CN115073005A - Anti-precipitation LTCC insulating medium slurry - Google Patents
Anti-precipitation LTCC insulating medium slurry Download PDFInfo
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- CN115073005A CN115073005A CN202210856599.3A CN202210856599A CN115073005A CN 115073005 A CN115073005 A CN 115073005A CN 202210856599 A CN202210856599 A CN 202210856599A CN 115073005 A CN115073005 A CN 115073005A
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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
-
- 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
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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
- H01B3/084—Glass or glass wool in binder
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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 an anti-precipitation LTCC insulating medium slurry which comprises the following components in percentage by mass: 55 to 72 percent of glass powder binder phase, 20 to 35 percent of organic carrier,5 to 10 percent of additive and 1 to 5 percent of organic pigment. Wherein the glass powder bonding phase is glass powder obtained by carrying out double-liquid medium refining treatment (firstly water refining and then acetone refining) on Ca-B-Si system glass slag, and the additives are rye powder and ZrO 2 The organic carrier is a mixture with the mass ratio of 2: 1-4: 1 and consists of butyl carbitol acetate, terpineol, lecithin and ethyl cellulose. The dielectric paste has extremely high stability, does not precipitate after being placed for more than 18 days at constant temperature and constant humidity, has uniform color, has the characteristics of high breakdown voltage resistance, high insulation resistance, small dielectric loss and the like, solves the problem of easy precipitation of the dielectric paste, improves the printability and improves the stability of the paste.
Description
Technical Field
The invention belongs to the technical field of dielectric paste, and particularly relates to anti-precipitation LTCC insulating dielectric paste.
Background
LTCC is widely used as a novel technology, and comprises LTCC insulating medium paste, LTCC conductor paste and LTCC resistance paste. LTCC series slurry is widely applied to aerospace, computer communication and electronic industries as a main functional material of electronic components, is mainly prepared by mixing metal powder, a high polymer resin material and other auxiliaries through mechanical force, and physical precipitation generated in the storage process can influence the use performance of the slurry.
In the current application field of LTCC, LTCC insulating medium slurry occupies an important space. Because the LTCC technology has higher printing resolution and can be formed at one time, the LTCC technology can play a role of isolating and insulating the dielectric paste to a greater extent when being applied to the field of the dielectric paste. However, in recent years, the problems bothering users of LTCC dielectric paste are mostly the problem of paste precipitation, and the paste precipitation may cause a series of problems, such as poor printability, blocking of printing screens, low insulation resistance or even no insulation, and further affect the performance of the paste, so that the paste cannot be used normally. Therefore, the problem of easy precipitation of the LTCC dielectric slurry is urgently needed to be solved, the use market of the LTCC dielectric slurry is promoted more quickly, and the LTCC dielectric slurry surpasses other countries.
Disclosure of Invention
The invention aims to provide an anti-precipitation LTCC insulating dielectric paste with high breakdown voltage resistance, high insulation resistance and small dielectric loss.
Aiming at the purposes, the anti-precipitation LTCC insulating medium slurry adopted by the invention is composed of the following raw materials in percentage by mass: 55-72% of glass powder binding phase, 20-35% of organic carrier, 5-10% of additive and 1-5% of organic pigment.
The glass powder binding phase comprises the following components in percentage by mass: 30 to 65 percent of CaO and SiO 2 10%～20%、H 3 BO 3 20%～30%、Al 2 O 3 3%～10%、NiO 1%～5%、TiO 2 1-5%, and the preparation method comprises: CaO and H are mixed 3 BO 3 、SiO 2 、Al 2 O 3 、NiO、TiO 2 After being uniformly mixed, the obtained mixture is placed in a smelting furnace to be smelted for 0.5 to 1 hour at the temperature of 1100 to 1350 ℃ to form glass solution, and the glass solution is processed by waterAnd (3) obtaining glass slag after cold quenching, refining the glass slag for 16-20 hours by using deionized water, then drying, refining the glass slag to the granularity D50 of not more than 1.2 mu m by using acetone, then sieving the glass slag by using a 600-mesh sieve, and drying to obtain the glass powder binding phase.
The additive is rye powder and ZrO 2 The mass ratio of the mixture to the solid is 2: 1-4: 1.
The organic carrier consists of butyl carbitol acetate, terpineol, lecithin and ethyl cellulose, and preferably comprises the following components in percentage by mass: 50-65% of butyl carbitol acetate, 20-25% of terpineol, 5-10% of ethyl cellulose and 5-20% of lecithin.
The organic pigment is a quinacridone pigment or a cobalt blue pigment.
