CN101475312A - Copper seal powdered glass, as well as preparation and application thereof - Google Patents
Copper seal powdered glass, as well as preparation and application thereof Download PDFInfo
- Publication number
- CN101475312A CN101475312A CNA2009100457707A CN200910045770A CN101475312A CN 101475312 A CN101475312 A CN 101475312A CN A2009100457707 A CNA2009100457707 A CN A2009100457707A CN 200910045770 A CN200910045770 A CN 200910045770A CN 101475312 A CN101475312 A CN 101475312A
- Authority
- CN
- China
- Prior art keywords
- glass
- copper
- percent
- sealing
- glass powder
- 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.)
- Granted
Links
Images
Landscapes
- Glass Compositions (AREA)
Abstract
The invention relates to a copper-sealed glass powder. The copper-sealed glass powder comprises the following compositions in percentage by weight: 50 to 60 percent of SiO2, 20 to 30 percent of BaO, 3 to 5 percent of Li2O, 3 to 5 percent of Na2O, 3 to 5 percent of ZrO2, 2 to 4 percent of TiO2, 0.1 to 0.5 percent of CoO, 1 to 3 percent of Na3AlF6 and 3 to 5 percent of Al2O3; a preparation method comprises that: the compositions are charged and mixed, are smelted for 1 to 2 hours in a high-temperature smelter, are poured to clean cooling water, are put into an oven, are dried, are subjected to ball milling for 24 hours and are filtered by a sieve with 120 meshes to obtain the copper-sealed glass powder; and the application of the copper-sealed glass powder comprises that: after the copper-sealed glass powder is dewaxed by a dewaxing process, the copper-sealed glass powder and an electronic component are subjected to capsulation treatment in a sealing furnace. The copper-sealed glass powder has excellent mechanical performance and thermal performance and better capsulation molding; and the preparation method is simple, has low cost and can realize industrialized production.
Description
Technical field
The invention belongs to the preparation field of sealing glass powder, particularly relate to a kind of copper seal powdered glass and preparation thereof and application.
Background technology
The reliability of semiconductor components and devices will directly have influence on the work-ing life and the quality product of machine product.Along with the development of China's aerospace industry, more and more higher to the specification of quality of electronic devices and components, demand is more and more, and existing seal, sealing materials, sealing process all have been difficult to satisfy technical requirements.
Traditional sealing process adopts transition sealing method (i.e. three layers of sealing-in method) because the thermal expansivity of oxygen free copper is bigger, in the process of sealing-in, can produce very big stress, so can only adopt kovar alloy circle transition method, be the copper shell earlier with the sealing-in of kovar alloy circle, the kovar alloy circle is three layers of method for sealing by seal glass and the sealing-in of metallic conduction post again.Since there are oxygen free copper and kovar alloy circle, kovar alloy circle and seal glass, and therefore a plurality of seal interface of seal glass and these differing materials of conductive pole are easy to cause the gas leakage of seal glass cracking.
Copper sealing glass must have good sealing characteristic as a kind of seal, sealing materials, as good glass surface character and surface tension, and good glass machinery performance and thermal property, higher glass chemistry stability and electrical insulating property.The special sealing-in that also must satisfy the copper shell simultaneously requires can not be too high as sealing temperature, and the sealing-in formability will wait technical requirements well.
Therefore, the present invention is directed to the problems referred to above and carried out deep research, a kind of novel inorganic seal, sealing materials-copper sealing glass is provided.
Summary of the invention
Technical problem to be solved by this invention provides a kind of copper seal powdered glass and preparation and application, copper sealing glass of the present invention has favorable mechanical performance and thermal property, and higher chemical stability and electrical insulating property, and has sealing-in formability preferably, this preparation method is simple, cost is low, and the economic benefit height can be realized suitability for industrialized production.
A kind of copper seal powdered glass of the present invention, its component comprises by weight:
SiO2?50％-60％，Bao?20％-30％，Li2O?3％-5％，Na2O?3-5％，ZrO2?3％-5％，TiO22％-4％，CoO?0.1％-0.5％，Na3AlF6?1％-3％，Al2O3?3％-5％；
The transition temperature of described copper sealing glass is 460 ± 10 ℃, and the sealing temperature of glass is 870 ± 20 ℃, and the proportion of glass is 2.96 ± 0.1, and the glass powder color is green or blue, and the thermal expansivity of glass is in room temperature～400 ℃, (90 ± 2) * 10
-7/ ℃;
A kind of copper sealing glass powder, preparation method thereof of the present invention comprises:
Adopt the Li2O-Al2O3-SiO2 glass system, each component is fed intake by above-mentioned weight ratio weighing, mix, with 1000 milliliters of alumina crucibles in 1450 ℃ of high-temperature smelting pots, melting 1 hour, treat that glass melts clarification fully after, pour in the clean water coolant, hardening crack becomes the glass disintegrating slag, puts into 115 ℃ of-125 ℃ of baking ovens then 3.5-4.5 hours, after the oven dry, again the glass fragment is put into ceramic ball grinder, behind 24 hours ball millings, cross 120 mesh sieves, promptly get copper seal powdered glass.
