may have a coefficient of thermal expansion of-120 × 10-7/℃-250×10-7The filler can be selectively added according to the difference between the thermal expansion coefficient of the ZnO valve plate and the sintering temperature, so as to meet the requirement of matching and sealing the thermal expansion coefficients of the valve plates with different formulas.
The present invention will be further described with reference to the following specific examples.
Example 1
Weighing raw materials according to a weight ratio, putting the raw materials into a zirconium oxide bottle, performing ball milling for 1h in a planetary ball mill by using zirconium balls, and fully mixing to prepare a mixture; placing the mixture in a silicon-carbon rod resistance furnace, and melting for 3 hours at 1100 ℃ to obtain a melt; then, pouring the melt on a stainless steel rolling mill to roll into glass sheets, then putting the glass sheets into an alumina porcelain bottle, putting high-alumina balls into the alumina porcelain bottle, and putting the alumina porcelain bottle on a roller bottle machine to perform ball milling for 24 hours to obtain matrix glass powder; adding a filler into the matrix glass powder and mixing to obtain glass powder;
wherein the raw materials comprise:
the weight ratio of the matrix glass powder to the filler is 90: 10, the filler comprises aluminum titanate.
Mixing the glass powder and the dispersion liquid according to a proportion, and then putting the mixture into a horizontal grinding machine to be mixed for 4 hours to obtain uniform slurry, wherein the content of the glass powder in the slurry is 50%; the dispersion comprises ethyl cellulose and diethylene glycol butyl ether, wherein the weight ratio of the ethyl cellulose to the diethylene glycol butyl ether is 39: 16;
spraying the slurry on the side surface of an unannealed valve block blank, wherein the valve block blank is a zinc oxide material piece;
heating the sprayed valve element blank to 480 ℃ after 6h, and preserving heat for 0.5h at 480 ℃;
and (3) cooling the sprayed valve element blank from 480 ℃ for 3h to 320 ℃, and then cooling the valve element blank to room temperature along with a furnace to obtain the valve element structure with the glass glaze layer.
Example 2
Weighing raw materials according to a weight ratio, putting the raw materials into a zirconium oxide bottle, performing ball milling for 1h in a planetary ball mill by using zirconium balls, and fully mixing to prepare a mixture; placing the mixture in a silicon-carbon rod resistance furnace, and melting for 1h at 1300 ℃ to obtain a melt; then, pouring the melt on a stainless steel rolling mill to roll into glass sheets, then putting the glass sheets into an alumina porcelain bottle, putting high-alumina balls into the alumina porcelain bottle, and putting the alumina porcelain bottle on a roller bottle machine to perform ball milling for 24 hours to obtain matrix glass powder; adding a filler into the matrix glass powder and mixing to obtain glass powder;
wherein the raw materials comprise:
the weight ratio of the matrix glass powder to the filler is 80: the filler comprises aluminum titanate 20.
Mixing the glass powder and the dispersion liquid according to a proportion, and then putting the mixture into a horizontal grinding machine to be mixed for 4 hours to obtain uniform slurry, wherein the content of the glass powder in the slurry is 20%; the dispersion comprises ethyl cellulose and diethylene glycol butyl ether, wherein the weight ratio of the ethyl cellulose to the diethylene glycol butyl ether is 39: 16;
spraying the slurry on the side surface of an unannealed valve block blank, wherein the valve block blank is a zinc oxide material piece;
heating the sprayed valve element blank to 580 ℃ after 6 hours, and preserving heat for 0.5 hour at 580 ℃;
and (3) cooling the sprayed valve element blank from 580 ℃ to 320 ℃ after 3h, and then cooling the valve element blank to room temperature along with a furnace to obtain the valve element structure with the glass glaze layer.
Example 3
Weighing raw materials according to a weight ratio, putting the raw materials into a zirconium oxide bottle, performing ball milling for 1h in a planetary ball mill by using zirconium balls, and fully mixing to prepare a mixture; placing the mixture in a silicon-carbon rod resistance furnace, and melting for 2h at 1200 ℃ to obtain a melt; then, pouring the melt on a stainless steel rolling mill to roll into glass sheets, then putting the glass sheets into an alumina porcelain bottle, putting high-alumina balls into the alumina porcelain bottle, and putting the alumina porcelain bottle on a roller bottle machine to perform ball milling for 24 hours to obtain matrix glass powder; adding a filler into the matrix glass powder and mixing to obtain glass powder;
wherein the raw materials comprise:
1.5% of regulating material, including NiO and Co2O3、MnO2And CuO, NiO, Co2O3、MnO2And CuO in a weight ratio of 1: 1: 0.7: 0.3;
the weight ratio of the matrix glass powder to the filler is 60: the filler comprises lead titanate 40.
