CN100360474C - Once sintering method ceramic metallization treatment process - Google Patents
Once sintering method ceramic metallization treatment process Download PDFInfo
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- CN100360474C CN100360474C CNB2005100200761A CN200510020076A CN100360474C CN 100360474 C CN100360474 C CN 100360474C CN B2005100200761 A CNB2005100200761 A CN B2005100200761A CN 200510020076 A CN200510020076 A CN 200510020076A CN 100360474 C CN100360474 C CN 100360474C
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- Prior art keywords
- sintering
- temperature
- glazing
- treatment process
- sintering time
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- 238000005245 sintering Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000001465 metallisation Methods 0.000 title claims abstract description 12
- 239000000919 ceramic Substances 0.000 title claims abstract description 11
- 230000008569 process Effects 0.000 title claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 230000009467 reduction Effects 0.000 claims description 16
- 239000012141 concentrate Substances 0.000 claims description 4
- 239000002184 metal Substances 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000010304 firing Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000011505 plaster Substances 0.000 abstract 3
- 239000011248 coating agent Substances 0.000 abstract 2
- 238000000576 coating method Methods 0.000 abstract 2
- 238000001514 detection method Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 229910052573 porcelain Inorganic materials 0.000 description 5
- 230000008676 import Effects 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
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- Furnace Details (AREA)
Abstract
The present invention relates to a once sintering treatment process for ceramic metallization, which comprises the following steps: glazing and coating metal plaster, glazing on ceramic tube surface and coating the metal plaster in the position needs metallization treatment; sintering, the ceramic tube which is glazed and coated with the metal plaster is put into an atmosphere reducing furnace to sinter; wet hydrogen with dew point at 25 to 39 DEG C is introduced in the atmosphere reducing furnace by the speed of 4.6 to 5.8M3/h; the temperature of the atmosphere reducing furnace at different segments is set as: the temperature of a heating zone is from 1000 to 1200 DEG C with sintering time of 30 to 50 min; the temperature of a thermostatic zone is from 1300 to 1460 DEG C with sintering time of 60 to 120 min; the temperature of a cooling zone is from 900 to 1200 DEG C with sintering time of 30 to 50 min. The present invention has the advantages that the glazed firing single program and the equipment investment are reduced, the production efficiency is improved by more than 25%, and the energy consumption for unit product is lowered by about 20%. The primary technical index of the present invention is in the domestic lead level by the detection of users.
Description
Technical field
The present invention relates to the ceramic metallization treatment process field.
Background technology
The present domestic various vacuum tube relaies that only are used to produce, the year demand of single series products such as isolating switch promptly reaches more than 3,000,000, and annual with 30% left and right sides speed increment.Electrovacuum porcelain tube metallization technology exploitation is shorter in China's time, and at present domestic still do not have a professional production in enormous quantities producer, needs dependence on import in a large number.Metallized ceramic tubes product cheaply satisfies the domestic market and strives for exporting very strong competitive edge is all arranged in alternative import.Because vacuum electron device is to work under high vacuum state, and is very high to metallized precision of porcelain tube and reliability requirement.At present electric vacuum tube adopts the ceramic-to-metal seal technology mostly because the needs that connect, need the vitrified pipe connecting portion carry out metalized, the coated metallic membrane.Its technology is that sintering forms in two steps, and concrete processing step is:
1, vitrified pipe surface glazing;
2, send into High Temperature Furnaces Heating Apparatus, carry out the glaze sintering;
3, (muscle place in both ends of the surface reach) matel coated creme at the position that is needing metalized through the vitrified pipe behind the glaze sintering;
4, the vitrified pipe that will coat the metal creme is sent into atmosphere reduction furnace sintering.To each section (heating zone, flat-temperature zone, cooling area) of reducing atmosphere stove multiple spot input wet hydrogen and do wet mixing and close hydrogen respectively.The porcelain spare that sintering is finished again through the nickel plating subsequent disposal, is the metallization finished product.Its weak point need to be sintering twice, and the time-consuming effort of taking a lot of work wastes energy, and equipment is established money greatly, and the gradation sintering quality is difficult to stable control.
Summary of the invention
Purpose of the present invention provides a kind of once sintering method ceramic metallization treatment process at the above-mentioned deficiency of existing ceramic metallization treatment process exactly, and its treatment process steps is:
A, glazing and matel coated creme: glazing and needing the position matel coated creme of metalized on the vitrified pipe surface;
B, sintering: the vitrified pipe behind glazing and the matel coated creme is sent into the atmosphere reduction furnace carry out sintering; Concentrate the feeding wet hydrogen to point of atmosphere reduction furnace cooling section,, the wet hydrogen amount of feeding is controlled at 4.6-5.8M
3/ hour, the wet hydrogen dew point is at 25-39 ℃, the setting of each section of atmosphere reduction furnace temperature: 1000 ℃-1200 ℃ of heating zones, sintering time 30-50 minute; 1300 ℃-1460 ℃ of flat-temperature zones, sintering time 60-120 minute; 900 ℃-1200 ℃ of cooling areas.Sintering time 30-50 minute;
When sintering, feeding wet hydrogen to the atmosphere reduction furnace is to adopt the point in latter end that only is selected in reduction furnace to concentrate to feed wet hydrogen.Both guarantee the glaze sintering quality, also guaranteed the sintering quality of metal layer simultaneously.
