CN101538170B - Combination for ceramic metallization and using method thereof - Google Patents
Combination for ceramic metallization and using method thereof Download PDFInfo
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- CN101538170B CN101538170B CN2009101162731A CN200910116273A CN101538170B CN 101538170 B CN101538170 B CN 101538170B CN 2009101162731 A CN2009101162731 A CN 2009101162731A CN 200910116273 A CN200910116273 A CN 200910116273A CN 101538170 B CN101538170 B CN 101538170B
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- powder
- ceramic
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- alumina
- metallized
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- 238000000034 method Methods 0.000 title claims abstract description 10
- 238000001465 metallisation Methods 0.000 title abstract description 14
- 239000000919 ceramic Substances 0.000 title abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 57
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 12
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 12
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 10
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000292 calcium oxide Substances 0.000 claims abstract description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 13
- 238000009413 insulation Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 8
- 239000000020 Nitrocellulose Substances 0.000 claims description 8
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical group O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 claims description 8
- 229940043232 butyl acetate Drugs 0.000 claims description 8
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical group CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 8
- 229920001220 nitrocellulos Polymers 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 238000005538 encapsulation Methods 0.000 abstract 4
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052748 manganese Inorganic materials 0.000 abstract 1
- 239000011572 manganese Substances 0.000 abstract 1
- 229910052750 molybdenum Inorganic materials 0.000 abstract 1
- 239000011733 molybdenum Substances 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000007789 sealing Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000006071 cream Substances 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a combination used for 95 aluminium oxide ceramic metallization and a using method thereof, wherein the combination comprises the following components by weight parts: 70-75 parts of molybdenum powders, 10-15 parts of manganese powders, 2-4 parts of aluminium trioxide powders, 7-9 parts of silicon dioxide powders, 1-3 parts of magnesia powders, 0.5-1.5 parts of calcium oxide powders and 0.1-1 parts of titanium dioxide powders. Compared with the prior art, the titanium dioxide powders and magnesia powders added in the combination improve the soakage of ceramic metallization combination to the ceramics, thus improving the encapsulation strength between a 95-Al2O3 ceramic and a metal encapsulation part, wherein the encapsulation strength achieves 300-400MPa and the air leakage rate of the encapsulation part is less than 3%.
Description
Technical field
The invention belongs to the compoistion and method of use that is used for ceramic metallization, belong to especially and be used for vacuum electronic 95-Al
2O
3Metallized compoistion and method of use on the pottery.
Background technology
95-Al
2O
3The ceramic-metal sealing-in is a technology that ceramic dielectic and metal firmly are connected; (it is 95% pottery that 95 alumina-ceramic refer to alumina content); Be mainly used in industries such as vacuum electron device, semi-conductor, unicircuit, electric light source, laser, nuclear power, high energy physics, the energy, aerospace, chemical industry, metallurgy, medical treatment, power equipment, support or the like as device outer case, electrode insulation, substrate, clamping.At present, the domestic compsn that is used for ceramic metallization commonly used all is the seventies and eighties research and development, can't cooperate with present raw material and equipment, and itself and metal sealing exists leak rate height and the low shortcoming of sealing strength.
Summary of the invention
Technical problem to be solved by this invention provides that a kind of package strength is high, leak rate is low is used for the metallized compsn of 95 alumina-ceramic.
Another one technical problem to be solved by this invention provides the method for use of above-mentioned compsn.
The technical scheme of technical solution problem of the present invention is: be used for the metallized compsn of 95 alumina-ceramic, comprise following material and weight part:
Molybdenum powder 70-75
Manganese powder 10-15
Alchlor powder 2-4
Silicon dioxide powder 7-9
Magnesia powder 1-3
Calcium oxide powder 0.5-1.5
Titanium dioxide powder 0.1-1.
The purity of described molybdenum powder, manganese powder, alchlor powder, silicon dioxide powder, magnesia powder, calcium oxide powder, titanium dioxide powder is greater than 99%.
The granularity D50 of described molybdenum powder, manganese powder is 1-5 μ m.
The granularity D50 of alchlor powder, silicon dioxide powder, magnesia powder, calcium oxide powder and titanium dioxide powder is 2-5 μ m.
The method of use of described compsn with made mixture, is added sticker and solubility promoter, mixes the back evenly, is coated in 95-Al
2O
3On the pottery, carry out sintering, the agglomerating condition is: temperature 1400-1450 ℃, and insulation 40-60min, its dew point of control is 15 ± 5 ℃ more than 800 ℃; The sintering atmosphere is a hydrogen-nitrogen mixture gas, and hydrogen, nitrogen volume ratio are 3: 1-2, and after insulation finishes, to control its dew point and be-20 ± 5 ℃, the bulking value of described mixture, sticker (g/ml) is than being 100: 40-60; The volume ratio of described caking agent and solvent is 1.5-2.5: 1.
Described caking agent is a guncotton, and viscosity is the 38-43 centipoise.