Mixing the glass powder and the dispersion liquid according to a proportion, and then putting the mixture into a horizontal grinding machine to be mixed for 4 hours to obtain uniform slurry, wherein the content of the glass powder in the slurry is 45%; the dispersion comprises ethyl cellulose and diethylene glycol butyl ether, wherein the weight ratio of the ethyl cellulose to the diethylene glycol butyl ether is 39: 16;
spraying the slurry on the side surface of an unannealed valve block blank, wherein the valve block blank is a zinc oxide material piece;
heating the sprayed valve element blank to 480 ℃ after 6h, and preserving heat for 0.5h at 480 ℃;
and (3) cooling the sprayed valve element blank from 480 ℃ for 3h to 320 ℃, and then cooling the valve element blank to room temperature along with a furnace to obtain the valve element structure with the glass glaze layer.
Example 4
Weighing raw materials according to a weight ratio, putting the raw materials into a zirconium oxide bottle, performing ball milling for 1h in a planetary ball mill by using zirconium balls, and fully mixing to prepare a mixture; placing the mixture in a silicon-carbon rod resistance furnace, and melting for 2 hours at 1300 ℃ to obtain a melt; then, pouring the melt on a stainless steel rolling mill to roll into glass sheets, then putting the glass sheets into an alumina porcelain bottle, putting high-alumina balls into the alumina porcelain bottle, and putting the alumina porcelain bottle on a roller bottle machine to perform ball milling for 24 hours to obtain matrix glass powder; adding a filler into the matrix glass powder and mixing to obtain glass powder;
wherein the raw materials comprise:
3% of regulating material, wherein the regulating material comprises NiO and Co2O3、MnO2And CuO, NiO, Co2O3、MnO2And CuO in a weight ratio of 1: 1: 0.7: 0.3;
the weight ratio of the matrix glass powder to the filler is 90: 10.
mixing the glass powder and the dispersion liquid according to a proportion, and then putting the mixture into a horizontal grinding machine to be mixed for 4 hours to obtain uniform slurry, wherein the content of the glass powder in the slurry is 40%; the dispersion comprises ethyl cellulose, diethylene glycol butyl ether and ethanol, wherein the weight ratio of the ethyl cellulose to the diethylene glycol butyl ether to the ethanol is 39: 16: 20;
spraying the slurry on the side surface of an unannealed valve block blank, wherein the valve block blank is a zinc oxide material piece;
heating the sprayed valve element blank to 520 ℃ after 6 hours, and preserving heat for 0.5 hour at 520 ℃;
and (3) cooling the sprayed valve element blank from 520 ℃ for 3h to 320 ℃, and then cooling the valve element blank to room temperature along with a furnace to obtain the valve element structure with the glass glaze layer.
Example 5
Weighing raw materials according to a weight ratio, putting the raw materials into a zirconium oxide bottle, performing ball milling for 1h in a planetary ball mill by using zirconium balls, and fully mixing to prepare a mixture; placing the mixture in a silicon-carbon rod resistance furnace, and melting for 1h at 1300 ℃ to obtain a melt; then, pouring the melt on a stainless steel rolling mill to roll into glass sheets, then putting the glass sheets into an alumina porcelain bottle, putting high-alumina balls into the alumina porcelain bottle, and putting the alumina porcelain bottle on a roller bottle machine to perform ball milling for 24 hours to obtain matrix glass powder; adding a filler into the matrix glass powder and mixing to obtain glass powder;
wherein the raw materials comprise:
3% of regulating material, wherein the regulating material comprises NiO and Co2O3、MnO2And CuO, NiO, Co2O3、MnO2And CuO in a weight ratio of 1: 1: 0.7: 0.3;
the weight ratio of the matrix glass powder to the filler was 80: 20, the filler comprised β -eucryptite and lead titanate, and the weight ratio of β -eucryptite and lead titanate was 5: 15.
Mixing the glass powder and the dispersion liquid according to a proportion, and then putting the mixture into a horizontal grinding machine to be mixed for 4 hours to obtain uniform slurry, wherein the content of the glass powder in the slurry is 45%; the dispersion comprises ethyl cellulose and diethylene glycol butyl ether, wherein the weight ratio of the ethyl cellulose to the diethylene glycol butyl ether is 39: 16;
spraying the slurry on the side surface of an unannealed valve block blank, wherein the valve block blank is a zinc oxide material piece;
heating the sprayed valve element blank to 540 ℃ after 6 hours, and preserving heat for 0.5 hour at 540 ℃;
and (3) cooling the sprayed valve element blank from 540 ℃ to 320 ℃ after 3h, and then cooling the valve element blank to room temperature along with a furnace to obtain the valve element structure with the glass glaze layer.
