CN110171981A - A kind of ceramic metallizing paste, preparation method and applications - Google Patents
A kind of ceramic metallizing paste, preparation method and applications Download PDFInfo
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- CN110171981A CN110171981A CN201910467783.7A CN201910467783A CN110171981A CN 110171981 A CN110171981 A CN 110171981A CN 201910467783 A CN201910467783 A CN 201910467783A CN 110171981 A CN110171981 A CN 110171981A
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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
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
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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
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/023—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
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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
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/12—Metallic interlayers
- C04B2237/122—Metallic interlayers based on refractory metals
Abstract
The invention particularly discloses a kind of ceramic metallizing pastes, based on parts by weight, including 70-80 parts of molybdenum powder, 17-22 parts of manganese powder, 3-10 parts of the low-temperature eutectic object calcined, 15-22 parts of binder.The constitutive materials such as the low-temperature eutectic object, including aluminium oxide, Suzhou soil, silica, barium carbonate, calcium oxide, zirconium oxide.Preparation method includes: that low-temperature eutectic object is prepared；Binder making；The preparation of ceramic metallizing paste and etc..The present invention joined barium carbonate on the basis of conventional formulation, formula is innovated, enhance the formula composition of metalization layer, it will be sintered auxiliary material simultaneously, calcining pretreatment is first carried out by phasor, generate preliminary eutectic, enhance metalization layer and ceramic diffusion transition, the bond strength of metalization layer and ceramics is enhanced, the versatility of formula is also enhanced, the metallization welding of 95 aluminium oxide ceramics, 99 aluminium oxide ceramics and zirconia ceramics can be adapted to simultaneously.
Description
Technical field
The invention belongs to ceramic metallization material applied technical fields, and in particular to a kind of ceramic metallizing paste, preparation
Method and its application.
Background technique
Special cermacis using more and more extensive, such as 95 aluminium oxide ceramics are used for vacuum switch pipe shell；99 aluminium oxide pottery
Porcelain is for the igniter in space flight and aviation；Zirconia ceramics be used for engine cavity etc., but these ceramics using past
It, need to be with ceramic metallizing paste in ceramic surface in order to make welding for china with metal together toward needing to weld together with metal
One layer of metal coating is coated, most widely used at present is molybdenum manganese metal technology.
Traditional molybdenum manganese metal is mainly made of molybdenum, manganese, aluminium oxide, silica, zirconium oxide, calcium oxide.For ceramics
Metallizing paste and preparation method thereof, having seen has the disclosure of some patented technologies.Such as: application No. is CN201310126321.1,
Disclosed a kind of high-strength alumina ceramic metallizing paste and preparation method thereof, molybdenum powder, 5- of the paste by 70-85%
The AL of 15% manganese powder, 5-15%2O3Powder, the silicon dioxide powder of 5-10%, the calcium oxide of 0.2-1.2%, 0.2-1.5% oxygen
Change the titanium dioxide powder composition of magnesium, the zirconia powder of 0.2-1.5%, 0.2-1.0%；Preparation method is: will in the above ratio
Above-mentioned substance is respectively put into baking oven, 100-110 DEG C at a temperature of dry 1-2 hours；Molybdenum powder is put into ball mill, nothing is added
Water-ethanol, grind 24-48 hours, 100-110 DEG C at a temperature of dry；By manganese powder, AL2O3Powder, silicon dioxide powder, calcium oxide,
Magnesia, zirconia powder and titanium dioxide powder are put into ball mill, grind 4-6 hours, the molybdenum powder of milled is added, continues to grind
36-48 hours, obtain the mixed powder of above-mentioned material；Binder is added into mixed powder again, grinds 24-48 hours, obtains metallization cream
Agent.This patented technology there is: in the change paste of preparing metal the problems such as long period, complex procedures.
