CN116119934A - NTC thermistor coated glass powder and preparation method thereof - Google Patents

NTC thermistor coated glass powder and preparation method thereof Download PDF

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Publication number
CN116119934A
CN116119934A CN202310151299.XA CN202310151299A CN116119934A CN 116119934 A CN116119934 A CN 116119934A CN 202310151299 A CN202310151299 A CN 202310151299A CN 116119934 A CN116119934 A CN 116119934A
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glass
ntc thermistor
glass powder
layer
mgo
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尹梦迪
尹嘉琦
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Jiangsu Hongpu Electronic Material Technology Co ltd
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Jiangsu Hongpu Electronic Material Technology Co ltd
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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
    • C03C12/00—Powdered glass; Bead compositions
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Thermistors And Varistors (AREA)

Abstract

The invention relates to the technical field of glass, and particularly discloses NTC thermistor coated glass powder and a preparation method thereof, wherein the preparation method comprises the following steps: weighing and mixing the raw materials to obtain a mixture, wherein the following raw materials comprise the following components in percentage by weight: 20% -50% of CaO, 10% -40% of MgO, 10% -40% of SiO2, 1% -30% of B2O3, 0% -5% of ZrO2, 0% -5% of Al2O3 and 0% -5% of La2O3, and after the glass powder is subjected to using, processing and coating, the color of a sintered glass layer is transparent, the temperature resistance is high, the porosity of the glass is improved, a compact, cracking-free and breakage-free glass protective layer is formed, other processes in the subsequent processing process cannot be caused to damage the glass layer, the surface of the NTC thermistor is wrapped and protected, the production detection requirement of the NTC thermistor is met, the corrosion resistance of the glass layer is improved, the chemical stability is good, the raw material is simple, the glass powder is easy to obtain, the manufacturing cost is low, and the environmental protection performance is good.

