CN114933414B - Temperature sensitivity resistant LTCC insulating medium slurry - Google Patents
Temperature sensitivity resistant LTCC insulating medium slurry Download PDFInfo
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- CN114933414B CN114933414B CN202210875591.1A CN202210875591A CN114933414B CN 114933414 B CN114933414 B CN 114933414B CN 202210875591 A CN202210875591 A CN 202210875591A CN 114933414 B CN114933414 B CN 114933414B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/20—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
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- 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
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- 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
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/002—Inhomogeneous material in general
- H01B3/006—Other inhomogeneous material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/08—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances quartz; glass; glass wool; slag wool; vitreous enamels
- H01B3/087—Chemical composition of glass
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/10—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances metallic oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/185—Substances or derivates of cellulose
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/307—Other macromolecular compounds
Abstract
The invention discloses temperature sensitivity resistant LTCC insulating medium slurry, which adopts Zn-B-Si system glass powder subjected to modification treatment by poly-N-isopropylacrylamide as a binding phase, adopts triisopropyl borate, oleic acid and methyl cellulose to prepare an organic carrier, and adds niobium pentoxide, titanium dioxide, zirconium oxide and the like as oxide additives to further enhance the stability and durability of the slurry. The dielectric paste has the advantages of small thermal expansion coefficient, small temperature coefficient of resonance frequency, high breakdown voltage resistance, high insulation resistance, compact surface of a sintered film and the like, can reduce the sensitivity to temperature when being applied to the field of LTCC dielectric paste, enables the LTCC dielectric paste to adapt to different temperature environments, reduces the use limitation, correspondingly prolongs the service life, and has obvious economic benefit.
Description
Technical Field
The invention belongs to the technical field of dielectric paste, and particularly relates to temperature sensitivity resistant LTCC insulating dielectric paste.
Background
The LTCC technology is a novel multilayer substrate process technology emerging in the last 80 years, has higher sintering temperature, can be co-fired with various metals such as gold, silver, palladium and the like, and also enables the LTCC technology to be developed in the direction of diversification, miniaturization and high reliability, including LTCC medium slurry, LTCC conductor slurry, LTCC resistance slurry and the like. The related technology of the LTCC dielectric paste is characterized in that the conductor paste and the resistor paste are matched with the excellent insulation property of the LTCC dielectric paste, so that the application fields of the LTCC dielectric paste are quite wide, including the fields of drivers, inductors, sensors, filters, military aerospace, automobile electronics and the like, but the LTCC dielectric paste has a long preparation period and is easy to volatilize in components, and products deviate from expected compositions and form a multi-phase structure after sintering, so that the performance can be degraded and unstable. The most of the existing problems are caused by the temperature sensitivity of the dielectric slurry, and further influence the use of the whole substrate. In complex environments such as high temperature, low temperature and high and low temperature alternation, the properties such as the viscosity of the slurry are changed due to the temperature change, and the service performance of the slurry is further influenced. Therefore, the problem of avoiding or improving the temperature sensitivity resistance of the LTCC insulating medium slurry is difficult in the industry, and needs to be solved urgently.
Disclosure of Invention
The invention aims to provide the temperature sensitivity resistant LTCC insulating medium paste which has the advantages of small thermal expansion coefficient, small temperature coefficient of resonance frequency, high breakdown voltage resistance, high insulating resistance and compact surface of a sintering film.
Aiming at the purposes, the temperature sensitivity resistant LTCC insulating medium slurry adopted by the invention is composed of the following raw materials in percentage by mass: 55-75% of modified glass powder, 20-35% of organic carrier and 5-10% of oxide additive.
The modified glass powder is obtained by putting Zn-B-Si system glass powder into a poly N-isopropylacrylamide aqueous solution with the mass concentration of 20 percent, soaking for 5 to 10 hours, drying and sieving. The Zn-B-Si system glass powder comprises the following components in percentage by mass: 40-65% of zinc oxide, 10-20% of silicon dioxide, 20-30% of boric anhydride and 5-10% of zirconium oxide. The preparation method comprises the following steps: uniformly mixing zinc oxide, boric anhydride, silicon dioxide and zirconium oxide according to mass percent, putting the obtained mixture into a smelting furnace, smelting for 1-2 hours at 1300-1500 ℃ to obtain glass solution, carrying out air cooling quenching on the glass solution to obtain glass slag, refining the glass slag until the granularity D50 is less than or equal to 1.6 mu m, sieving the glass slag by a 600-mesh sieve, and drying.
The oxide additive is one or more of niobium pentoxide, cadmium trioxide and titanium dioxide.