The preparation that is applied to electronic devices and components of a kind of copper seal powdered glass of the present invention, concrete preparation process comprises:
(1) be that 10% medical paraffin mixes by mass ratio 9:1 with the copper seal powdered glass of above-mentioned preparation and mass percent, after stirring, on shaper, be pressed into the copper sealing glass base of the content of wax, put into the chain type dewaxing furnace again, little through room temperature-100 ℃ insulation 2 successively, 100 ℃-200 ℃ are incubated 1 hour, 200 ℃-420 ℃ are incubated 1 hour, be warming up to 620 ℃ then rapidly, be incubated 3-5 minutes, promptly get the glass gob that dewaxes;
(2) will by the copper shell of sealing-in and Precise Alloy plain conductor clean respectively with pre-oxidation treatment after be assembled into the copper sealing glass base of dewaxing and treat the sealing-in part, put into 850 ℃-950 ℃ sealing-in stove, through 200 ℃ of preheatings 20 minutes, 900 ℃ of sealing-ins were annealed 40 minutes in 15 minutes and 900 ℃-50 ℃, after the cooling, promptly get and have high insulating property, the electronic devices and components of high-air-tightness.
Described paraffin needs to handle through heat fused in advance.
Adopt Li in the present invention
2O-Al
2O
3-SiO
2In the glass system, by in the copper sealing glass formulating of recipe, introducing nucleus agent TiO
2And ZrO
2Improved the microtexture of glass; make glass in the process of sealing-in; elder generation's vitreous; back crystallization had both guaranteed the resistance to air loss of glass sealing part, had improved the electrical insulating property and the physical strength of glass sealing part again; realized that shell is the direct sealing-in of the high-power base and the Precise Alloy conductive pole of oxygen free copper, solved the mechanical stress rimose technical barrier of seal glass because of the copper shell.
Beneficial effect
(1) copper sealing glass of the present invention has favorable mechanical performance and thermal property, and higher chemical stability and electrical insulating property, and have sealing-in formability preferably, solved the electronic component high power valve, the problem of insulated enclosure between copper pipe seat and the conductive pole;
(2) this preparation method is simple, and cost is low, and the economic benefit height can be realized suitability for industrialized production;
(3) this copper seal powdered glass changes three layers of traditional sealing-in into two layers of direct sealing-in, be that the oxygen free copper shell is by copper seal powdered glass and the direct sealing-in of conductive pole, owing to reduced seal interface, simplified sealing process, thereby the gas leakage that has significantly reduced part is scrapped, and has improved the qualification rate and the reliability of closure.
Description of drawings
Fig. 1 is the electronic devices and components sample photograph figure through the copper seal powdered glass sealing-in
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The oxide compound of raw material is respectively that the introducing oxide compound of raw material is that the content of raw material is
No. 8 quartz sands 99.5% of SiO2 50%-60%
Bao 20%-30% barium carbonate 77.31%
Li2O 3%-5% Quilonum Retard 40.14%
Na2O 3-5% anhydrous sodium carbonate 58.36%
ZrO2 3%-5% zirconium dioxide 99%
TiO2 2%-4% titanium dioxide 98%
CoO 0.1%-0.5% cobalt sesquioxide 98.5%
Na3AlF6 1%-3% sodium fluoroaluminate 99.5%
Al2O3 3%-5% aluminium hydroxide 64.7%
It is good to introduce the correct weighing of oxide compound by the raw material of the basic chemical constitution of above-mentioned copper sealing glass, mixes stand-by;
1000 milliliters of alumina crucibles are raised to 1410 ℃ with stove, carry out the first time then and feed in raw material, carried out the second time after being separated by 10 minutes and feed in raw material, being separated by, it is reinforced for the third time to carry out in 8 minutes again.Reinforced altogether three times, be incubated 40 minutes then, treat that glass metal melts clarification fully after, pour in the clean water coolant, hardening crack becomes the glass disintegrating slag, puts into 120 ℃ of left and right sides baking oven bakings about 4 hours again, oven dry back glass fragment was put into ceramic ball grinder again after weighing, through 24 hours ball millings.Behind 120 mesh sieves stand-by copper seal powdered glass.
