CN104876647A - Tungsten metalizing process of ceramic tube for ceramic discharge tube - Google Patents
Tungsten metalizing process of ceramic tube for ceramic discharge tube Download PDFInfo
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- CN104876647A CN104876647A CN201510176224.2A CN201510176224A CN104876647A CN 104876647 A CN104876647 A CN 104876647A CN 201510176224 A CN201510176224 A CN 201510176224A CN 104876647 A CN104876647 A CN 104876647A
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Abstract
The invention discloses a tungsten metalizing process of a ceramic tube for a ceramic discharge tube. The tungsten metalizing process comprises the following steps: step 1, paste preparation, namely 1, weighing tungsten powder and ceramic powder in the weight percentage ratio of 68% and 32%, and putting the tungsten powder and the ceramic powder in a ball-milling bottle for ball-milling by use of a 300-mesh sieve, 2, preparing an ethyecellulose solution, and 3, mixing the paste powder with the ethyecellulose solution and stirring evenly, and putting the mixture into the ball-milling bottle for ball-milling by use of the 300-mesh sieve, and filtering; step 2, paste coating; step 3, putting the ceramic tube coated in the step 2 on a molybdenum plate and performing metalizing sintering in an atmosphere protection furnace; step 4, further electroplating a nickel layer on the end face of the ceramic tube obtained after the metalizing sintering. The process only requires once coating, the metalizing cost is reduced, and the ceramic metalized layer obtained by use of the process is flat and good in solderability.
Description
Technical field
The present invention relates to the metallization technology field of high-alumina ceramic, refer to a kind of metallization technology field being applicable to compact ceramic discharge tube porcelain tube especially.
Background technology
At present, the porcelain tube that China produces discharge tube used is high-alumina ceramic (92 ~ 95Al
2o
3), the metallization process of porcelain piece generally adopts Activated Molybdenum manganese method, namely in metallizing formula, main component is molybdenum and manganese (or oxide compound of manganese), adds the composition (activator) such as aluminum oxide, calcium oxide, silicon oxide easily forming glassy phase in addition.This is a kind of thick film metal metallization processes, and the thickness of metalized film is generally at 15 ~ 40 μm.This needs metallization layer of paste coating thickness at 40 ~ 80 μm.And the layer of paste primary coating thickness that metallizes in our production process is generally 10 ~ 30 μm, this needs us painting cream operation layer of paste coating 2 ~ 3 times, or after the coating of metallization layer of paste, sintering, the layer of paste that metallizes again applies, then sinters, and so just can reach the requirement of metallization quality.If our metalized film layer thickness is thin, easily generation metalized film and porcelain piece bond bad, and during soldering, discharge tube leak rate is high.If we reach 60 ~ 80 μm by disposable coating thickness, will inevitably produce layer of paste in painting cream operation and along the circumferential direction produce a groove, namely affect the outward appearance of product, when discharge tube soldering, solder usage quantity is many again, and leak rate is high.
Summary of the invention
In order to solve the problem, the invention provides a kind of layer of metallized film thin, can disposable coating produce, metal layer is bonding with ceramic matrix firmly, the good ceramic metalizing process of intensity.
The tungsten metallization technique of the effective porcelain tube of ceramic discharge of the present invention, comprises the following steps:
Step one, prepared by paste:
Get the ultrafine tungsten powder that commercially available median size is 0.5 ~ 0.8 μm, median size is the porcelain powder of 1.3 ~ 1.8 μm;
Preparation cream powder: in (68% ~ 75%): the ratio of (32% ~ 25%) takes above-mentioned tungsten powder and porcelain powder, is placed in ball milling bottle ball milling 24 hours, and cross 300 mesh sieves;
Preparation ethyl cellulose solution: by Terpineol 350: ethyl cellulose=10:1 prepares ethyl cellulose solution;
Preparation paste: by cream powder: ethyl cellulose solution=3:1 takes starting material, be placed in special ball milling bottle ball milling more than 20 hours, use 300 mesh screen, for subsequent use;
B) paste coating
Use silk-screen printing machine special that paste is coated in discharge tube end face, coating thickness is 10 ~ 15 μm;
C) metalized film sintering
Coated porcelain tube is placed on molybdenum plate, loads in molybdenum boat, in atmosphere protection stove 1400 DEG C-1450 DEG C, wet hydrogen atmosphere (dew point 20 DEG C), sinter 1 ?2 hours; After sintering, metalized film thickness is about 4 ~ 8 μm;
D) electroplate
After metalized film sinters, re-plating one deck 1 ~ 5 μm of nickel dam, is beneficial to solder and scatters.
