CN103102180A - Metallized surface of zirconia ceramic and preparation method - Google Patents
Metallized surface of zirconia ceramic and preparation method Download PDFInfo
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- CN103102180A CN103102180A CN2013100575875A CN201310057587A CN103102180A CN 103102180 A CN103102180 A CN 103102180A CN 2013100575875 A CN2013100575875 A CN 2013100575875A CN 201310057587 A CN201310057587 A CN 201310057587A CN 103102180 A CN103102180 A CN 103102180A
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Abstract
The invention relates to a metallized surface of zirconia ceramic and a preparation method. The metallized surface of zirconia ceramic comprises of the following components by weight: 50-70% Mo powder, 11-19% of Mn powder, 6-14% of SiO2 powder, 0.2-2.5% of CaO, 5-15% of 75% alumina ceramic powder, 0-4% of ZrO2, and 0-5% of TiO2. Specifically, the 75% alumina ceramic powder is composed of the following components by weight: 73-79% of Al2O3, 11-17% of SiO2, 0-5% of BaO, 0.5-4% of CaO, and 0.5-2.5% of MgO. The preparation method includes: 1) conducting weighing and mixing according to the metallized formula proportion, placing the mixture in a high energy ball mill, carrying out high-energy ball milling for over 180h in an organic medium to prepare metallized powder; 2) adding a proper amount of an organic binder into the prepared metallized powder, fully stirring them, covering a cleaned zirconia ceramic surface with the mixture by means of silk screen printing, pad printing, spraying coating, pen coating or other modes, and performing natural drying or infrared ray drying; 3) sintering the metallized powder-covered zirconia ceramic under protection of a weak reducing atmosphere; and 4) subjecting the sintered product to nickel plating, thus obtaining a zirconia ceramic surface metallized product.
Description
Technical field
What the present invention relates to is a kind of metalization process of preparing of zirconia ceramics, is convenient to metallized zirconia ceramics and can carries out soldering with metallic substance and be connected.
Background technology
That zirconia ceramics has is high temperature resistant, corrosion-resistant, good toughness, specific heat capacity and the excellent properties such as thermal conductivity is little, more and more be applied to the industries such as machinery, metallurgy, chemical industry, weaving, aerospace, biology, electronics, in application process, zirconia ceramics need to be connected with metal.At present, zirconia ceramics in use with being connected of metal, generally adopt mechanical connection or directly use activated solder that zirconia ceramics and metal solder are in the same place, although mechanical connection intensity is high, but be applied on vacuum or other airtight devices, the mode of mechanical connection can not satisfy the resistance to air loss requirement of the device condition of high temperature; Adopt activated solder (as silver-bearing copper titanium braze) directly metal and zirconia ceramics at high temperature to be carried out soldering, strength of joint is generally in the 50MPa left and right.Expansion along with the zirconia ceramics range of application, a lot of devices not only require the strength of joint of zirconia ceramics and metal high, and resistance to air loss is good, above-mentioned two kinds of technology can not satisfy the technical need of modern industry, must study technology more reliably, make zirconia ceramics and being connected of metal have the advantage of high strength and high-air-tightness concurrently.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, and provide a kind of metallization process system easily to control, dependable performance can effectively improve metalized surface and the preparation method of the zirconia ceramics of zirconia ceramics and metal connection intensity.
The objective of the invention is to complete by following technical solution, the metalized surface of described zirconia ceramics, it is comprised of following component and weight proportion: 50～70% Mo powder, 11～19% Mn powder, 6～14% SiO
2Powder, 0.2～2.5% CaO, 5～15% 75% alumina ceramics powder, the ZrO of 0-4%
2, the TiO2 of 0-5%, the proportioning of above-mentioned component consists of absolutely.
75% alumina ceramics powder of the present invention is comprised of following component and weight proportion: 73～79% Al
2O
3, 11～17% SiO
2, 0～5% BaO, 0.5～4% CaO, 0.5～2.5% MgO, and the proportioning of said ratio consists of absolutely.