Example 6
Weighing raw materials according to a weight ratio, putting the raw materials into a zirconium oxide bottle, performing ball milling for 1h in a planetary ball mill by using zirconium balls, and fully mixing to prepare a mixture; placing the mixture in a silicon-carbon rod resistance furnace, and melting for 1h at 1300 ℃ to obtain a melt; then, pouring the melt on a stainless steel rolling mill to roll into glass sheets, then putting the glass sheets into an alumina porcelain bottle, putting high-alumina balls into the alumina porcelain bottle, and putting the alumina porcelain bottle on a roller bottle machine to perform ball milling for 24 hours to obtain matrix glass powder; adding a filler into the matrix glass powder and mixing to obtain glass powder;
wherein the raw materials comprise:
3% of regulating material, wherein the regulating material comprises NiO and Co2O3、MnO2And CuO, NiO, Co2O3、MnO2And CuO in a weight ratio of 1: 1: 0.7: 0.3;
the weight ratio of the matrix glass powder to the filler is 73: 27, the filler comprises lead titanate.
Mixing the glass powder and the dispersion liquid according to a proportion, and then putting the mixture into a horizontal grinding machine to be mixed for 4 hours to obtain uniform slurry, wherein the content of the glass powder in the slurry is 45%; the dispersion comprises ethyl cellulose and diethylene glycol butyl ether, wherein the weight ratio of the ethyl cellulose to the diethylene glycol butyl ether is 39: 16;
spraying the slurry on the side surface of an unannealed valve block blank, wherein the valve block blank is a zinc oxide material piece;
heating the sprayed valve element blank to 530 ℃ after 6h, and preserving heat at 530 ℃ for 0.5 h;
and (3) cooling the sprayed valve element blank from 530 ℃ for 3h to 320 ℃, and then cooling the valve element blank to room temperature along with a furnace to obtain the valve element structure with the glass glaze layer.
Example 7
Weighing raw materials according to a weight ratio, putting the raw materials into a zirconium oxide bottle, performing ball milling for 1h in a planetary ball mill by using zirconium balls, and fully mixing to prepare a mixture; placing the mixture in a silicon-carbon rod resistance furnace, and melting for 1h at 1300 ℃ to obtain a melt; then, pouring the melt on a stainless steel rolling mill to roll into glass sheets, then putting the glass sheets into an alumina porcelain bottle, putting high-alumina balls into the alumina porcelain bottle, and putting the alumina porcelain bottle on a roller bottle machine to perform ball milling for 24 hours to obtain matrix glass powder; adding a filler into the matrix glass powder and mixing to obtain glass powder;
wherein the raw materials comprise:
3% of regulating material, wherein the regulating material comprises NiO and Co2O3、MnO2And CuO, NiO, Co2O3、MnO2And CuO in a weight ratio of 1: 1: 0.7: 0.3;
the weight ratio of the matrix glass frit to the filler was 90: 10, and the filler included β -eucryptite.
Mixing the glass powder and the dispersion liquid according to a proportion, and then putting the mixture into a horizontal grinding machine to be mixed for 4 hours to obtain uniform slurry, wherein the content of the glass powder in the slurry is 45%; the dispersion comprises ethyl cellulose and diethylene glycol butyl ether, wherein the weight ratio of the ethyl cellulose to the diethylene glycol butyl ether is 39: 16;
spraying the slurry on the side surface of an unannealed valve block blank, wherein the valve block blank is a zinc oxide material piece;
heating the sprayed valve element blank to 520 ℃ after 6 hours, and preserving heat for 0.5 hour at 520 ℃;
and (3) cooling the sprayed valve element blank from 520 ℃ for 3h to 320 ℃, and then cooling the valve element blank to room temperature along with a furnace to obtain the valve element structure with the glass glaze layer.
The thermal expansion coefficients of the glass frits prepared in the above examples are shown in table 1 below.
TABLE 1 thermal expansion coefficients of glass frits in different examples
The valve plate element blank in the embodiment can be a ZnO valve plate of D30 type, and the valve plate structure in the embodiment is polished and then aluminum layers are respectively sprayed on the upper surface and the lower surface of the valve plate to obtain a sample to be tested, wherein the sample to be tested has a smooth surface.