Description

NTC thermistor coated glass powder and preparation method thereof
Technical Field
The invention relates to the technical field of glass, in particular to NTC thermistor coated glass powder and a preparation method thereof.
Background
The Negative Temperature Coefficient (NTC) thermistor material is an important composite metal oxide ceramic material with definite application value, NTC refers to thermistor phenomenon and material with negative temperature coefficient, the resistance of which is exponentially reduced along with the rising of temperature, wherein one of the key technologies is NTC thermistor material, the material is prepared by taking metal oxides such as manganese, cobalt, nickel, copper and the like as main raw materials and adopting a solid-phase oxide method, a common ternary system comprises MnCoNi, mnCoFe, mnNiAl and the like, a common quaternary system comprises MnCoNiAl, mnCoFeNi and the like, the resistivity range of the NTC thermistor material is 2.5-700 KOmegamm, and the B25/50 is 3380-4700K.
The glass powder is inorganic amorphous hard particle powder, is usually used as a high-transparency high-hardness filling material, is prepared by uniformly mixing electronic-grade raw materials such as PbO, siO2, tiO2 and the like, and then carrying out solid phase reaction at high temperature to form a glass homogeneous body with a disordered structure, has stable chemical property, and has acid resistance far exceeding that of lead oxide, but is formed by being converted into oxide according to common practice in chemical composition expression, such as: pbO, siO2, etc.
The current NTC thermistor manufacturing process comprises the following steps: the NTC heat-sensitive ceramic powder is manufactured according to the technological processes of material proportioning, pulping and casting, lamination, static pressure, cutting, glue discharging and sintering, chamfering, epoxy end sealing, coating, glass burning, chamfering, end electrode plating, test sorting, braiding, and has the functions of connection, sealing and the like.
The existing NTC thermistor and glass powder cannot be well matched in the coating and vitrification processes, so that a glass protection layer with uneven cracking and defects is formed, defective products are formed, and the electrical property of the NTC thermistor is inflexible when subsequent electroplating is carried out.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides NTC thermistor coated glass powder and a preparation method thereof, which are used for solving the problems in the prior art.
The invention provides the following technical scheme: an NTC thermistor coated glass frit comprising; weighing and mixing the raw materials to obtain a mixture, wherein the following raw materials comprise the following components in percentage by weight: caO of 20%
About 50 percent of MgO, 10 to 40 percent of SiO 2 10% -40%, B 2 O 3 1 to 30 percent of ZrO2, 0 to 5 percent of Al2O 3 0 to 5 percent of La 2 O 3 0 to 5 percent of the glass, na and K are not needed to be added, mgO and CaO are not easy to volatilize at high temperature, so that unstable performance of the glass caused by volatilization of Na and K at high temperature is avoided, the chemical stability of the glass is better,
further, the glass raw material generates Ca in use when optimizing the glass formulation 2 Si，Ca 2 MgO 7 Si 2 ，CaSi 2 O 5， Mg 2 B 2 O 5 ，MgSiO 3 CaO-MgO-SiO of (2) 2 -B 2 O 3 The crystallization phase has high expansion coefficient and stable expansion coefficient, and meets the sealing requirement of glass.
Further, the MgO is CaO-MgO-SiO-forming 2 -B 2 O 3 The essential components of the crystal are favorable for improving the heat-resistant stability of the glass, and SiO 2 The glass powder is very important for melting glass, the melting temperature of the glass can be reduced by adding the glass powder, the porosity of the glass is improved, the thermal expansion coefficient of the glass powder is 10.95 ppm/DEG C-11.65 ppm/DEG C, the sintering can be realized at 1000-1400 ℃, and the glass layer obtained after the sintering is transparent.
A preparation method of NTC thermistor coated glass powder comprises the following steps: the glass powder is obtained by taking materials according to the proportion, mixing, smelting, water quenching, drying, grinding and screening.
S1, smelting, namely putting the mixed raw materials into a high-temperature smelting furnace, keeping the temperature of 1300-1500 ℃ for smelting for a specified time, and smelting into uniform glass liquid.
S2, rolling the glass into 0.5mm broken sheets by using the heat-resistant stainless steel water cooling continuous sheet rolling machine, quenching, and drying.
And S3, screening, namely using a jadeite tank ball mill to crush the glass powder which is screened by a 200-250 mesh screen.
Further, the glass paste prepared by the screened glass powder, the adhesive, the solvent and other materials and ball-milled is coated on the surface of the NTC thermistor by adopting a dip coating method, a spray coating method or a printing method, wherein the prepared glass paste is coated with a layer of 10-50 mu m, and the original piece coated with the glass paste is sintered in a mesh belt type sintering furnace or a box type sintering furnace, so that a compact glass protection layer is formed on the glass paste layer, the thickness of a glass packaging layer is controlled to be 10-30 mu m, and a compact glass wrapping layer is formed on the surface of the NTC thermistor.
Further, the adhesive and the solvent comprise propyl acetate, isobutanol, a dispersing agent, polymethyl methacrylate and a plasticizer, and the adhesive and the solvent are subjected to batching and ball milling to obtain the adhesive with the density of 1.15+/-0.2 g/cm 3 Is a glass paste of (a);
