CN113582732B - Paste formula for improving bonding force of metallization and ceramics - Google Patents
Paste formula for improving bonding force of metallization and ceramics Download PDFInfo
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- CN113582732B CN113582732B CN202110913700.XA CN202110913700A CN113582732B CN 113582732 B CN113582732 B CN 113582732B CN 202110913700 A CN202110913700 A CN 202110913700A CN 113582732 B CN113582732 B CN 113582732B
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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
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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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
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
- C04B41/90—Coating or impregnation for obtaining at least two superposed coatings having different compositions at least one coating being a metal
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Abstract
The invention discloses a paste formula for improving the bonding force between metallization and ceramics, belonging to the technical field of ceramic metallization. The ceramic metallization paste comprises the following raw materials in percentage by mass: 12.5 to 15.5 percent of manganese powder, 5.4 to 8.2 percent of low-temperature melting oxide, 0.4 to 0.7 percent of strontium sulfate, 14.0 to 16.8 percent of binder and the balance of molybdenum powder. Wherein, the low-temperature melting oxide comprises the following components in percentage by mass: 84 to 89 percent of alumina, 10.5 to 15 percent of silicon dioxide, 0.3 to 0.6 percent of calcium oxide and 0.1 to 0.4 percent of montmorillonite. The invention optimizes the formula of the traditional ceramic metallization molybdenum-manganese paste, reduces the content of low-temperature molten oxides by increasing the content of manganese, and adds the strontium sulfate microspheres to prepare the novel molybdenum-manganese paste which is applied to the welding of 95 percent alumina ceramic and metal, the welding performance is obviously improved, the thickness of the obtained metallization coating is 8-40 mu m, the thickness of a nickel layer is 1-5 mu m, the metallization tensile strength is not lower than 175MPa, and the application is wide.
Description
Technical Field
The invention belongs to the technical field of ceramic metallization, and particularly relates to a paste formula for improving the bonding force between metallization and ceramic.
Background
The essence of ceramic metallization is a process of coating a metal film on the surface of a ceramic to make it have new and special characteristics. The ceramic metallization provides possibilities for late welding, packaging, electric conduction, heat dissipation and the like of ceramic products, and is widely applied to various advanced technical fields of semiconductors, integrated circuits, electric light sources, lasers, atomic energy, high-energy physics, aerospace and the like and departments of chemical industry, textile, metallurgy, machinery and the like.
Although the ceramic metallization is more and more widely used, the ceramic metallization process is difficult, and the combination of the ceramic substrate and the metal film needs to be effectively guaranteed. The existing ceramic metallization process mainly comprises a molybdenum-manganese method, a gold plating method, a copper plating method, a LAP method and the like, and the molybdenum-manganese method is widely applied at present in consideration of similar thermal expansion coefficients and sintering properties of refractory metal powder such as molybdenum and alumina ceramic. The key point of the molybdenum-manganese method is the preparation of molybdenum-manganese paste, and the traditional molybdenum-manganese paste mainly comprises a metal phase (molybdenum powder), a glass phase (manganese powder, silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide and the like) and an organic binder (ethyl cellulose and terpineol). For example, chinese patent application publication No. CN 109627036A discloses a metallization paste suitable for 99% alumina ceramics and a method for preparing the same, wherein the metallization paste comprises, by weight, 60-80 parts of molybdenum, 5-15 parts of manganese, 10-25 parts of alumina, 5-15 parts of silicon dioxide, and further comprises a mixture of terpineol and ethyl cellulose in a weight ratio of 1: (20-30) mixing the prepared binder. The metallization paste prepared by the patent is coated on the alumina ceramic by screen printing, and the final metallization layer of the alumina ceramic formed after sintering has the drawing force of more than or equal to 90MPa. The problems with this patent are: the bonding force between the metal film prepared by finally sintering the metallization paste prepared by the patent and the ceramic matrix material is general, and the metallization paste has obvious limitation in more application fields.
Disclosure of Invention
The invention provides a paste formula for improving the bonding force of metallization and ceramics, aiming at the technical defect of general bonding force of ceramic matrix materials and metal films in the existing ceramic metallization technology.
The invention is realized by the following technical scheme:
the invention provides a paste for improving the bonding force of metallization and ceramics, which comprises the following raw materials in percentage by mass:
12.5 to 15.5 percent of manganese powder, 5.4 to 8.2 percent of low-temperature melting oxide, 0.4 to 0.7 percent of strontium sulfate, 14.0 to 16.8 percent of binder and the balance of molybdenum powder.