Mo Powder Particle Size≤2.5um of the present invention, particle diameter are 60～90wt% that the particle of 0.5～1.8um accounts for Mo powder gross weight, and the Mo granularity is less is conducive to the Mo powder and glassy phase is fully wetting, improves simultaneously tensile strength and the resistance to air loss of metal layer;
Described manganese powder purity 〉=99.5wt%, manganese in metallization processes at first oxidation form MnO, be the main modification composition of glassy phase, make glassy phase and Mo particle surface that good wetting property be arranged, promote simultaneously the atomic diffusion between metal layer and ceramic matrix;
Described SiO
2Powder foreign matter content≤0.1wt%, SiO
2It is the major ingredient that forms glassy phase;
Described ZrO
2Powder foreign matter content≤0.1wt%;
Described TiO
2Powder foreign matter content≤0.1wt%;
A kind of metalized surface preparation method of zirconia ceramics as mentioned above, the method is comprised of following steps:
1) weigh, mix in the ratio of metallizing formula, be placed in high energy ball mill, high-energy ball milling is made the metallization powder more than 180 hours under organic medium, and abrading-ball is agate ball or alumina balls, then oven dry, sieving for standby;
2) with the above-mentioned metallization powder for preparing, add appropriate organic binder bond, through fully stirring, cover on clean zirconia ceramics surface with silk screen printing, bat printing, spraying or the mode such as be coated with, seasoning or infrared baking all can;
3) be coated with zirconia ceramics sintering under weak reducing atmosphere protection of metallization powder, dew point of hydrogen in 30 ± 10 ℃ of scopes, 1350～1430 ℃ of sintering temperatures, sintered heat insulating time 30～70min;
4) product that sinters is zirconia ceramics surface metalation product through nickel plating.
The formula of metalized surface of the present invention is applicable to the different stabilizers zirconia ceramics, as Y
2O
3, CeO
2, MgO, CaO be as the stablizer zirconia ceramics, and be strong to the suitability of pottery;
With the production of metallizing of the formula of metalized surface of the present invention, process system is controlled easily, constant product quality, reliable;
Ceramic metallization product with the preparation of the composition and engineering of metalized surface of the present invention, metal layer is even, fine and close, and the high and high conformity with the bonding strength of pottery is surveyed tensile strength with Φ 3 kovar alloys rod bikinis, its average tensile strength value 〉=130MPa, leak rate≤1 * 10
-11Pa.m
3/ s, metallization layer thickness is at 15～45um, and nickel layer thickness satisfies accurate device to the requirement of ceramic metallization product fully at 2.0～6.5um.
Embodiment
Below in conjunction with specific embodiment, the present invention is done detailed introduction: the metalized surface of zirconia ceramics of the present invention, it is comprised of following component and weight proportion: 50～70% Mo powder, 11～19% Mn powder, 6～14% SiO
2Powder, 0.2～2.5% CaO, 5～15% 75% alumina ceramics powder, 04% ZrO
2, the TiO of 0-5%
2, the proportioning of above-mentioned component consists of absolutely.
75% alumina ceramics powder of the present invention is comprised of following component and weight proportion: 73～79% Al
2O
3, 11～17% SiO
2, 0～5% BaO, 0.5～4% CaO, 0.5～2.5% MgO, and the proportioning of said ratio consists of absolutely.
Mo Powder Particle Size≤2.5um of the present invention, particle diameter are 60～90wt% that the particle of 0.5～1.8um accounts for Mo powder gross weight, and the Mo granularity is less is conducive to the Mo powder and glassy phase is fully wetting, improves simultaneously tensile strength and the resistance to air loss of metal layer;
Described manganese powder purity 〉=99.5wt%, manganese in metallization processes at first oxidation form MnO, be the main modification composition of glassy phase, make glassy phase and Mo particle surface that good wetting property be arranged, promote simultaneously the atomic diffusion between metal layer and ceramic matrix;
Described SiO
2Powder foreign matter content≤0.1wt%, SiO
2It is the major ingredient that forms glassy phase;
Described ZrO
2Powder foreign matter content≤0.1wt%;
Described TiO
2Powder foreign matter content≤0.1wt%;
A kind of metalized surface preparation method of zirconia ceramics as mentioned above, the method is comprised of following steps:
1) weigh, mix in the ratio of metallizing formula, be placed in high energy ball mill, high-energy ball milling is made the metallization powder more than 180 hours under organic medium, and abrading-ball is agate ball or alumina balls, then oven dry, sieving for standby;
2) with the above-mentioned metallization powder for preparing, add appropriate organic binder bond, through fully stirring, cover on clean zirconia ceramics surface with silk screen printing, bat printing, spraying or the mode such as be coated with, seasoning or infrared baking all can;
3) be coated with zirconia ceramics sintering under weak reducing atmosphere protection of metallization powder, dew point of hydrogen in 30 ± 10 ℃ of scopes, 1350～1430 ℃ of sintering temperatures, sintered heat insulating time 30～70min;
4) product that sinters is zirconia ceramics surface metalation product through nickel plating.
Embodiment:
Technical process of the present invention is as follows: and the mixing and ball milling → oven dry by weight ratio of each powder sieves → and adding additives stirs → is coated in (wet-film thickness is in the 30-100um left and right) → sintering → nickel plating of metallizing → metallized product performance test on the zirconia ceramics surface under atmosphere protection.
