CN112920641A - Additive for metallized sealing composite material - Google Patents
Additive for metallized sealing composite material Download PDFInfo
- Publication number
- CN112920641A CN112920641A CN201911231167.8A CN201911231167A CN112920641A CN 112920641 A CN112920641 A CN 112920641A CN 201911231167 A CN201911231167 A CN 201911231167A CN 112920641 A CN112920641 A CN 112920641A
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- CN
- China
- Prior art keywords
- terpineol
- additive
- parts
- auxiliary agent
- ethyl cellulose
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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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
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
-
- 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
- C04B41/88—Metals
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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)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses an additive for a metallized sealing composite material, which comprises an SA auxiliary agent, terpineol and ethyl cellulose, wherein the weight ratio of the SA auxiliary agent to the terpineol is 25: (60-90) preparing a terpineol solvent, and preparing the additive from the ethyl cellulose and the terpineol solvent according to the weight ratio of (30-45): 1000; the SA auxiliary agent is formed by mixing butyl carbitol, tributyl citrate, isobutyl alcohol and castor oil, and the weight percentage of each component is as follows: butyl carbitol: 45-70%, tributyl citrate: 10-30% of isobutanol: 7-15%; castor oil: 5 to 12 percent. Through developing the composite additive mixed by terpineol, ethyl cellulose and SA auxiliary agent, the fluidity and uniformity of the screen printing metal slurry are improved, and the metal powder is ensured to be uniformly and flatly coated on the surface of the ceramic.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to an additive for a metallized sealing composite material.
Background
Ceramics having electrical and magnetic properties can be used in the electronics industry and are called electronic ceramics. The electronic ceramic is a ceramic with new functions finally obtained through controlling the surface, grain boundary and size structure. Can be widely applied to the aspects of energy sources, household appliances, automobiles and the like. Ceramic is a good insulating material, usually solder cannot wet the ceramic, so direct sealing cannot be realized, and the solution is to firmly sinter a layer of metal film on the surface of the ceramic, which is called ceramic metallization. At present, the Mo-Mn activating method is a widely applied ceramic metallization process, and the key process of ceramic metallization is to print a metal film on a 95 alumina ceramic substrate, and the printing paste is required to ensure enough fluidity so that the printed metal layer is uniform and flat. And the printing effect of the metal paste is determined to the maximum extent by selecting proper paste additives.
The paste additive generally adopts an organic vehicle, is an important composition of the printing metal paste, and comprises a binder, a solvent and the like. Although temporary, should be evaporated as much as possible after sintering of the thick film. However, it is important to do so throughout the entire screen printing process. It significantly affects many parameters of thick film processing and performance. In the early ceramic metallization technology applied in the technical field of vacuum electronics, the research and development of the formula composition and the performance of metal and glass phases in the thick-film paste are emphasized comparatively, and therefore, a plurality of scientific achievements are obtained. However, to date, as the field of application continues to be developed and the requirements for thick film properties increase, paste additives have been considered and increased with the requirements of the application.
When the molybdenum-manganese method is adopted to produce and manufacture metallized ceramics in China, ethyl cellulose is generally adopted as a binder and terpineol is adopted as a solvent for preparing the screen printing paste, and the ethyl cellulose and the terpineol are mixed in different proportions to form the additive. The carrier is simple and single, but has poor manufacturability, and microscopically reflects that the slurry composition is often uneven and the dispersion is not good. The sintered thick film develops porosity and microcracks. Macroscopically, the sealing strength is poor, the air tightness is not good enough, and the like.
Disclosure of Invention
In order to solve the problems in the prior art, the embodiment of the invention provides an additive for a metallization sealing composite material. The technical scheme is as follows:
the invention provides an additive for a metallized sealing composite material, which comprises an auxiliary agent, terpineol and ethyl cellulose,
the auxiliary agent and the terpineol are mixed according to the weight ratio of 15: (75-90) preparing a terpineol solvent, wherein the additive is prepared from the ethyl cellulose and the terpineol solvent according to the weight ratio of (20-30): 100;
the auxiliary agent is formed by mixing butyl carbitol, tributyl citrate, isopropanol and tea seed oil, and the auxiliary agent comprises the following components in parts by weight: 10-15 parts of butyl carbitol, 5-10 parts of tributyl citrate, 2-5 parts of isopropanol and 1-3 parts of tea seed oil.