For another example: application No. is CN200610041036.X, a kind of disclosed powder for ceramic metallizing paste and its system
Preparation Method, the paste are made of 60-80 parts of molybdenum powder, 20-40 parts of glass phase component, in which: glass phase component is again by aluminium oxide 25-
40 parts, the original of 0.5-2.5 parts of calcium oxide, 25-40 parts of silica, 30-40 parts of manganese powder, 2-4 parts of titanium valve, 2-4 parts of zirconium dioxide
Material is constituted, and must first sintering auxiliary materials other to molybdenum powder, manganese powder and silica etc. be distinguished when preparing the metallizing paste
400 meshes of mistake after the 90-100 hour above dry ball milling are carried out, then different materials dry ball milling together again, discharged and 400 sieve
Required paste is finally hybridly prepared into binder ultrasonic wave, the method is not only there is that need to carry out multiple ball milling, and time-consuming is big, gold
The defects of sintering temperature of categoryization is high, and energy consumption is big, the deficiencies of gluing wall there is also powder and ball milling altar caused to be broken, and due to
Powder is ultra-fine, and it is also extremely difficult to cross 400 meshes.
Summary of the invention
The technical problems to be solved by the present invention are: for the defects of existing special cermacis metallizing paste with not
Foot provides a kind of ceramic metallizing paste, preparation method and applications.
The present invention adopts the following technical scheme that, Lai Shixian goal of the invention.
A kind of ceramic metallizing paste, based on parts by weight, including constitutive material below: 70-80 parts of molybdenum powder, manganese powder
17-22 parts, 3-10 parts of the low-temperature eutectic object calcined, 15-22 parts of binder.
Further, the low-temperature eutectic object, based on parts by weight, including constitutive material below: aluminium oxide 90-96
Part, 1-4 parts of Suzhou soil, -3 parts of silica 1,0.3-0.6 parts of barium carbonate, 0.2-0.7 parts of calcium oxide, 0.2-0.6 parts of zirconium oxide.
Further, the binder, based on parts by weight, including constitutive material below: ethyl cellulose 5-10
Part, 90-95 parts of terpinol, 0-3 parts of castor oil.
Further, the molybdenum powder and manganese powder, 2.5 microns of D50 <.
A kind of preparation method of ceramic metallizing paste, comprising the following steps: (1) low-temperature eutectic object is prepared；(2) binder
It prepares；(3) preparation of ceramic metallizing paste.
Further, low-temperature eutectic object described in step (1) is prepared, specifically: based on parts by weight, by 90-96 parts
Aluminium oxide, 1-4 parts of Suzhou soil, 1-3 parts of silica, 0.3-0.6 parts of barium carbonate, 0.2-0.7 parts of calcium oxide, 0.2-
0.6 part of zirconium oxide, is put into ball milling altar mixing 1-2 hours, and discharging, which is put into crucible, calcines, and 1300-1400 DEG C of temperature, heat preservation 2
Hour.
Further, binder making described in step (2), specifically: it is based on parts by weight, 5-10 parts of ethyl is fine
Element, 90-95 parts of terpinol, 0-3 parts of castor oil are tieed up, is fitted into container, water proof is heated and stirred, wait until being completely dissolved.
Further, the preparation of ceramic metallizing paste described in step (3), specifically: based on parts by weight, by 70-
80 parts of molybdenum powder, 17-22 parts of manganese powder, 3-10 parts of the low-temperature eutectic object calcined are put into planetary ball mill, add
15-22 parts of binder, while alumina balls are added, material ball ratio 1:4, ball milling 2-4 hours, discharged 200 meshes, that is, obtains
Required paste.
A kind of ceramic metallizing paste, in the application that special cermacis and metal welding connect.
Further, the special cermacis and metal weld, to coat one layer of ceramic metallization on special cermacis surface
Paste.
Further, the special cermacis be 95 aluminium oxide ceramics, it is 99 aluminium oxide ceramics, any in zirconia ceramics
It is a kind of.