The preparation method of the anti-precipitation LTCC insulating medium slurry comprises the following steps: and (2) mixing the glass powder binding phase, the organic carrier, the additive and the organic pigment according to the mass percentage, mixing after mixing, and rolling until the fineness reaches below 8 mu m to obtain the anti-precipitation LTCC insulating medium slurry.
The invention has the following beneficial effects:
1. in the preparation process of the glass powder binding phase, the glass slag is refined by using double liquids (firstly, deionized water is used for refining, and then acetone is used for refining), so that the particle size distribution of the glass powder is more uniform, and the sintered film after the slurry is printed has better compactness;
2. according to the invention, the mixture of rye powder and zirconia is added into the medium slurry, the carbohydrate contained in the rye powder loses moisture after being heated, and the fine amorphous carbon particles are generated and can be uniformly distributed in the slurry to prevent precipitation, and meanwhile, the stability of the slurry can be greatly improved by introducing the zirconia, which is specifically embodied in the processes of printing, sintering and the like;
3. the dielectric paste has the advantages of high breakdown voltage resistance, high insulation resistance, small dielectric loss, compact surface of a sintered film and the like;
4. the solvent used by the medium slurry carrier is butyl carbitol acetate matched with terpineol, so that the medium slurry carrier has better printing performance and excellent wettability, the glass powder bonding phase and other functional phases in the slurry are uniformly dispersed, and agglomeration and precipitation are avoided.
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 omissions, substitutions, and modifications made by those skilled in the art based on the examples disclosed herein are intended to be included in the scope of the present invention.
1. Preparing a glass powder binding phase: CaO and H are added according to the mass percentage composition and preparation process of glass 1-4 in Table 1 3 BO 3 、SiO 2 、Al 2 O 3 、NiO、TiO 2 Uniformly mixing, putting the obtained mixture into a smelting furnace, keeping the temperature at different temperatures for different times, smelting the mixture into a glass solution, performing water-cooling quenching on the glass solution to obtain glass slag, refining the glass slag for 18 hours by using deionized water, drying the glass slag, refining the glass slag by using acetone until the granularity D50 is less than or equal to 1.2 mu m, sieving the glass slag by using a 600-mesh sieve, and drying the glass slag to obtain the glass powder binding phase. Meanwhile, according to the mass percentage composition and preparation process of the glass 5-6 in the table 1, a comparison test is carried out on the glass powder binding phase obtained by refining the glass slag only by using deionized water or acetone.
TABLE 1 formulation and preparation of glass powder binder phase
Note: the refining medium "water + ketone" in table 1 indicates that the refining is performed first with deionized water and then with acetone.
2. Preparation of organic vehicle: adding butyl carbitol acetate, terpineol and lecithin into a beaker according to the mass percentage in the table 2, stirring and heating to 70 ℃, adding ethyl cellulose, continuously stirring until the ethyl cellulose is completely dissolved, and then preserving heat and stirring for 30 minutes to obtain the organic carrier 1-4.
Table 2 composition of organic vehicle in mass%)
3. Preparing medium slurry: according to the mass percentage in the table 3, after all the components are uniformly mixed, a three-roll mill is used for dispersedly rolling the mixture until the fineness is less than 8 μm, and the medium slurry of the embodiment 1-4 and the comparative example 1-3 is prepared.
TABLE 3 media slurry composition in percent by mass (%)
The dielectric slurries of examples 1 to 4 and comparative examples 1 to 3 were printed on an alumina ceramic substrate by a screen printing process, and relevant performance tests including anti-settling property (time for precipitation to occur when the substrate is left at a constant temperature and humidity), breakdown voltage, insulation resistance, dielectric loss, and whether the surface of a sintered film is dense were performed, and specific results are shown in table 4.
Table 4 dielectric paste performance test results
Note: the surface state of the sintered film is the state which appears after 30 times of 800 ℃ sintering.
As can be seen from the table 3, compared with the comparative examples 1 to 3, the dielectric slurry in the embodiments 1 to 4 of the invention has better anti-precipitation performance, and after 30 times of sintering, the surface of the sintered film is smooth, so that the sintered film has higher breakdown voltage and insulation resistance, and the slurry does not generate precipitation after being placed for 18 days in a constant temperature and humidity room while ensuring extremely low dielectric loss; comparing the dielectric slurry of the example 2, the comparative example 1 and the comparative example 2, the result shows that the anti-precipitation performance of the slurry is better when the glass powder binding phase in the example 2 is refined by deionized water and then acetone; comparing the medium slurry of the example 2 with the medium slurry of the comparative example 3, the addition of the mixture of the rye flour and the zirconia greatly improves the anti-settling property of the slurry; it can be seen from the comprehensive examples 1 and 2 and the comparative examples 1 to 3 that deionized water and acetone are used for carrying out double-liquid refining treatment on Ca-B-Si system glass, and meanwhile, a mixture of rye powder and zirconia is added into a slurry formula, so that the medium slurry has the optimal anti-settling property.