Further, the auxiliary agent is formed by mixing butyl carbitol, tributyl citrate, isobutyl alcohol and tea seed oil, and the auxiliary agent comprises the following components in parts by weight: 9 parts of butyl carbitol, 7 parts of tributyl citrate, 3 parts of isopropanol and 2 parts of tea seed oil.
The preparation method of the additive comprises the following steps:
step one, preparation of an auxiliary agent:
s11, weighing the components according to the preset proportion of the auxiliary agents, sequentially adding the components into a glass bottle, tightly covering the glass bottle cover, continuously shaking the glass bottle for 2-3 minutes, and continuously rolling the glass bottle during shaking;
s12, placing the shaken glass bottle on a ball milling frame with an environment temperature control function for ball milling, wherein the environment temperature is controlled to be 48-50 ℃, and the ball milling time is 20-28 hours;
s13, taking down the glass bottle, and cooling for standby application, wherein the standby application time is not more than 7 days;
step two, preparation of terpineol alcohol solvent: taking the adjuvant prepared in the step one and terpineol according to the weight ratio of 15: (75-90) uniformly mixing to prepare a terpineol solvent for later use;
step three, preparation of an additive:
s31, weighing ethyl cellulose and the terpineol solvent according to the weight ratio (20-30): 100, putting the terpineol solvent into a 2L ground glass bottle, and separately containing the ethyl cellulose by using wax paper;
s32, placing the ground glass bottle filled with the terpineol alcohol solvent and the wax paper filled with the ethyl cellulose in a constant-temperature oven at 100 ℃ for preheating for 1 hour, wherein the oven is a stainless steel band hot air circulation oven, and the set temperature is 100 ℃;
s33, taking the terpineol alcohol solvent and the ethyl cellulose out of the oven, pouring the ethyl cellulose into the preheated ground glass bottle, fully shaking up, and putting into the oven with the constant temperature of 100 ℃;
in the dissolving process, shaking up for 1 time every 20 minutes until the ethyl cellulose is completely dissolved, wherein the dissolving time is 2 hours, and the dissolved mixed solution becomes a binder;
s34, sieving the binder with a 500-mesh nylon sieve to prevent undissolved crystal grains from existing, and then filling the mixture into a ground glass bottle for sealing for standby, wherein the standing time is not more than 15 days.
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
through developing the composite additive mixed by terpineol, ethyl cellulose and SA auxiliary agent, the fluidity and uniformity of the screen printing metal slurry are improved, and the metal powder is ensured to be uniformly and flatly coated on the surface of the ceramic.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in further detail below.
Example one
This example provides an additive for a metallized sealing composite, the additive comprising an adjuvant, terpineol, and ethyl cellulose,
the auxiliary agent and the terpineol are mixed according to the weight ratio of 15: (75-90) preparing a terpineol solvent, wherein the additive is prepared from the ethyl cellulose and the terpineol solvent according to the weight ratio of (20-30): 100;
the auxiliary agent is formed by mixing butyl carbitol, tributyl citrate, isopropanol and tea seed oil, and the auxiliary agent comprises the following components in parts by weight: 10-15 parts of butyl carbitol, 5-10 parts of tributyl citrate, 2-5 parts of isopropanol and 1-3 parts of tea seed oil.
The preparation method of the additive comprises the following steps:
step one, preparation of an auxiliary agent:
s11, weighing the components according to the preset proportion of the auxiliary agents, sequentially adding the components into a glass bottle, tightly covering the glass bottle cover, continuously shaking the glass bottle for 2-3 minutes, and continuously rolling the glass bottle during shaking;
s12, placing the shaken glass bottle on a ball milling frame with an environment temperature control function for ball milling, wherein the environment temperature is controlled to be 48-50 ℃, and the ball milling time is 20-28 hours;
s13, taking down the glass bottle, and cooling for standby application, wherein the standby application time is not more than 7 days;
step two, preparation of terpineol alcohol solvent: taking the adjuvant prepared in the step one and terpineol according to the weight ratio of 15: (75-90) uniformly mixing to prepare a terpineol solvent for later use;
step three, preparation of an additive:
s31, weighing ethyl cellulose and the terpineol solvent according to the weight ratio (20-30): 100, putting the terpineol solvent into a 2L ground glass bottle, and separately containing the ethyl cellulose by using wax paper;
s32, placing the ground glass bottle filled with the terpineol alcohol solvent and the wax paper filled with the ethyl cellulose in a constant-temperature oven at 100 ℃ for preheating for 1 hour, wherein the oven is a stainless steel band hot air circulation oven, and the set temperature is 100 ℃;
s33, taking the terpineol alcohol solvent and the ethyl cellulose out of the oven, pouring the ethyl cellulose into the preheated ground glass bottle, fully shaking up, and putting into the oven with the constant temperature of 100 ℃;
in the dissolving process, shaking up for 1 time every 20 minutes until the ethyl cellulose is completely dissolved, wherein the dissolving time is 2 hours, and the dissolved mixed solution becomes a binder;
s34, sieving the binder with a 500-mesh nylon sieve to prevent undissolved crystal grains from existing, and then filling the mixture into a ground glass bottle for sealing for standby, wherein the standing time is not more than 15 days.