Claims (4)
1. copper seal powdered glass, its component comprises by weight:
SiO2?50％-60％，Bao?20％-30％，Li2O?3％-5％，Na2O?3-5％，ZrO2?3％-5％，TiO22％-4％，CoO?0.1％-0.5％，Na3AlF6?1％-3％，Al2O3?3％-5％。
2. a kind of copper seal powdered glass according to claim 1, it is characterized in that: the transition temperature of described copper sealing glass is 460 ± 10 ℃, the sealing temperature of glass is 870 ± 20 ℃, the proportion of glass is 2.96 ± 0.1, the glass powder color is green or blue, the thermal expansivity of glass is in room temperature～400 ℃, (90 ± 2) * 10
-7/ ℃.
3. copper sealing glass powder, preparation method thereof comprises:
Adopt the Li20-Al203-SiO2 glass system, each component is fed intake by above-mentioned weight ratio weighing, mix, with 1000 milliliters of alumina crucibles in 1450-1500 ℃ of high-temperature smelting pots, melting 1-2 hours, treat that glass melts clarification fully after, pour in the clean water coolant, hardening crack becomes the glass disintegrating slag, puts into 115 ℃ of-125 ℃ of baking ovens then 3.5-4.5 hours, after the oven dry, again the glass fragment is put into ceramic ball grinder, behind 24 hours ball millings, cross 120 mesh sieves, promptly get copper seal powdered glass.
4. the application of a copper seal powdered glass is characterized in that: this copper seal powdered glass is applied to the preparation of electronic devices and components.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100457707A CN101475312B (en) | 2009-02-05 | 2009-02-05 | Copper seal powdered glass, as well as preparation and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100457707A CN101475312B (en) | 2009-02-05 | 2009-02-05 | Copper seal powdered glass, as well as preparation and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101475312A true CN101475312A (en) | 2009-07-08 |
| CN101475312B CN101475312B (en) | 2012-01-11 |
Family
ID=40836103
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100457707A Expired - Fee Related CN101475312B (en) | 2009-02-05 | 2009-02-05 | Copper seal powdered glass, as well as preparation and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101475312B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265176A (en) * | 2013-05-20 | 2013-08-28 | 京东方科技集团股份有限公司 | Sealing microcrystalline glass, and sealing method and application thereof |
| CN103415479A (en) * | 2011-03-07 | 2013-11-27 | 肖特公开股份有限公司 | Glass system for hermetically connecting cu components, and housing for electronic components |
| CN103539355A (en) * | 2013-10-25 | 2014-01-29 | 上海大学 | Frit composition for air-right sealing, preparation method thereof and sealing method based on frit composition |
| CN103708728A (en) * | 2013-11-26 | 2014-04-09 | 清华大学 | Glass-metal seal material for high-temperature gas-cooled reactor electrical penetration assembly and preparation method thereof |
| CN103880290A (en) * | 2012-12-19 | 2014-06-25 | 辽宁省轻工科学研究院 | Preparation method and application of high expansion coefficient copper sealing glass powder |
| CN105845186A (en) * | 2016-03-30 | 2016-08-10 | 清华大学 | Medium-voltage power electrical penetration assembly of high-temperature gas-cooled reactor and preparation method thereof |
| CN111333330A (en) * | 2018-12-19 | 2020-06-26 | 辽宁省轻工科学研究院有限公司 | Glass powder for sealing nickel-based superalloy and preparation and use methods thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU404797A1 (en) * | 1971-12-13 | 1973-10-22 | SOIL ENAMEL | |
| CN101157518A (en) * | 2007-09-14 | 2008-04-09 | 东华大学 | Sealing glass member for electrothermal tube and preparation method thereof |
-
2009
- 2009-02-05 CN CN2009100457707A patent/CN101475312B/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103415479B (en) * | 2011-03-07 | 2016-08-31 | 肖特公开股份有限公司 | For sealingly engaging the glass system of Cu parts and for the housing of electronic unit |
| CN103415479A (en) * | 2011-03-07 | 2013-11-27 | 肖特公开股份有限公司 | Glass system for hermetically connecting cu components, and housing for electronic components |
| CN103880290A (en) * | 2012-12-19 | 2014-06-25 | 辽宁省轻工科学研究院 | Preparation method and application of high expansion coefficient copper sealing glass powder |
| CN103880290B (en) * | 2012-12-19 | 2016-10-05 | 辽宁省轻工科学研究院 | A kind of preparation method and applications of high expansion coefficient copper sealing glass powder |
| CN103265176A (en) * | 2013-05-20 | 2013-08-28 | 京东方科技集团股份有限公司 | Sealing microcrystalline glass, and sealing method and application thereof |