The organic carrier consists of triisopropyl borate, oleic acid and methyl cellulose, and preferably comprises the following components in percentage by mass: 70-90% of triisopropyl borate, 5-15% of methyl cellulose and 5-20% of oleic acid.
The preparation method of the LTCC insulating medium slurry comprises the following steps: and (2) mixing the modified glass powder, the organic carrier and the oxide additive according to the mass percentage, mixing after mixing, and rolling until the fineness reaches below 10 mu m to obtain the LTCC insulating medium slurry.
The invention has the following beneficial effects:
1. the preparation process of the modified glass powder in the LTCC insulating medium slurry adopts an air cooling mode for quenching, the operation is convenient, the internal stress generated by water quenching is avoided, and certain guarantee is provided for the subsequent slurry printing and use;
2. after being modified by poly N-isopropyl acrylamide, zn-B-Si series glass powder used by the LTCC insulating medium slurry can form temperature sensitivity resistant hydrogel when being applied to the medium slurry, the temperature sensitivity resistant hydrogel has a certain proportion of hydrophilic groups and hydrophobic groups, and the change of temperature can influence the interaction of the groups in water molecules and among molecules, so that the internal network structure is adjusted, the sensitivity of the temperature sensitive hydrogel to the temperature is reduced, the temperature sensitive hydrogel adapts to different use temperature environments, the use limitation of the temperature sensitive hydrogel is reduced, the service life of the temperature sensitive hydrogel is correspondingly prolonged, and obvious economic benefits are achieved;
3. the LTCC insulating medium slurry has the advantages of small thermal expansion coefficient, small temperature coefficient of resonance frequency, high breakdown voltage resistance, high insulating resistance, compact surface of a sintered film and the like;
4. the Zn-B-Si glass powder used in the invention has high zinc oxide content and a certain amount of zirconium oxide is added, thus improving the crystallization capacity of the glass and ensuring the sintering stability.
Detailed Description
The present invention is described in detail with reference to the following examples, but the scope of the present invention is not limited to the following examples, and any omission, replacement, or modification made by those skilled in the art based on the examples of the present invention disclosed herein will be included in the scope of the present invention.
Preparing modified glass powder: according to the mass percentages and the process conditions shown in the table 1, after various oxides are uniformly mixed, the obtained mixture is placed in a high-temperature smelting furnace to be smelted at different temperatures and different times, the obtained molten glass is cooled by air and then crushed into glass slag, the glass slag is refined to different particle sizes, and then the glass slag is screened by a 600-mesh screen and dried to obtain Zn-B-Si series glass powder; and then putting the Zn-B-Si system glass powder into a poly N-isopropylacrylamide aqueous solution with the mass concentration of 20 percent to be soaked for different time, drying and sieving to obtain glass 1-9 which are respectively used as modified glass powder.
TABLE 1 modified glass powder formulation and preparation Process parameters
Preparation of organic vehicle: triisopropyl borate (or terpineol) and oleic acid are stirred and heated to 70 ℃ in a beaker, then methyl cellulose is added and stirred continuously until the methyl cellulose is completely dissolved, and then the mixture is stirred for 30 minutes under the condition of heat preservation to obtain the organic carrier.
Preparing medium slurry: after all the components were uniformly mixed in the mass percentages shown in table 2, the media slurries of examples 1 to 7 and comparative examples 1 to 4 were prepared by dispersion rolling with a three-roll mill until the fineness was less than 10 μm.
TABLE 2 Medium size mass percent (%)
The dielectric slurries of examples 1 to 7 and comparative examples 1 to 4 were printed on a 96% alumina ceramic substrate by a screen printing process, and the related performance tests including the thermal expansion coefficient, the temperature coefficient of resonance frequency, the breakdown voltage, the insulation resistance, whether the surface of the sintered film is dense, etc. were performed, and the specific results are shown in table 3.
TABLE 3 slurry Performance test results
Note: the surface state of the sintered film in the table is a state exhibited after 30 times of sintering at 850 ℃. The rapid temperature change experiment is used for determining the storage, transportation and use adaptability of the product in the environment with rapid or slow change of high temperature and low temperature, the experiment process takes normal temperature → low temperature stay → high temperature stay → normal temperature as a cycle, and the temperature sensitivity is judged by observing the state and performance indexes such as related viscosity and the like.