The beneficial effect that the present invention adopts above-mentioned technical solution to reach is: 1, reduce glaze single fire program, the change double sintering is once-firing, need not dispose the glaze sintering oven, reduces facility investment.2, with each section multiple spot input wet hydrogen of former technology reducing atmosphere stove, change at cooling section and a bit import wet hydrogen, reduce impact and the stirring of cryogenic gas the flat-temperature zone temperature.Stablizing of the constant and atmosphere of assurance flat-temperature zone temperature prevents that the workpiece glaze quality from reducing or porcelain spare bursts, and guarantees the sintering quality of metal layer simultaneously.3, make full use of the interior hot conditions of atmosphere reduction furnace, in guaranteeing metallization agglomerating process, finish the glaze sintering, shortened the product process-cycle, enhance productivity more than 25%.4, because twice sintering of product merged into once-firing, energy consumption of unit product reduces about 20%.5, reduce production link, the stability that helps improving the quality of products.Detect through the user; the key technical indexes is on the leading domestic level; performances such as product bonding strength, resistance to air loss and thermal cycling have been improved; can adapt to the technical requirements of electrovacuum ceramics pipe metalized fully; large-scale production electrovacuum porcelain tube metallization series product, but also expanded application in the production of other special cermacis metal product.
Embodiment
The atmosphere reduction furnace is a common equipment, is provided with automated cycle in the reduction furnace and transports line, and whole sintering process circulation is carried out.Concrete operations are: glazing and needing the position matel coated creme of metalized on the vitrified pipe surface, glaze and metal creme belong to commercially available standard prod, then the vitrified pipe behind glazing and the matel coated creme is sent into the atmosphere reduction furnace and carry out sintering, concentrate the feeding wet hydrogen at point of end (cooling section) of atmosphere reduction furnace, the wet hydrogen amount that feeds in the atmosphere reduction furnace is adjusted at (during 5-5.8M3/), the wet hydrogen dew point is at 30-39 ℃, and whole sintering program is charging, preheating, intensification, constant temperature, cooling, cooled transition, water-cooled, discharging.Circulation section 8-10 of whole sintering time hour.The setting of each section of atmosphere reduction furnace temperature: 1000 ℃-1200 ℃ of heating zones, sintering time 30-50 minute; 1300 ℃-1460 ℃ of flat-temperature zones, sintering time 60-120 minute; 900 ℃-1200 ℃ of cooling areas, sintering time 30-50 minute.Concrete sintering time is decided on product.
Claims (1)
1, once sintering method ceramic metallization treatment process is characterized in that its treatment process steps is:
A, glazing and matel coated creme: glazing and needing the position matel coated creme of metalized on the vitrified pipe surface;
B, sintering: the vitrified pipe behind glazing and the matel coated creme is sent into the atmosphere reduction furnace carry out sintering; Concentrate the feeding wet hydrogen to point of atmosphere reduction furnace cooling section, the wet hydrogen amount of feeding is controlled at 4.6-5.8M
3/ hour, the wet hydrogen dew point is at 25-39 ℃, the setting of each section of atmosphere reduction furnace temperature: 1000 ℃-1200 ℃ of heating zones, sintering time 30-50 minute; 1300 ℃-1460 ℃ of flat-temperature zones, sintering time 60-120 minute; 900 ℃-1200 ℃ of cooling areas, sintering time 30-50 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100200761A CN100360474C (en) | 2005-12-15 | 2005-12-15 | Once sintering method ceramic metallization treatment process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100200761A CN100360474C (en) | 2005-12-15 | 2005-12-15 | Once sintering method ceramic metallization treatment process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1803726A CN1803726A (en) | 2006-07-19 |
| CN100360474C true CN100360474C (en) | 2008-01-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100200761A Expired - Fee Related CN100360474C (en) | 2005-12-15 | 2005-12-15 | Once sintering method ceramic metallization treatment process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100360474C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105734325A (en) * | 2016-03-17 | 2016-07-06 | 合肥晨煦信息科技有限公司 | Ceramic metal matrix composite and preparing method thereof |
| CN106830683A (en) * | 2017-03-17 | 2017-06-13 | 无锡康伟工程陶瓷有限公司 | The effective ceramic glazing technology of vacuum switch |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6272188A (en) * | 1985-09-26 | 1987-04-02 | Toshiba Corp | Laser tube |
| JPH04116170A (en) * | 1990-08-31 | 1992-04-16 | Nobuatsu Watanabe | Metallizing method |
| CN1415581A (en) * | 2002-10-24 | 2003-05-07 | 上海利浦电子陶瓷厂 | Method for preparing heat elimination base plate made from metalized ceramics |
-
2005
- 2005-12-15 CN CNB2005100200761A patent/CN100360474C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6272188A (en) * | 1985-09-26 | 1987-04-02 | Toshiba Corp | Laser tube |
| JPH04116170A (en) * | 1990-08-31 | 1992-04-16 | Nobuatsu Watanabe | Metallizing method |
| CN1415581A (en) * | 2002-10-24 | 2003-05-07 | 上海利浦电子陶瓷厂 | Method for preparing heat elimination base plate made from metalized ceramics |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1803726A (en) | 2006-07-19 |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080109 Termination date: 20121215 |