Further, the low-temperature melting oxide comprises the following components in percentage by mass: 84 to 89 percent of alumina, 10.5 to 15 percent of silicon dioxide, 0.3 to 0.6 percent of calcium oxide and 0.1 to 0.4 percent of montmorillonite.
Further, the manganese powder is spherical, the purity is not lower than 99.5%, and the grain size is 1.5-2 μm; the molybdenum powder is flaky, the purity is not lower than 99.5%, and the grain size is 4-10 mu m.
The strontium sulfate selected by the invention is strontium sulfate microspheres with the particle size of less than 3 mu m, has good binding force, and can effectively enhance the binding force between a metal layer and a ceramic matrix in the ceramic metallization process with molybdenum-manganese paste prepared from mixed powder of other low-temperature molten oxides through ball milling.
Further, the binder comprises the following components in percentage by mass: 90-95% of terpineol and 5-10% of ethyl cellulose.
The invention also aims to provide a preparation method of the paste for improving the bonding force of metallization and ceramics, which comprises the following steps:
1) Weighing molybdenum powder, manganese powder, low-temperature molten oxide, strontium sulfate and binder according to the formula ratio for later use;
2) Putting manganese powder, low-temperature molten oxide and strontium sulfate into a planetary ball mill, wherein the ball material ratio is 1:1, ball milling for 3-4h to obtain mixed powder;
3) Adding molybdenum powder and a binder into the mixed powder, and changing the ball-material ratio to be 1: and 2.5, continuing ball milling for 8-12h, and discharging to obtain paste.
Further, the terpineol and the ethyl cellulose are mixed in a water bath and heated to be completely dissolved to prepare the binder.
Further, the paste is applied to welding of special alumina ceramics and metals.
Further, the application specifically comprises: coating the prepared molybdenum-manganese paste on the surface of 95% alumina ceramic by a screen printing mode through a screen of 100 meshes to 400 meshes, drying the printed alumina ceramic at 120-160 ℃ to form a metalized coating with the thickness of 8-40 mu m, placing the alumina ceramic with the metalized coating on the surface in a wet hydrogen atmosphere furnace at 1200-1300 ℃ for high-temperature sintering, preserving the heat for 1-1.5h, and finally plating a nickel layer with the thickness of 1-5 mu m on the surface of the molybdenum-manganese layer.
Compared with the prior art, the invention has the beneficial effects that:
the invention optimizes the formula of the traditional ceramic metalized molybdenum-manganese paste, reduces the content of low-temperature fused oxides by increasing the content of manganese, and adds the strontium sulfate microspheres to prepare the novel molybdenum-manganese paste. The ceramic metallization molybdenum-manganese paste prepared by the invention is applied to welding of 95% alumina ceramic and metal, the welding performance is obviously improved, the thickness of the obtained metallization coating is 8-40 mu m, the thickness of the nickel layer is 1-5 mu m, and the metallization tensile strength is not lower than 175MPa.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
A paste for improving the bonding force of metallization and ceramics:
1. according to the mass percentage, 14 percent of manganese powder, 6.5 percent of low-temperature melting oxide, 0.6 percent of strontium sulfate microsphere, 15.6 percent of binder and the balance of molybdenum powder are taken. Wherein, the low-temperature melting oxide comprises the following components in percentage by mass: 85% of aluminum oxide, 14.3% of silicon dioxide, 0.5% of calcium oxide and 0.2% of montmorillonite; the binder comprises the following components in percentage by mass: terpineol 92% and ethyl cellulose 8%.
2. Putting manganese powder, low-temperature molten oxide and strontium sulfate into a planetary ball mill, wherein the ball-material ratio is 1:1, ball milling for 3.5 hours to obtain mixed powder; adding molybdenum powder and a binder into the mixed powder, and changing the ball-material ratio to be 1: and 2.5, continuing ball milling for 10 hours, and discharging to obtain paste.
3. Coating the prepared molybdenum-manganese paste on the surface of 95% alumina ceramic by adopting a screen printing mode through a screen of 100 meshes to 400 meshes, drying the printed alumina ceramic at 150 ℃ to form a metalized coating with the thickness of 28 mu m, placing the alumina ceramic with the metalized coating on the surface in a 1260 ℃ wet hydrogen atmosphere furnace for high-temperature sintering, preserving the temperature for 1.2h, and finally plating a nickel layer with the thickness of 4 mu m on the surface of the molybdenum-manganese layer.
The sintered metallized alumina ceramic of this example had a tensile strength of 184.4MPa.