Be described in detail as follows below by specific embodiment:
1, the powder of respectively selecting according to the form below ratio weighing respectively is placed in 99% alumina ceramics ball grinder, makes medium with organic solvents such as dehydrated alcohol or N-BUTYL ACETATEs, make abrading-ball with agate ball or alumina ball, ball milling took out to be placed in Stainless Steel Disc and dries more than 180 hours, crossed 250 mesh sieves.
Table 1: metallizing formula (weight percent)
| Numbering and composition | Mo | Mn | SiO 2 | CaO | 75% porcelain powder | ZrO 2 | TiO 2 |
| 1 | 50 | 19 | 10.8 | 0.2 | 15 | 0.1 | 4.9 |
| 2 | 55 | 17 | 12 | 1.5 | 11.0 | 2.5 | 1.0 |
| 3 | 60 | 15 | 14 | 2.5 | 8 | 0.4 | 0.1 |
| 4 | 65 | 13 | 8 | 1.2 | 11.5 | 0.9 | 0.4 |
| 5 | 70 | 11 | 6 | 0.9 | 6 | 4.0 | 2.1 |
2, take above-mentioned each powder for preparing of 50g, be placed in agitator, then to add 20ml organic binder bond, organic binder bond be the terpineol solution of ethyl cellulose of 4.5wt%, stir standby more than 6 hours.
3, with method for printing screen, the above-mentioned slurry for preparing is printed on clean different stabilizers zirconia ceramics surface, represents Y with A
2O
3Stabilization zirconium oxide ceramic represents CeO with B
2Stabilization zirconium oxide ceramic represents the MgO stabilization zirconium oxide ceramic with C, namely gets and respectively implements sample such as 1A, 1B, 1C, 2A, 2B etc.
4, respectively implement sample such as 1A, 1B, 1C, 2A, 2B etc. and put into metallization stove sintering, sintering process parameter is as shown in table 2 below:
Table 2: sintering process parameter
| Time temperature | 1350℃ | 1370℃ | 1390℃ | 1410℃ | 1430℃ |
| 30 minutes | ? | ? | √ | √ | √ |
| 50 minutes | ? | √ | √ | √ | √ |
| 70 minutes | √ | √ | √ | √ | ? |
Annotate: beat the processing parameter for actual enforcement of " √ ", protective atmosphere (H
2) dew point be 30 ± 10 ℃.
Sample after sintering is through nickel plating.
Each sample is carried out performance test, and result is described below table 3:
Table 3: the performance test results
Claims (4)
1. the metalized surface of a zirconia ceramics, is characterized in that this metalized surface is comprised of following component and weight proportion: 50～70% Mo powder, 11～19% Mn powder, 6～14% SiO
2Powder, 0.2～2.5% CaO, 5～15% 75% alumina ceramics powder, the ZrO of 0-4%
2, the TiO of 0-5%
2, the proportioning of above-mentioned component consists of absolutely.
2. the metalized surface of zirconia ceramics according to claim 1, is characterized in that described 75% alumina ceramics powder is comprised of following component and weight proportion: 73～79% Al
2O
3, 11～17% SiO
2, 0～5% BaO, 0.5～4% CaO, 0.5～2.5% MgO, and the proportioning of said ratio consists of absolutely.
3. the metalized surface of zirconia ceramics according to claim 1, is characterized in that described Mo Powder Particle Size≤2.5um, and particle diameter is 60～90wt% that the particle of 0.5～1.8um accounts for Mo powder gross weight;
Described manganese powder purity 〉=99.5wt%;
Described SiO
2Powder foreign matter content≤0.1wt%;
Described ZrO
2Powder foreign matter content≤0.1wt%;
Described TiO
2Powder foreign matter content≤0.1wt%.
4. preparation method as the metalized surface of zirconia ceramics as described in claim 1 or 2 or 3, the method is comprised of following steps:
1) weigh, mix in the ratio of metallizing formula, be placed in high energy ball mill, high-energy ball milling is made the metallization powder more than 180 hours under organic medium, and abrading-ball is agate ball or alumina balls, then oven dry, sieving for standby;
2) with the above-mentioned metallization powder for preparing, add appropriate organic binder bond, through fully stirring, cover on clean zirconia ceramics surface with silk screen printing, bat printing, spraying or the mode such as be coated with, seasoning or infrared baking all can;
3) be coated with zirconia ceramics sintering under weak reducing atmosphere protection of metallization powder, dew point of hydrogen in 30 ± 10 ℃ of scopes, 1350～1430 ℃ of sintering temperatures, sintered heat insulating time 30～70min;
4) product that sinters is zirconia ceramics surface metalation product through nickel plating.