further, the adding amounts of the propyl acetate, the isobutanol, the dispersing agent, the polymethyl methacrylate and the plasticizer respectively account for the weight percentage of the glass powder: 70% -80%, 50% -65%, 1%, 10.5%, 13.5%; the granularity of the glass powder in the glass slurry is 1.8+/-0.2 mu m.
The invention has the technical effects and advantages that:
1. after the glass powder is used for processing and coating, the color of the sintered glass layer is transparent, the temperature resistance is high, the porosity of the glass is improved, a compact, cracking-free and breakage-free glass protection layer is formed, other processes cannot damage the glass layer in the subsequent processing process, the surface of the NTC thermistor is wrapped and protected, the production detection requirement is met, the corrosion resistance of the glass layer is improved, and the chemical stability is good.
2. The invention has the advantages of simple raw materials, easy acquisition, low manufacturing cost and good environmental protection.
Drawings
Fig. 1 is a flowchart of the preparation of the NTC thermistor coated glass frit of the present invention.
Detailed Description
The embodiments of the present invention will be clearly and completely described below with reference to the drawings in the present invention, and the forms of the structures described in the following embodiments are merely examples, and the NTC thermistor coated glass powder and the preparation method thereof according to the present invention are not limited to the structures described in the following embodiments, and all other embodiments obtained by a person having ordinary skill in the art without making any inventive effort are within the scope of the present invention.
In one embodiment, the present invention provides an NTC thermistor coated glass frit comprising; weighing and mixing the raw materials to obtain a mixture, wherein the following raw materials comprise the following components in percentage by weight: 20 to 50 percent of CaO, 10 to 40 percent of MgO and SiO 2 10% -40%, B 2 O 3 1 to 30 percent of ZrO2, 0 to 5 percent of Al2O 3 0 to 5 percent of La 2 O 3 0% -5%, na and K are not needed to be added, mgO and CaO are not easy to volatilize at high temperature, so that unstable performance of the glass caused by volatilization of Na and K at high temperature can be avoided, and the chemical stability of the glass is better;
in a preferred embodiment, optimization of the glass formulation, in use, generates Ca 2 Si，Ca 2 MgO 7 Si 2 ，CaSi 2 O 5 ，Mg 2 B 2 O 5 ，MgSiO 3 CaO-MgO-SiO of (2) 2 -B 2 O 3 The crystallization phase has high expansion coefficient and stable expansion coefficient, and can meet the sealing requirement of glass
In a preferred embodiment, the MgO is CaO-MgO-SiO-forming 2 -B 2 O 3 The essential components of the crystal are favorable for improving the heat-resistant stability of the glass, and SiO 2 The glass powder is very important for glass melting, the addition can reduce the melting temperature of the glass, and is also beneficial to improving the porosity of the glass, the thermal expansion coefficient of the glass powder is 10.95 ppm/DEG C-11.65 ppm/DEG C, the sintering can be realized at 1000-1400 ℃, and the glass layer obtained after the sintering is transparent.
In another embodiment, a method for preparing an NTC thermistor coated glass frit includes the steps of: the glass powder is obtained by taking materials according to the proportion, mixing, smelting, water quenching, drying, grinding and screening.
S1, smelting, namely putting the mixed raw materials into a high-temperature smelting furnace, keeping the temperature of 1300-1500 ℃ for smelting for a specified time, and smelting into uniform glass liquid.
S2, rolling the glass into 0.5mm broken sheets by using the heat-resistant stainless steel water cooling continuous sheet rolling machine, quenching, and drying.
And S3, screening, namely using a jadeite tank ball mill to grind the glass powder which is screened by a 200-250 mesh sieve.
In a preferred embodiment, the glass powder, the adhesive, the solvent and other materials are prepared and ball-milled to obtain glass slurry, a layer of 10-50 μm prepared glass slurry is coated on the surface of the NTC thermistor by adopting a dip coating method, a spray coating method or a printing method, and the original piece coated with the glass slurry is sintered in a mesh belt type sintering furnace or a box type sintering furnace to form a compact glass protection layer on the glass slurry layer, the thickness of a glass packaging layer is controlled to be 10-30 μm, so that a compact glass packaging layer is obtained on the surface of the NTC thermistor.
In a preferred embodiment, the binder is ball milled with a solvent comprising propyl acetate, isobutanol, a dispersant, polymethyl methacrylate, a plasticizer to a density of 1.15.+ -. 0.2g/cm 3 Is a glass paste of (a);
in a preferred embodiment, the adding amounts of the propyl acetate, the isobutanol, the dispersing agent, the polymethyl methacrylate and the plasticizer respectively account for the weight percentage of the glass powder: 70% -80%, 50% -65%, 1%, 10.5% and 13.5%; the granularity of the glass powder in the glass slurry is 1.8+/-0.2 mu m.
Figure BDA0004090867620000051
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Figure BDA0004090867620000061
TABLE 1 material proportions
Figure BDA0004090867620000062
TABLE 2 coefficient of thermal expansion
The thermal expansion coefficient of the glass is 10.95 ppm/DEG C-11.65 ppm/DEG C, the thermal expansion coefficient is larger, the glass paste is well matched with the NTC thermistor in the vitrification process to form a compact transparent glass protective layer which is free from cracking and breakage, the appearance requirement is met, and meanwhile, the requirements of good temperature resistance, high electrical stability, plating solution corrosion resistance and the like are met.