Example 2
1. According to the mass percentage, 12.5 percent of manganese powder, 8.2 percent of low-temperature melting oxide, 0.4 percent of strontium sulfate microsphere, 15.8 percent of binder and the balance of molybdenum powder are taken. Wherein, the low-temperature melting oxide comprises the following components in percentage by mass: 85% of alumina, 14.3% of silicon dioxide, 0.5% of calcium oxide and 0.2% of montmorillonite; the binder comprises the following components in percentage by mass: terpineol 92% and ethyl cellulose 8%.
2. Putting manganese powder, low-temperature molten oxide and strontium sulfate into a planetary ball mill, wherein the ball material ratio is 1:1, ball milling for 3.6 hours to obtain mixed powder; adding molybdenum powder and a binder into the mixed powder, and changing the ball-material ratio to be 1: and 2.5, continuing ball milling for 9 hours, and discharging to obtain paste.
3. And (2) coating the prepared molybdenum-manganese paste on the surface of 95% of alumina ceramic by adopting a screen printing mode through a screen mesh of 100-400 meshes, drying the printed alumina ceramic at 140 ℃ to form a metalized coating with the thickness of 30 mu m, placing the alumina ceramic with the metalized coating on the surface in a wet hydrogen atmosphere furnace at 1260 ℃, sintering at high temperature for 1.2h, and finally plating a nickel layer with the thickness of 5 mu m on the surface of the molybdenum-manganese layer.
The sintered metallized alumina ceramic of this example had a tensile strength of 178.1MPa.
Example 3
1. According to the mass percentage, 15.5 percent of manganese powder, 5.4 percent of low-temperature melting oxide, 0.6 percent of strontium sulfate microsphere, 15.2 percent of binder and the balance of molybdenum powder are taken. Wherein, the low-temperature melting oxide comprises the following components in percentage by mass: 85% of alumina, 14.3% of silicon dioxide, 0.5% of calcium oxide and 0.2% of montmorillonite; the binder comprises the following components in percentage by mass: terpineol 92% and ethyl cellulose 8%.
2. Putting manganese powder, low-temperature molten oxide and strontium sulfate into a planetary ball mill, wherein the ball-material ratio is 1:1, ball milling for 3 hours to obtain mixed powder; adding molybdenum powder and a binder into the mixed powder, and changing the ball-material ratio to be 1: and 2.5, continuing ball milling for 10.5h, and discharging to obtain paste.
3. And (2) coating the prepared molybdenum-manganese paste on the surface of 95% of alumina ceramic by adopting a screen printing mode through a screen with 100 meshes to 400 meshes, drying the printed alumina ceramic at 155 ℃ to form a metalized coating with the thickness of 24 mu m, placing the alumina ceramic with the metalized coating on the surface in a 1280 ℃ wet hydrogen atmosphere furnace for high-temperature sintering, preserving heat for 1h, and finally plating a nickel layer with the thickness of 4 mu m on the surface of the molybdenum-manganese layer.
The sintered metallized alumina ceramic of this example had a tensile strength of 185.8MPa.
Example 4
1. According to the mass percentage, 14 percent of manganese powder, 6.5 percent of low-temperature melting oxide, 0.7 percent of strontium sulfate microsphere, 14.0 percent of binder and the balance of molybdenum powder are taken. Wherein, the low-temperature melting oxide comprises the following components in percentage by mass: 88 percent of alumina, 11 percent of silicon dioxide, 0.6 percent of calcium oxide and 0.4 percent of montmorillonite; the binder comprises the following components in percentage by mass: 95% of terpineol and 5% of ethyl cellulose.
2. Putting manganese powder, low-temperature molten oxide and strontium sulfate into a planetary ball mill, wherein the ball-material ratio is 1:1, ball milling for 4 hours to obtain mixed powder; adding molybdenum powder and a binder into the mixed powder, and changing the ball-material ratio to be 1:2.5, continuing ball milling for 12 hours, and discharging to obtain paste.
3. And (2) coating the prepared molybdenum-manganese paste on the surface of 95% of alumina ceramic by adopting a screen printing mode through a screen with 100 meshes to 400 meshes, drying the printed alumina ceramic at 160 ℃ to form a metalized coating with the thickness of 20 mu m, placing the alumina ceramic with the metalized coating on the surface in a 1300 ℃ wet hydrogen atmosphere furnace for high-temperature sintering, preserving the heat for 1.5h, and finally plating a nickel layer with the thickness of 2 mu m on the surface of the molybdenum-manganese layer.
The sintered metallized alumina ceramic of this example had a tensile strength of 177.0MPa.