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Cited By (12)
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| CN103288494A (en) * | 2013-05-16 | 2013-09-11 | 长安大学 | Method for preparing titanium metal coating on ceramic surface |
| CN103449846A (en) * | 2013-09-13 | 2013-12-18 | 陈晓炜 | Formula for high-strength metallization of ceramic vacuum switch tube and application method thereof |
| CN103755390A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院上海硅酸盐研究所 | Method for improving metallization intensity of zirconia ceramics of oxygen sensor |
| CN104058794A (en) * | 2014-07-02 | 2014-09-24 | 南京三乐电子信息产业集团有限公司 | Microwave device energy transmitting window ceramic chip metallization coating and metallization coating method thereof |
| CN105112741A (en) * | 2015-08-25 | 2015-12-02 | 东莞劲胜精密组件股份有限公司 | Aluminum alloy material used for electronic product shells and manufacture method |
| CN105948826A (en) * | 2016-06-16 | 2016-09-21 | 常熟市银洋陶瓷器件有限公司 | High-temperature metallization technology for yttria ceramic |
| CN107365171A (en) * | 2017-08-28 | 2017-11-21 | 北京京东方真空电器有限责任公司 | A kind of ceramic metallizing paste and its preparation method and application |
| CN111266590A (en) * | 2020-01-21 | 2020-06-12 | 中科英冠(厦门)陶瓷科技有限公司 | Ceramic metallizing raw material, ceramic metallizing method and metallized ceramic |
| CN112979346A (en) * | 2021-02-08 | 2021-06-18 | 东莞信柏结构陶瓷股份有限公司 | Zirconia ceramic surface conduction method |
| CN113004060A (en) * | 2021-02-08 | 2021-06-22 | 东莞信柏结构陶瓷股份有限公司 | ZrO (ZrO)2Ceramic surface conduction method |
| CN113754471A (en) * | 2021-09-28 | 2021-12-07 | 中国原子能科学研究院 | Zirconium oxide ceramic metalized gold-based slurry, metalized layer and preparation method |
| 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 |
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Cited By (18)
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| CN103288494B (en) * | 2013-05-16 | 2014-10-15 | 长安大学 | Method for preparing titanium metal coating on ceramic surface |
| CN103288494A (en) * | 2013-05-16 | 2013-09-11 | 长安大学 | Method for preparing titanium metal coating on ceramic surface |
| CN103449846A (en) * | 2013-09-13 | 2013-12-18 | 陈晓炜 | Formula for high-strength metallization of ceramic vacuum switch tube and application method thereof |
| CN103755390A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院上海硅酸盐研究所 | Method for improving metallization intensity of zirconia ceramics of oxygen sensor |
| CN104058794B (en) * | 2014-07-02 | 2016-03-30 | 南京三乐电子信息产业集团有限公司 | Microwave device delivery of energy window ceramics metallised paint and metalized coated method thereof |
| CN104058794A (en) * | 2014-07-02 | 2014-09-24 | 南京三乐电子信息产业集团有限公司 | Microwave device energy transmitting window ceramic chip metallization coating and metallization coating method thereof |
| CN105112741B (en) * | 2015-08-25 | 2017-03-22 | 东莞劲胜精密组件股份有限公司 | Aluminum alloy material used for electronic product shells and manufacture method |
| CN105112741A (en) * | 2015-08-25 | 2015-12-02 | 东莞劲胜精密组件股份有限公司 | Aluminum alloy material used for electronic product shells and manufacture method |
| CN105948826A (en) * | 2016-06-16 | 2016-09-21 | 常熟市银洋陶瓷器件有限公司 | High-temperature metallization technology for yttria ceramic |
| CN107365171A (en) * | 2017-08-28 | 2017-11-21 | 北京京东方真空电器有限责任公司 | A kind of ceramic metallizing paste and its preparation method and application |
| CN107365171B (en) * | 2017-08-28 | 2021-02-05 | 北京京东方真空电器有限责任公司 | Ceramic metallization paste and preparation method and application thereof |
| CN111266590A (en) * | 2020-01-21 | 2020-06-12 | 中科英冠(厦门)陶瓷科技有限公司 | Ceramic metallizing raw material, ceramic metallizing method and metallized ceramic |
| CN111266590B (en) * | 2020-01-21 | 2022-02-15 | 中科英冠(厦门)陶瓷科技有限公司 | Ceramic metallizing raw material, ceramic metallizing method and metallized ceramic |
| 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 |
| CN112979346A (en) * | 2021-02-08 | 2021-06-18 | 东莞信柏结构陶瓷股份有限公司 | Zirconia ceramic surface conduction method |
| CN113004060A (en) * | 2021-02-08 | 2021-06-22 | 东莞信柏结构陶瓷股份有限公司 | ZrO (ZrO)2Ceramic surface conduction method |
| CN113754471A (en) * | 2021-09-28 | 2021-12-07 | 中国原子能科学研究院 | Zirconium oxide ceramic metalized gold-based slurry, metalized layer and preparation method |
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Application publication date: 20130515 |