And (3) sample testing: the sample is subjected to a 65kA heavy current test of national standard 4/10 mu s, the glass glaze layer on the sample can pass the 65kA heavy current test twice, the surface of the glaze layer is smooth, the sample is subjected to three continuous heavy current tests without cooling, the test standard is 70kA, and the test results are shown in Table 2 below.
TABLE 2 test results for different samples
| Number of samples/time | 1 | 2 | 3 |
| Example 1 | 69.20 | 69.15 | × |
| Example 2 | 68.82 | 68.66 | × |
| Example 3 | 71.68 | 70.65 | 69.67 |
| Example 4 | 70.11 | 68.12 | × |
| Example 5 | 75.15 | 69.27 | 67.74 |
| Example 6 | 70.22 | 68.11 | × |
| Example 7 | 72.06 | 67.67 | × |
Through the test, the glass glaze layer on the sample can pass two 65kA heavy current tests, and has a good protection effect on the side face of the valve plate. The result shows that the sample in the experimental example 5 has the best effect of resisting the large current, can resist the large current for three times without damage, and the ZnO valve plate of the D30 model can resist the large current impact of 4/10 mu s to 75.15kA after the insulating glaze layer in the example 5 is used.
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 mixed material into a melt;
cooling the melt and grinding to obtain matrix glass powder;
adding a filler into the matrix glass powder and mixing to obtain the glass powder;
wherein the raw materials comprise:
0-3% of regulating material, wherein the regulating material comprises NiO and Co2O3、MnO2And CuO;
the weight ratio of the matrix glass powder to the filler is (60-90): (10-40).
2. The method of manufacturing according to claim 1, wherein the filler comprises:
aluminum titanate, lead titanate, barium titanate, boron nitride, aluminum nitride, silicon nitride, β -eucryptite, leucite, cordierite, zircon, a synthetic pigment of zircon, silica, alumina, titania, zinc oxide, magnesium oxide.
3. The method of claim 1, wherein the step of melting the mix into a melt comprises:
and melting the mixture for 1h-3h at 1100-1300 ℃ to obtain the melt.
4. The glass powder is characterized in that the glass powder comprises matrix glass powder and filler, and the matrix glass powder comprises the following components:
0-3% of regulating material, wherein the regulating material comprises NiO and Co2O3、MnO2And CuO;
the weight ratio of the matrix glass powder to the filler is (60-90): (10-40).
5. The glass frit of claim 4, wherein the filler comprises:
aluminum titanate, lead titanate, barium titanate, boron nitride, aluminum nitride, silicon nitride, β -eucryptite, leucite, cordierite, zircon, a synthetic pigment of zircon, silica, alumina, titania, zinc oxide, magnesium oxide.
6. A preparation method of a valve plate structure is characterized by comprising the following steps:
mixing the glass frit of any of claims 4-5 with a dispersion to form a paste;
spraying the slurry on the side surface of an unannealed valve block blank, wherein the valve block blank is a zinc oxide material piece;
and sintering the sprayed valve sheet blank to obtain the valve sheet structure with the glass glaze layer.
7. The preparation method of claim 6, wherein the step of sintering the sprayed valve element blank to obtain the valve element structure with the glass glaze layer comprises the following steps:
heating the sprayed valve element blank to 480-580 ℃ and preserving heat at 480-580 ℃;
and cooling the sprayed valve element blank from 480-580 ℃ to obtain the valve plate structure with the glass glaze layer.
8. The method of claim 6, wherein the dispersion comprises ethyl cellulose and a solvent.
9. A valve sheet structure, comprising:
the valve plate is made of zinc oxide material;
the glass glaze layer is coated on the side face of the valve plate;
wherein the glass glaze layer comprises matrix glass powder and a filler, and the matrix glass powder comprises:
0-3% of regulating material, wherein the regulating material comprises NiO and Co2O3、MnO2And CuO;
the weight ratio of the matrix glass powder to the filler is (60-90): (10-40).
10. The valve sheet structure according to claim 9, wherein the filler includes:
aluminum titanate, lead titanate, barium titanate, boron nitride, aluminum nitride, silicon nitride, β -eucryptite, leucite, cordierite, zircon, a synthetic pigment of zircon, silica, alumina, titania, zinc oxide, magnesium oxide.
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| CN114249529A (en) * | 2021-12-06 | 2022-03-29 | 北京北旭电子材料有限公司 | Lithium-aluminum-silicon filler composition, lithium-aluminum-silicon filler and preparation method thereof, glass sealing material and application thereof |
| CN114249529B (en) * | 2021-12-06 | 2024-03-01 | 北京北旭电子材料有限公司 | Lithium aluminum silicon filler composition, lithium aluminum silicon filler and preparation method thereof, glass sealing material and application thereof |
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