Claims (5)
1. The anti-precipitation LTCC insulating medium slurry is characterized by being prepared from the following raw materials in percentage by mass: 55-72% of glass powder binding phase, 20-35% of organic carrier, 5-10% of additive and 1-5% of organic pigment;
the glass powder binding phase is Ca-B-Si system glass powder obtained by firstly refining glass slag by using water and then refining the glass slag by using acetone until the granularity D50 is less than or equal to 1.2 mu m; wherein the Ca-B-Si system glass powder consists of CaO and H 3 BO 3 、SiO 2 、Al 2 O 3 、NiO、TiO 2 Composition is carried out;
the additive is rye flour and ZrO 2 The mixture is 2: 1-4: 1 in mass ratio;
the organic carrier is composed of butyl carbitol acetate, terpineol, lecithin and ethyl cellulose.
2. The anti-settling LTCC insulation media paste according to claim 1, wherein the Ca-B-Si system glass frit comprises in mass percent: 30 to 65 percent of CaO and SiO 2 10%～20%、H 3 BO 3 20%～30%、Al 2 O 3 3%～10%、NiO 1%～5%、TiO 2 1%～5%。
3. The anti-settling LTCC insulation media paste as claimed in claim 2, wherein the glass frit bonding phase is prepared by: CaO and H are mixed 3 BO 3 、SiO 2 、Al 2 O 3 、NiO、TiO 2 Uniformly mixing the components according to the mass percentage, putting the obtained mixture into a smelting furnace, smelting for 0.5-1 hour at 1100-1350 ℃ to obtain a glass solution, performing water cooling quenching on the glass solution to obtain glass slag, refining the glass slag for 16-20 hours by using deionized water, drying, refining by using acetone until the granularity D50 is less than or equal to 1.2 mu m, sieving by using a 600-mesh sieve, and drying to obtain a glass powder binding phase.
4. The anti-settling LTCC insulation media slurry according to claim 1, wherein the organic vehicle comprises, in mass percent: 50-65% of butyl carbitol acetate, 20-25% of terpineol, 5-10% of ethyl cellulose and 5-20% of lecithin.
5. The anti-settling LTCC insulation media paste according to claim 1, wherein the organic pigment is a quinacridone pigment or a cobalt blue pigment.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210856599.3A CN115073005B (en) | 2022-07-21 | 2022-07-21 | Anti-precipitation LTCC insulating medium slurry |
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| CN202210856599.3A CN115073005B (en) | 2022-07-21 | 2022-07-21 | Anti-precipitation LTCC insulating medium slurry |
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| CN115073005B CN115073005B (en) | 2022-11-08 |
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| CN106007804A (en) * | 2016-05-18 | 2016-10-12 | 中国人民解放军国防科学技术大学 | Radar wave-absorbing material with high-temperature-resistant and high-impedance surface and preparation method of radar wave-absorbing material |
| CN109161331A (en) * | 2018-07-27 | 2019-01-08 | 上海交通大学 | The resistance to ablative coatings of ceramic screw fiber reinforcement silicon rubber lightweight and its application |
| CN110028057A (en) * | 2019-01-31 | 2019-07-19 | 广东思泉新材料股份有限公司 | A kind of graphene slurry and preparation method thereof with Investigation of stabilized dispersion of nano |
| CN112499977A (en) * | 2020-11-30 | 2021-03-16 | 华东理工大学 | Superfine silicate glass powder and preparation method thereof |
| CN113436783A (en) * | 2021-08-27 | 2021-09-24 | 西安宏星电子浆料科技股份有限公司 | Preparation method of LTCC (Low temperature Co-fired ceramic) dielectric slurry transparent after casting and sintering |
-
2022
- 2022-07-21 CN CN202210856599.3A patent/CN115073005B/en active Active
Patent Citations (8)
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|---|---|---|---|---|
| CN101560060A (en) * | 2009-05-08 | 2009-10-21 | 苏州晶讯科技股份有限公司 | Surface treatment method of low temperature glass for solar cell conductive slurry |
| US20110186336A1 (en) * | 2010-01-29 | 2011-08-04 | Asahi Glass Company, Limited | Substrate for mounting element and process for its production |
| CN102831949A (en) * | 2012-08-24 | 2012-12-19 | 合肥中南光电有限公司 | Efficient lead-free silver paste on back of solar cell and preparation method of silver paste |
| CN106007804A (en) * | 2016-05-18 | 2016-10-12 | 中国人民解放军国防科学技术大学 | Radar wave-absorbing material with high-temperature-resistant and high-impedance surface and preparation method of radar wave-absorbing material |
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