The utility model has the advantages that
(1) invention joined barium monoxide (being provided by barium carbonate through calcining) on the basis of conventional formulation, has innovated and has matched
Side, enhances the formula composition of metalization layer, and barium monoxide has high density, high-melting-point, high refractive index, chemical high stability etc. excellent
Different characteristic generates baryta fledspar low-temperature solvent with calcium carbonate, silica, aluminium oxide etc., while first will sintering auxiliary by phasor
Material carries out calcining pretreatment, generates preliminary eutectic, enhances metalization layer and ceramic diffusion transition, enhances metallization
Layer and ceramic bond strength, also enhance the versatility of formula, can adapt to simultaneously 95 aluminium oxide ceramics, 99 aluminium oxide ceramics and
The metallization of zirconia ceramics is welded.
(2) sintering auxiliary material need to only be put into crucible when low-temperature eutectic object is prepared and calcine 1300-1400 by the present invention
DEG C, keep the temperature 2 hours, eutectic it is pre-prepared so that ceramic can preferably realize molybdenum manganese layer in a metallization processes
Binding force is spread and enhanced to ceramic matrix, and sintering temperature and time far below traditional handicraft reduce primary metallization temperature
Degree, has saved the energy, and porcelain piece deforms when reducing primary metallization.
(3) present invention is disposably assisted molybdenum powder, manganese powder, sintering using advanced planetary ball mill when paste is prepared
Material and organic binder ball milling 2-4 hours cross 200 meshes and complete paste and prepare.Become from the multiple ball milling in traditional handicraft
A ball milling is only needed, simplify and has innovated preparation method, the paste preparation time is greatly shortened, paste is significantly improved and prepares effect
Rate.
(4) by the obtained ceramic metallizing paste of the present invention, it is applied to special cermacis and metal welds, welding performance
It is much better than similar high temperature metallization technology.Weld obtained metallization thickness 15-45 microns, 2-10 microns of nickel layer thickness, gold
Categoryization tensile strength is greater than 160MPa, and sealing-in air-tightness is less than 1 × 10-10Pa·m3/s。
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, but the present invention is not limited to following embodiments.
The method is conventional method unless otherwise instructed.The raw material can obtain unless otherwise instructed from public commercial source
?.
Embodiment 1: ceramic metallizing paste A
(1) low-temperature eutectic object is prepared: based on parts by weight, by 93 parts of aluminium oxide, 2 parts of Suzhou soil, 2 parts of titanium dioxide
Silicon, 0.5 part of barium carbonate, 0.5 part of calcium oxide, 0.5 part of zirconium oxide, are put into ball milling altar mixing 1.5 hours, and discharging is put into earthenware
It is calcined in crucible, 1350 DEG C of temperature, keeps the temperature 2 hours.
(2) binder making: based on parts by weight, by 8 parts of ethyl cellulose, 93 parts of terpinol, 2 parts of castor-oil plant
Oil is fitted into enamelled cup, and water proof heating is stirred with cloth glue stick, wait until being completely dissolved.
(3) preparation of ceramic metallizing paste: based on parts by weight, by 75 parts of molybdenum powder, 20 parts of manganese powder, 6 parts are forged
Burned low-temperature eutectic object, is put into planetary ball mill, adds 20 parts of binder, while alumina balls are added, material ball ratio
For 1:4, ball milling 3 hours, discharged 200 meshes, that is, paste A needed for obtaining.
Paste A is coated 95 alumina ceramic faces to be used to weld with metal, welds obtained metallization thickness
45 microns, 5 microns of nickel layer thickness, metallization tensile strength is greater than 160MPa, and sealing-in air-tightness is less than 1 × 10-10Pa·m3/s。
Embodiment 2: ceramic metallizing paste B
(1) low-temperature eutectic object is prepared: based on parts by weight, by 96 parts of aluminium oxide, 1 part of Suzhou soil, 3 parts of titanium dioxide
Silicon, 0.3 part of barium carbonate, 0.7 part of calcium oxide, 0.2 part of zirconium oxide, are put into ball milling altar mixing 2 hours, and discharging is put into crucible
Middle calcining, keeps the temperature 2 hours by 1300 DEG C of temperature.