As can be seen from Table 3, the dielectric slurries of the embodiments 1 to 7 of the invention have better temperature sensitivity resistance, and after 30 times of sintering, the sintered film has a flat surface, higher breakdown voltage and insulation resistance, and meanwhile, the sensitivity to temperature is greatly reduced, and the thermal expansion coefficient and the temperature coefficient of resonance frequency are both kept at lower levels; compared with the medium slurry in the comparative example 1, the medium slurry in the example 3 has better performance after the glass powder is modified by using the poly N-isopropylacrylamide aqueous solution with the mass concentration of 20%; comparing the dielectric slurry of example 3 with the dielectric slurry of comparative example 4, the effect of using triisopropyl borate as a solvent in an organic carrier is better than that of a conventional solvent terpineol; it can be seen from the combination of examples 1 and 3 and comparative examples 1 to 3 that when the glass powder is modified by using an aqueous solution of poly-N-isopropylacrylamide with a mass concentration of 20% and the carrier uses triisopropyl borate instead of terpineol, the medium slurry has the best temperature sensitivity resistance.
Claims (3)
1. The temperature sensitivity resistant LTCC insulating medium slurry is characterized by being prepared from the following raw materials in percentage by mass: 55-75% of modified glass powder, 20-35% of organic carrier and 5-10% of oxide additive;
the modified glass powder is obtained by modifying Zn-B-Si system glass powder by using a poly N-isopropyl acrylamide aqueous solution with the mass concentration of 20%; wherein the Zn-B-Si system glass powder consists of zinc oxide, boron anhydride, silicon dioxide and zirconium oxide, and the preparation method comprises the following steps: uniformly mixing zinc oxide, boric anhydride, silicon dioxide and zirconium oxide according to mass percentage, putting the obtained mixture into a smelting furnace, smelting for 1-2 hours at 1300-1500 ℃ to obtain glass solution, carrying out air cooling quenching on the glass solution to obtain glass slag, refining the glass slag until the granularity D50 is less than or equal to 1.6 mu m, sieving the glass slag with a 600-mesh sieve, and drying to obtain Zn-B-Si system glass powder;
the organic carrier consists of triisopropyl borate, oleic acid and methyl cellulose, and the organic carrier comprises the following components in percentage by mass: 70-90% of triisopropyl borate, 5-15% of methyl cellulose and 5-20% of oleic acid;
the oxide additive is one or a mixture of more of niobium pentoxide, cadmium trioxide and titanium dioxide.
2. The temperature-sensitive LTCC insulation dielectric paste as claimed in claim 1, wherein the Zn-B-Si system glass frit consists of, by mass: 40-65% of zinc oxide, 10-20% of silicon dioxide, 20-30% of boric anhydride and 5-10% of zirconium oxide.
3. The temperature-sensitive LTCC insulation dielectric paste as claimed in claim 1, wherein the preparation method of the modified glass powder comprises: and (3) putting the Zn-B-Si system glass powder into a poly N-isopropylacrylamide aqueous solution with the mass concentration of 20 percent, soaking for 5 to 10 hours, drying and sieving to obtain the modified glass powder.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106098140A (en) * | 2016-05-23 | 2016-11-09 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of PTC thermistor slurry based on stainless steel substrate and preparation method thereof |
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| US5997961A (en) * | 1998-03-06 | 1999-12-07 | Battelle Memorial Institute | Method of bonding functional surface materials to substrates and applications in microtechnology and antifouling |
| CN1243355C (en) * | 2003-02-27 | 2006-02-22 | 京东方科技集团股份有限公司 | Insulating slurry for manufacturing insulating layer of vacuum fluorescent display, and preparation method thereof |
| CN103435830B (en) * | 2013-09-02 | 2016-03-02 | 苏州大学张家港工业技术研究院 | A kind of method of modifying of functionalizing material surface |
| CN112499977B (en) * | 2020-11-30 | 2023-03-31 | 华东理工大学 | Superfine silicate glass powder and preparation method thereof |
| CN113540277B (en) * | 2021-08-04 | 2022-08-12 | 周丽 | Intelligent adjustable energy-saving glass and preparation method thereof |
| CN113555146B (en) * | 2021-09-22 | 2021-12-21 | 西安宏星电子浆料科技股份有限公司 | High-acid-resistance medium slurry |
| CN113903497B (en) * | 2021-12-09 | 2022-03-08 | 西安宏星电子浆料科技股份有限公司 | Isolation medium slurry and preparation method thereof |
| CN114255908B (en) * | 2022-03-01 | 2022-05-17 | 西安宏星电子浆料科技股份有限公司 | Acid and alkali resistant salt-fog-resistant medium slurry and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106098140A (en) * | 2016-05-23 | 2016-11-09 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of PTC thermistor slurry based on stainless steel substrate and preparation method thereof |
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