Described solvent is a butylacetate.
The present invention compared with prior art, through in compsn, add titanium dioxide powder, magnesia powder has improved the infiltration of the compsn of ceramic metallization to pottery, thereby improved 95-Al
2O
3The sealing strength of pottery and metal sealing spare, sealing strength reaches 300-400MPa, and the leak rate of closure is less than 3%.
Embodiment
Below in conjunction with embodiment the present invention is done detailed explanation.
The purity of the molybdenum powder that present embodiment is used >=99.9% does not have the grey of tramp material, mean particle size 2 μ m.
The purity of used manganese powder >=99.9% does not have the lead of tramp material, mean particle size 2 μ m.
Used aluminum oxide powder, silicon dioxide powder, magnesia powder, calcium oxide powder, titanium dioxide powder are purity >=99.9%, and powder does not have the white of tramp material, mean particle size 3 μ m.
Sealing strength of the present invention detects according to the SJ3226-199 standard.
Leak rate of the present invention detects according to the SJ20600-1996 standard.
Embodiment 1:
A) get molybdenum powder 70 weight parts, manganese powder 15 weight parts, alchlor powder 2 weight parts, silicon dioxide powder 9 weight parts, magnesia powder 2.4 weight parts, calcium oxide powder 1.5 weight parts, titanium dioxide powder 0.1 weight part and agate ball and put into ball grinder; Mix the powder gross weight: agate ball weight=1: 2;
B) in the good powder of ball mill mixing, add butylacetate and guncotton, and then on ball mill, mix, the volume of butylacetate and guncotton and powder gross weight, volume, weight ratio are 25ml: 50ml: 100g;
C) the ceramic metallization cream mixture that step b is prepared is coated in 95-Al
2O
3On the pottery, coating thickness is 50 μ m, with 95-Al
2O
3Pottery is put into the metallization sintering oven, 1400 ℃ of sintering temperatures, and insulation 60min, the sintering atmosphere is the hydrogen and nitrogen gas body, and its volume ratio is 3: 2, and its dew point of control is 15 ℃ ± 5 ℃ more than 800 ℃, and it is-20 ℃ ± 5 ℃ that 1400 ℃ of insulations finish back its dew point of control.
Embodiment 2:
A) get molybdenum powder 73 weight parts, manganese powder 12 weight parts, alchlor powder 3 weight parts, silicon dioxide powder 8.5 weight parts, magnesia powder 2 weight parts, calcium oxide powder 1 weight part, titanium dioxide powder 0.5 weight part and agate ball and put into ball grinder; Mix the powder gross weight: agate ball weight=1: 2;
B) in the good powder of ball mill mixing, add butylacetate and guncotton, and then on ball mill, mix, the volume of butylacetate and guncotton and powder gross weight, volume, weight ratio are 15ml: 40ml: 100g;
C) the ceramic metallization cream mixture that step b is prepared is coated in 95-Al
2O
3On the pottery, coating thickness is 60 μ m, with 95-Al
2O
3Pottery is put into the metallization sintering oven, 1430 ℃ of sintering temperatures, and insulation 50min, the sintering atmosphere is the hydrogen and nitrogen gas body, and its volume ratio is 3: 1, and its dew point of control is 20 ℃ ± 5 ℃ more than 800 ℃, and it is-25 ℃ ± 5 ℃ that 1430 ℃ of insulations finish back its dew point of control.
Embodiment 3:
A) get molybdenum powder 75 weight parts, manganese powder 11 weight parts, alchlor powder 4 weight parts, silicon dioxide powder 7 weight parts, magnesia powder 1.5 weight parts, calcium oxide powder 0.5 weight part, titanium dioxide powder 1 weight part and agate ball and put into ball grinder; Mix the powder gross weight: agate ball weight=1: 2;
B) in the good powder of ball mill mixing, add butylacetate and guncotton, and then on ball mill, mix, the volume of butylacetate and guncotton and powder gross weight, volume, weight ratio are 30ml: 60ml: 100g;
C) the ceramic metallization cream mixture that step b is prepared is coated in 95-Al
2O
3On the pottery, coating thickness is 70 μ m, with 95-Al
2O
3Pottery is put into the metallization sintering oven, 1450 ℃ of sintering temperatures, and insulation 40min, the sintering atmosphere is the hydrogen and nitrogen gas body, and its volume ratio is 3: 1.5, and its dew point of control is 20 ℃ ± 5 ℃ more than 800 ℃, and it is-15 ℃ ± 5 ℃ that 1450 ℃ of insulations finish back its dew point of control.