The above-described embodiments are only preferred embodiments of the present invention and are not intended to limit the present invention. Various changes and modifications can be made by one skilled in the art, and any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. The paste for improving the bonding force of metallization and ceramics is characterized by comprising the following raw materials in percentage by mass: 12.5 to 15.5 percent of manganese powder, 5.4 to 8.2 percent of low-temperature melting oxide, 0.4 to 0.7 percent of strontium sulfate, 14.0 to 16.8 percent of binder and the balance of molybdenum powder; wherein the strontium sulfate is strontium sulfate microspheres with the particle size of less than 3 mu m; the low-temperature melting oxide comprises the following components in percentage by mass: 84 to 89 percent of alumina, 10.5 to 15 percent of silicon dioxide, 0.3 to 0.6 percent of calcium oxide and 0.1 to 0.4 percent of montmorillonite.
2. The paste for improving the bonding force of metallization and ceramics according to claim 1, wherein the manganese powder is spherical, the purity is not less than 99.5%, and the grain size is 1.5-2 μm; the molybdenum powder is flaky, the purity is not lower than 99.5%, and the grain size is 4-10 mu m.
3. The paste for improving the bonding force between the metallization and the ceramic according to claim 1, wherein the binder comprises the following components in percentage by mass: 90% -95% of terpineol and 5% -10% of ethyl cellulose.
4. A method of preparing a paste for improving the bonding strength of metallization and ceramics according to any of claims 1 to 3, comprising the steps of:
1) Weighing molybdenum powder, manganese powder, low-temperature molten oxide, strontium sulfate and binder according to the formula ratio for later use;
2) Putting manganese powder, low-temperature molten oxide and strontium sulfate into a planetary ball mill, wherein the ball-material ratio is 1:1, ball milling for 3-4h to obtain mixed powder;
3) Adding molybdenum powder and a binder into the mixed powder, and changing the ball-material ratio to be 1:2.5, continuing ball milling for 8-12h, and discharging to obtain paste.
5. The method for preparing a paste for improving the bonding force between a metallized substrate and a ceramic substrate according to claim 4, wherein the binder is prepared by mixing terpineol and ethyl cellulose in a water bath and heating the mixture until the mixture is completely dissolved.
6. The method for preparing the paste for improving the bonding force of metallization and ceramics according to claim 4, wherein the paste is applied to special alumina ceramics and metal welding.
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Citations (3)
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|---|---|---|---|---|
| US4647477A (en) * | 1984-12-07 | 1987-03-03 | Kollmorgen Technologies Corporation | Surface preparation of ceramic substrates for metallization |
| WO2004054751A1 (en) * | 2002-12-13 | 2004-07-01 | Corus Aluminium Walzprodukte Gmbh | Brazing sheet product and method of its manufacture |
| JP2017201686A (en) * | 2016-04-28 | 2017-11-09 | 三ツ星ベルト株式会社 | Metallized substrate and method of manufacturing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3312533A (en) * | 1963-06-26 | 1967-04-04 | Philips Corp | Ceramic article with sintered metallic layer and flux |
| FR2751640B1 (en) * | 1996-07-23 | 1998-08-28 | Commissariat Energie Atomique | COMPOSITION AND METHOD FOR REACTIVE BRAZING OF CERAMIC MATERIALS CONTAINING ALUMINUM |
| CN101104567B (en) * | 2007-07-25 | 2010-09-15 | 浙江亚通金属陶瓷有限公司 | Metal composite layer on aluminum oxide ceramic surface and composite technique thereof |
| CN103951468A (en) * | 2014-03-14 | 2014-07-30 | 西安市元兴真空电子技术有限公司 | Metallization sintering powder for 95 alumina ceramic middle temperate metallization paste and preparation method thereof |
| CN110171981B (en) * | 2019-05-31 | 2021-09-03 | 景德镇景华特种陶瓷有限公司 | Ceramic metallization paste, preparation method and application thereof |
| CN111548193A (en) * | 2020-05-18 | 2020-08-18 | 宜宾红星电子有限公司 | Metallization method for ultra-high purity alumina ceramic |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4647477A (en) * | 1984-12-07 | 1987-03-03 | Kollmorgen Technologies Corporation | Surface preparation of ceramic substrates for metallization |
| WO2004054751A1 (en) * | 2002-12-13 | 2004-07-01 | Corus Aluminium Walzprodukte Gmbh | Brazing sheet product and method of its manufacture |
| JP2017201686A (en) * | 2016-04-28 | 2017-11-09 | 三ツ星ベルト株式会社 | Metallized substrate and method of manufacturing the same |
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