(2) binder making: based on parts by weight, by 10 parts of ethyl cellulose, 90 parts of terpinol, 3 parts of castor-oil plant
Oil is fitted into enamelled cup, and water proof heating is stirred with cloth glue stick, wait until being completely dissolved.
(3) preparation of ceramic metallizing paste: based on parts by weight, by 70 parts of molybdenum powder, 22 parts of manganese powder, 3 parts are forged
Burned low-temperature eutectic object, is put into planetary ball mill, adds 15 parts of binder, while alumina balls are added, material ball ratio
For 1:4, ball milling 4 hours, discharged 200 meshes, that is, paste B needed for obtaining.
Paste B is coated 99 alumina ceramic faces to be used to weld with metal, welds obtained metallization thickness
30 microns, 6 microns of nickel layer thickness, metallization tensile strength is greater than 160MPa, and sealing-in air-tightness is less than 1 × 10-10Pa·m3/s。
Embodiment 3: ceramic metallizing paste C
(1) low-temperature eutectic object is prepared: based on parts by weight, by 90 parts of aluminium oxide, 4 parts of Suzhou soil, 1 part of titanium dioxide
Silicon, 0.6 part of barium carbonate, 0.2 part of calcium oxide, 0.6 part of zirconium oxide, are put into ball milling altar mixing 1 hour, and discharging is put into crucible
Middle calcining, keeps the temperature 2 hours by 1400 DEG C of temperature.
(2) binder making: based on parts by weight, by 5 parts of ethyl cellulose, 95 parts of terpinol, 1 part of castor-oil plant
Oil is fitted into enamelled cup, and water proof heating is stirred with cloth glue stick, wait until being completely dissolved.
(3) preparation of ceramic metallizing paste: based on parts by weight, by 80 parts of molybdenum powder, 17 parts of manganese powder, 10 parts are forged
Burned low-temperature eutectic object, is put into planetary ball mill, adds 22 parts of binder, while alumina balls are added, material ball ratio
For 1:4, ball milling 2 hours, discharged 200 meshes, that is, paste C needed for obtaining.
Paste C coated with zirconia ceramic surface is used to weld with metal, welds obtained metallization thickness 28
Micron, 5 microns of nickel layer thickness, metallization tensile strength is greater than 160MPa, and sealing-in air-tightness is less than 1 × 10-10Pa·m3/s。
Embodiment 4: ceramic metallizing paste D
(1) low-temperature eutectic object is prepared: based on parts by weight, by 90 parts of aluminium oxide, 1 part of Suzhou soil, 1 part of titanium dioxide
Silicon, 0.4 part of barium carbonate, 0.4 part of calcium oxide, 0.4 part of zirconium oxide, are put into ball milling altar mixing 1 hour, and discharging is put into crucible
Middle calcining, keeps the temperature 2 hours by 1300 DEG C of temperature.
(2) binder making: based on parts by weight, by 7 parts of ethyl cellulose, 93 parts of terpinol, 0 part of castor-oil plant
Oil is fitted into enamelled cup, and water proof heating is stirred with cloth glue stick, wait until being completely dissolved.
(3) preparation of ceramic metallizing paste: based on parts by weight, by 70 parts of molybdenum powder, 17 parts of manganese powder, 10 parts are forged
Burned low-temperature eutectic object, is put into planetary ball mill, adds 15 parts of binder, while alumina balls are added, material ball ratio
For 1:4, ball milling 2 hours, discharged 200 meshes, that is, paste D needed for obtaining.
Paste D is coated 95 alumina ceramic faces to be used to weld with metal, welds obtained metallization thickness
35 microns, 3.5 microns of nickel layer thickness, metallization tensile strength is greater than 160MPa, and sealing-in air-tightness is less than 1 × 10-10Pa·m3/
s。
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on above description specific embodiment.To those skilled in the art, the equivalent modifications and replace that any couple of present invention carries out
In generation, is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and repair
Change, all covers within the scope of the present invention.