| CN103265176B (en) * | 2013-05-20 | 2015-10-14 | 京东方科技集团股份有限公司 | A kind of sealing glass ceramic, its method for sealing and purposes |
| CN103539355A (en) * | 2013-10-25 | 2014-01-29 | 上海大学 | Frit composition for air-right sealing, preparation method thereof and sealing method based on frit composition |
| CN103539355B (en) * | 2013-10-25 | 2016-03-09 | 上海大学 | The glass frit compositions of gas-tight seal and preparation method, sealing method based on glass frit compositions |
| CN103708728A (en) * | 2013-11-26 | 2014-04-09 | 清华大学 | Glass-metal seal material for high-temperature gas-cooled reactor electrical penetration assembly and preparation method thereof |
| CN103708728B (en) * | 2013-11-26 | 2015-10-28 | 清华大学 | A kind of Glass-metal seal material for high temperature gas cooled reactor electrical penetration and preparation method thereof |
| CN105845186A (en) * | 2016-03-30 | 2016-08-10 | 清华大学 | Medium-voltage power electrical penetration assembly of high-temperature gas-cooled reactor and preparation method thereof |
| CN105845186B (en) * | 2016-03-30 | 2018-05-29 | 清华大学 | The preparation method of pressure power electrical penetration in a kind of high temperature gas cooled reactor |
| CN111333330A (en) * | 2018-12-19 | 2020-06-26 | 辽宁省轻工科学研究院有限公司 | Glass powder for sealing nickel-based superalloy and preparation and use methods thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101475312B (en) | 2012-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101475312B (en) | Copper seal powdered glass, as well as preparation and application thereof | |
| CN101549958B (en) | Composition for high-performance glass fiber | |
| CN103193387B (en) | Enamel material for 1Cr18Ni9Ti stainless steel surface and preparation method thereof | |
| CN101570398B (en) | Sealing glass special for compressor and preparation and application thereof | |
| CN106810079B (en) | The method for preparing mica glass ceramic using granite waste residues | |
| CN101244889A (en) | Non-fluorin environment protection opacifiedglass material and method for manufacturing same | |
| CN106882923A (en) | A kind of devitrified glass of resistance to 650 DEG C of high temperature and preparation method thereof | |
| CN106882921A (en) | A kind of seal, sealing materials of resistance to 750 DEG C of high temperature and preparation method thereof | |
| CN102503149B (en) | Low-lead glass powder for silver paste of anode of solar cell and preparation method of low-lead glass powder | |
| CN108793756A (en) | A kind of glass powder and preparation method thereof for Fe-Si-Al magnetic core insulating wrapped | |
| CN103420614B (en) | A kind of preparation method of thick film dielectric glass powder | |
| CN106882922A (en) | A kind of seal glass of resistance to 550 DEG C of high temperature and preparation method thereof | |
| CN102276151A (en) | Technological method for preparing LTCC (low temperature co-fired ceramic) amorphous glass ceramic powder with microwave plasma torch | |
| CN103420689A (en) | Artistic pottery fancy glaze and manufacturing method thereof | |
| CN102060440B (en) | High-pressure-resistant sealing microcrystalline glass and use thereof | |
| CN115784605B (en) | Tantalate additive for aluminosilicate glass and preparation method and application thereof | |
| CN104478219A (en) | Nano-scale spinel glass ceramic and preparation method thereof | |
| CN109081687B (en) | High thermal shock resistance ceramic crucible suitable for calcining lithium battery anode material and preparation method thereof | |
| CN102351403B (en) | Method for preparing ultrafine glass powder used for solar battery slurry | |
| CN105906212A (en) | Mica-based glass ceramic and preparation method thereof | |
| CN102838278A (en) | Negative thermal expansion microcrystalline glass and preparation method thereof | |
| CN102633435A (en) | Lead-free low-temperature glass for manufacturing diode glass shell | |
| CN105502949A (en) | Bismuth oxide series low-melting-point glass for copper-aluminum sealing and preparation method thereof | |
| CN102153281B (en) | Piezoelectric ceramic glass and preparation method and application of piezoelectric ceramic glass | |
| CN118125814B (en) | High heat-resistant microcrystalline ceramic household appliance liner and preparation process thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120111 Termination date: 20150205 |
|
| EXPY | Termination of patent right or utility model |