Claims (7)

1. An NTC thermistor coated glass frit comprising: weighing and mixing the raw materials to obtain a mixture, wherein the following raw materials comprise the following components in percentage by weight: 20 to 50 percent of CaO, 10 to 40 percent of MgO and SiO 2 10% -40%, B 2 O 3 1 to 30 percent of ZrO2, 0 to 5 percent of Al2O 3 0 to 5 percent of La 2 O 3 0 to 5 percent.
2. The NTC thermistor coated glass powder according to claim 1, characterized in that: the glass raw material generates Ca in use when optimizing a glass formula 2 Si，Ca 2 MgO 7 Si 2 ，CaSi 2 O 5 ，Mg 2 B 2 O 5 ，MgSiO 3 CaO-MgO-SiO of (2) 2 -B 2 O 3 The crystallization phase has high expansion coefficient and stable expansion coefficient, and meets the sealing requirement of glass.
3. The NTC thermistor coated glass powder according to claim 1, characterized in that: the MgO is CaO-MgO-SiO-forming 2 -B 2 O 3 The essential components of the crystal are favorable for improving the heat-resistant stability of the glass, and SiO 2 The addition of the glass powder is very important for melting glass, can reduce the melting temperature of the glass, is beneficial to improving the porosity of the glass, and has the thermal expansion coefficient of 10.95 ppm/DEG C to 11.65 ppm/DEG C, and can be used for melting the glassSintering is realized at 1000-1400 ℃, and the glass layer obtained after sintering is transparent.
4. A method for preparing an NTC thermistor coated glass frit according to claims 1-3, comprising the steps of: the glass powder is obtained by taking materials according to the proportion, mixing, smelting, water quenching, drying, grinding and screening.
S1, smelting, namely putting the mixed raw materials into a high-temperature smelting furnace, keeping the temperature of 1300-1500 ℃ for smelting for a specified time, and smelting into uniform glass liquid.
S2, rolling the glass into 0.5mm broken sheets by using the heat-resistant stainless steel water cooling continuous sheet rolling machine, quenching, and drying.
And S3, screening, namely using a jadeite tank ball mill to crush the glass powder which is screened by a 200-250 mesh screen.
5. The method for preparing the NTC thermistor coated glass powder according to claim 4, wherein the method comprises the following steps: and (3) coating a layer of glass slurry which is prepared by 10-50 mu m on the surface of the NTC thermistor by adopting a dip coating method, a spray coating method or a printing method, wherein the original piece coated with the glass slurry is sintered in a mesh belt type sintering furnace or a box type sintering furnace, so that a compact glass protection layer is formed on the glass slurry layer, the thickness of a glass packaging layer is controlled to be 10-30 mu m, and a compact glass packaging layer is formed on the surface of the NTC thermistor.
6. The method for preparing the NTC thermistor coated glass powder according to claim 4, wherein the method comprises the following steps: the adhesive and the solvent comprise propyl acetate, isobutanol, a dispersing agent, polymethyl methacrylate and a plasticizer, and the density is 1.15+/-0.2 g/cm 3 Is used for the glass paste.
7. The method for preparing the NTC thermistor coated glass powder according to claim 4, wherein the method comprises the following steps: the adding amounts of the propyl acetate, the isobutanol, the dispersing agent, the polymethyl methacrylate and the plasticizer respectively account for the weight percentage of the glass powder: 70% -80%, 50% -65%, 1%, 10.5%, 13.5%; the granularity of the glass powder in the glass slurry is 1.8+/-0.2 mu m.
CN202310151299.XA 2023-02-22 2023-02-22 NTC thermistor coated glass powder and preparation method thereof Pending CN116119934A (en)

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