Claims (10)
1. a kind of ceramic metallizing paste, which is characterized in that based on parts by weight, including constitutive material below: molybdenum powder 70-80
Part, 17-22 parts of manganese powder, 3-10 parts of the low-temperature eutectic object calcined, 15-22 parts of binder.
2. a kind of ceramic metallizing paste according to claim 1, which is characterized in that the low-temperature eutectic object, with weight
Amount number meter, including constitutive material below: 90-96 parts of aluminium oxide, 1-4 parts of Suzhou soil, -3 parts of silica 1, barium carbonate
0.3-0.6 parts, 0.2-0.7 parts of calcium oxide, 0.2-0.6 parts of zirconium oxide.
3. a kind of ceramic metallizing paste according to claim 1, which is characterized in that the binder, with parts by weight
Number meter, including constitutive material below: 5-10 parts of ethyl cellulose, 90-95 parts of terpinol, 0-3 parts of castor oil.
4. a kind of ceramic metallizing paste according to claim 1, which is characterized in that the molybdenum powder and manganese powder, D50 <
2.5 micron.
5. a kind of preparation method of ceramic metallizing paste, which comprises the following steps: (1) low-temperature eutectic object is prepared；
(2) binder making；(3) preparation of ceramic metallizing paste.
6. a kind of preparation method of ceramic metallizing paste according to claim 5, which is characterized in that step (1) is described
Low-temperature eutectic object prepare, specifically: based on parts by weight, by 90-96 parts of aluminium oxide, 1-4 parts of Suzhou soil, 1-3 parts
Silica, 0.3-0.6 parts of barium carbonate, 0.2-0.7 parts of calcium oxide, 0.2-0.6 parts of zirconium oxide, are put into ball milling altar mixing
1-2 hours, discharging, which is put into crucible, calcined, and 1300-1400 DEG C of temperature, kept the temperature 2 hours.
7. a kind of preparation method of ceramic metallizing paste according to claim 5, which is characterized in that step (2) is described
Binder making, specifically: based on parts by weight, by 5-10 parts of ethyl cellulose, 90-95 parts of terpinol, 0-3 parts
Castor oil is fitted into container, and water proof is heated and stirred, wait until being completely dissolved.
8. a kind of preparation method of ceramic metallizing paste according to claim 5, which is characterized in that step (3) is described
Ceramic metallizing paste preparation, specifically: based on parts by weight, by 70-80 parts of molybdenum powder, 17-22 parts of manganese powder, 3-10
The low-temperature eutectic object calcined of part, is put into planetary ball mill, adds 15-22 parts of binder, while aluminium oxide is added
Ball, material ball ratio 1:4, ball milling 2-4 hours, discharged 200 meshes, that is, paste needed for obtaining.
9. a kind of application of ceramic metallizing paste, it is characterised in that: be applied to special cermacis and metal welds.
10. a kind of application of ceramic metallizing paste according to claim 9, it is characterised in that: the special cermacis
It is welded with metal, to coat one layer of ceramic metallizing paste on special cermacis surface；The special cermacis is 95 aluminium oxide pottery
Porcelain, 99 aluminium oxide ceramics, any one in zirconia ceramics.
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Cited By (3)
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| CN113582732A (en) * | 2021-08-10 | 2021-11-02 | 浮梁县景龙特种陶瓷有限公司 | Paste formula for improving bonding force of metallization and ceramics |
| CN114538948A (en) * | 2020-11-24 | 2022-05-27 | 娄底市安地亚斯电子陶瓷有限公司 | Metal transition layer suitable for welding zirconia ceramic and metal and preparation method thereof |
| CN116514568A (en) * | 2023-04-03 | 2023-08-01 | 湖南人文科技学院 | Ceramic-metal integrated package and packaging method |
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| CN110171981B (en) | 2021-09-03 |
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