The performance of the metallization aperture that embodiment 1,2,3 is made is as shown in table 1:
Table 1:
| Package strength (MPa) | Leak rate (%) | The coating uniformity coefficient | |
| Embodiment 1 | 360 | 2.4 | Evenly |
| Embodiment 2 | 410 | 2 | Evenly |
| Embodiment 3 | 390 | 2.8 | Evenly |
Claims (7)
1. one kind is used for the metallized compsn of 95 alumina-ceramic, it is characterized in that: comprise following material and weight part:
2. a kind of metallized compsn of 95 alumina-ceramic that is used for according to claim 1, it is characterized in that: described molybdenum powder, manganese powder, alchlor powder, silicon dioxide powder, magnesia powder, calcium oxide powder, titanium dioxide powder purity all are not less than 99.9%.
3. a kind of metallized compsn of 95 alumina-ceramic that is used for according to claim 1, it is characterized in that: the granularity D50 of described molybdenum powder, manganese powder is 1-5 μ m.
4. a kind of metallized compsn of 95 alumina-ceramic that is used for according to claim 1, it is characterized in that: the granularity D50 of alchlor powder, silicon dioxide powder, magnesia powder, calcium oxide powder and titanium dioxide powder is 2-5 μ m.
5. the described a kind of method of use that is used for the metallized compsn of 95 alumina-ceramic of claim 1 is characterized in that: with made mixture, add sticker and solubility promoter, mix the back evenly, be coated in 95-Al
2O
3On the pottery, carry out sintering, the agglomerating condition is: temperature 1400-1450 ℃, and insulation 40-60min, its dew point of control is 15 ± 5 ℃ more than 800 ℃; The sintering atmosphere is a hydrogen-nitrogen mixture gas, and hydrogen, nitrogen volume ratio are 3: 1-2, and insulation is controlled its dew point and is-20 ± 5 ℃ after finishing, and the bulking value g/ml ratio of described mixture, sticker is 100: 40-60; The volume ratio of described caking agent and solubility promoter is 1.5-2.5: 1.
6. a kind of method of use that is used for the metallized compsn of 95 alumina-ceramic according to claim 5 is characterized in that: described caking agent is a guncotton, and viscosity is the 38-43 centipoise.
7. a kind of method of use that is used for the metallized compsn of 95 alumina-ceramic according to claim 5 is characterized in that: described solubility promoter is a butylacetate.
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|---|---|---|---|
| CN2009101162731A CN101538170B (en) | 2009-03-04 | 2009-03-04 | Combination for ceramic metallization and using method thereof |
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| CN2009101162731A CN101538170B (en) | 2009-03-04 | 2009-03-04 | Combination for ceramic metallization and using method thereof |
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| CN101538170A CN101538170A (en) | 2009-09-23 |
| CN101538170B true CN101538170B (en) | 2012-11-14 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102049514B (en) * | 2009-11-11 | 2012-08-01 | 福建泉州万顺捷集团有限公司 | Powder for aluminum oxide ceramics nano metallized paste and preparation method thereof |
| CN102344301B (en) * | 2010-07-30 | 2015-12-09 | 奥斯兰姆有限公司 | Ceramic arc light tube working method, ceramic arc light tube and comprise the lamp of ceramic arc light tube |
| CN102290305B (en) * | 2011-07-22 | 2013-11-27 | 安徽华东光电技术研究所 | Method for metalizing inner circle of long ceramic cylinder |
| CN102400195B (en) * | 2011-11-23 | 2014-04-09 | 安徽华东光电技术研究所 | Nickel plating method after metallization of aluminum oxide ceramic |
| CN103373860A (en) * | 2012-04-27 | 2013-10-30 | 比亚迪股份有限公司 | Surface metalized coating composition of ceramic matrix, surface metalizing method of ceramic matrix, and coating and ceramic prepared from ceramic matrix |
| WO2014002306A1 (en) * | 2012-06-25 | 2014-01-03 | 京セラ株式会社 | Alumina ceramic, and ceramic wiring substrate and ceramic package using same |
| CN103172408A (en) * | 2013-04-12 | 2013-06-26 | 锦州金属陶瓷有限公司 | High-strength aluminum oxide ceramic metalized paste and preparation method thereof |
| CN107188613A (en) * | 2017-06-20 | 2017-09-22 | 合肥博之泰电子科技有限公司 | A kind of electronic ceramic component process of surface treatment |
| CN108314467A (en) * | 2018-04-11 | 2018-07-24 | 甘肃恒星特种陶瓷有限公司 | Heavy ion avcceleration ceramic-vacuum tube surface conductance layer formula and preparation method |
| CN109748574B (en) * | 2019-03-06 | 2021-08-31 | 娄底市安地亚斯电子陶瓷有限公司 | Ceramic connecting material and application thereof |
| CN113511915B (en) * | 2021-04-06 | 2022-11-08 | 上海富乐华半导体科技有限公司 | Preparation method of ceramic aluminum-coated lining plate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887814A (en) * | 2006-07-16 | 2007-01-03 | 常熟市银洋陶瓷器件有限公司 | Powder for ceramic metallizing paste and its prepn |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887814A (en) * | 2006-07-16 | 2007-01-03 | 常熟市银洋陶瓷器件有限公司 | Powder for ceramic metallizing paste and its prepn |
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