Example two
This example provides an additive for a metallized sealing composite, the additive comprising an adjuvant, terpineol, and ethyl cellulose,
the auxiliary agent and the terpineol are mixed according to the weight ratio of 15: (75-90) preparing a terpineol solvent, wherein the additive is prepared from the ethyl cellulose and the terpineol solvent according to the weight ratio of (20-30): 100;
the auxiliary agent is formed by mixing butyl carbitol, tributyl citrate, isopropanol and tea seed oil, and the auxiliary agent comprises the following components in parts by weight: 9 parts of butyl carbitol, 7 parts of tributyl citrate, 3 parts of isopropanol and 2 parts of tea seed oil.
In the experiment, the metallized ceramic and the metallic copper are welded in a brazing mode, when the sealing tension of the metallized ceramic and the metal is tested, an AgCu28 copper sheet is placed between the metallized ceramic and the metal, the welding is carried out in a hydrogen environment at 810 ℃, the copper metal is an actual working part, after the welding is finished, a destructive test is carried out through a tension resistance meter, and the test results are compared as follows:
| kind of additive | Sealing result (MPa) |
| Conventional additives | 90 |
| Additive for this patent | 135 |
The above-mentioned serial numbers of the embodiments of the present invention are merely for description and do not represent the merits of the embodiments.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (2)
1. An additive for a metallized sealing composite material, characterized in that the additive comprises an auxiliary agent, terpineol and ethyl cellulose,
the auxiliary agent and the terpineol are mixed according to the weight ratio of 15: (75-90) preparing a terpineol solvent, wherein the additive is prepared from the ethyl cellulose and the terpineol solvent according to the weight ratio of (20-30): 100;
the auxiliary agent is formed by mixing butyl carbitol, tributyl citrate, isopropanol and tea seed oil, and the auxiliary agent comprises the following components in parts by weight: 10-15 parts of butyl carbitol, 5-10 parts of tributyl citrate, 2-5 parts of isopropanol and 1-3 parts of tea seed oil.
2. The additive for metallized sealing composite material as claimed in claim 1, wherein said adjuvant is composed of butyl carbitol, tributyl citrate, isobutyl alcohol and tea seed oil, and the components are as follows by weight: 9 parts of butyl carbitol, 7 parts of tributyl citrate, 3 parts of isopropanol and 2 parts of tea seed oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911231167.8A CN112920641A (en) | 2019-12-05 | 2019-12-05 | Additive for metallized sealing composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911231167.8A CN112920641A (en) | 2019-12-05 | 2019-12-05 | Additive for metallized sealing composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112920641A true CN112920641A (en) | 2021-06-08 |
Family
ID=76160719
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911231167.8A Withdrawn CN112920641A (en) | 2019-12-05 | 2019-12-05 | Additive for metallized sealing composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112920641A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106631168A (en) * | 2016-12-15 | 2017-05-10 | 湖南省美程陶瓷科技有限公司 | Additive for new energy automobile metallization sealing-in ceramics and preparation method thereof |
-
2019
- 2019-12-05 CN CN201911231167.8A patent/CN112920641A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106631168A (en) * | 2016-12-15 | 2017-05-10 | 湖南省美程陶瓷科技有限公司 | Additive for new energy automobile metallization sealing-in ceramics and preparation method thereof |
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Application publication date: 20210608 |
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| WW01 | Invention patent application withdrawn after publication |