Beneficial effect of the present invention is: the first metallization cost reduces: conventional activation molybdenum manganese method metallized painting cream operation needs 2 ~ 3 coatings, and thickness reaches 40 ~ 80 μm, and some also needs twice metallization to sinter; The tungsten metallization technique of the effective porcelain tube of ceramic discharge of the present invention only needs primary coating thickness to be 10 ~ 15 μm, and the sintering that once metallizes completes.Two techniques are compared, and tungsten metallization technique had both saved paste cost, again save energy cost, cost of labor.Second production efficiency improves: tungsten metallization technique only needs primary coating, once sintered; And traditional molybdenum manganese method needs repeatedly to apply, repeatedly sinter.3rd good welding performance: the ceramic metallized layer that the tungsten metallization technique of the effective porcelain tube of ceramic discharge of the present invention obtains is smooth, and metalized film thickness is little, and size control is good, and the amount of solder used during soldering is few, good welding performance; Conventional activation molybdenum manganese method metal layer planeness is relatively poor, and metalized film is thicker, and weld interval, gap was comparatively large, used solder many, welding property relative mistake.
Embodiment
Below for the tungsten metallization technique of the effective porcelain tube of ceramic discharge of the present invention mainly comprises the steps:
Step one, prepared by paste, comprise the steps:
Step 1, takes tungsten powder and porcelain powder by the weight percent of 68%:32%, the two is mixed, and is placed in ball milling bottle ball milling 26 hours, and being equipped to cream powder, to cross 300 mesh sieves for subsequent use;
Step 2, preparation binding agent.Described binding agent is ethyl cellulose solution.Concrete is that 10:1 prepares ethyl cellulose solution by the weight percent of Terpineol 350 and ethyl cellulose.
Step 3 by the material powder for preparing and ethyl cellulose solution mixing and stirring, and is placed in ball milling bottle ball milling at least 20 hours, crosses 300 mesh sieves, makes paste for subsequent use.Concrete, the two is mixed with the weight percent 3:1 of ethyl cellulose solution by material powder.
Step 2, paste applies: the end face coating thickness paste screen process press prepared in step one being coated in porcelain tube is 10 ~ 15 μm.Preferably, with screen process press coating thickness be the coat of 12 μm.Except can adopting silk screen printing, described paste coating can also adopt the mode of spraying or machinery coating.
Step 3, the metalized film sintering of porcelain tube: porcelain tube coated in step 2 is placed on molybdenum plate, loads in molybdenum boat, in atmosphere protection stove 1400 DEG C-1450 DEG C, under wet hydrogen atmosphere, sintering 1-2 hour.During concrete enforcement, in protective atmosphere, the content of water is 3 ~ 4vol%, and the content of hydrogen is 1.6 ~ 2vol%.The metalized film of the tungsten metallization technique under this wet hydrogen atmosphere is more smooth, and metallization quality is relatively more stable.
After step 3 sinters, the thickness of metalized film is 4 ~ 8 μm.Preferably, after sintering, the thickness of metalized film is 6.5 μm.
Step 4, after metalized film sinters, electroplates the nickel dam of one deck 1 ~ 5 μm at the end face of porcelain tube, be beneficial to solder and scatter.Concrete, the nickel dam of plating one deck 3 μm.
Enumerate embodiment below further to describe the present invention in detail.
Embodiment one: weigh the ultrafine tungsten powder 340 grams that commercially available median size is 0.5 ~ 0.7 μm, median size is 160 grams, the porcelain powder of 1.3 ~ 1.5 μm, the two is placed in ball milling bottle ball milling 24 hours, for subsequent use as cream powder with 300 mesh screen.Terpineol 350 is mixed by 10:1 with ethyl cellulose, is mixed with ethyl cellulose solution.Weigh 300 grams, the good cream powder of above-mentioned outfit, ethyl cellulose solution gets 100 grams, the two is placed in ball milling bottle ball milling 22 hours, uses 300 mesh screen, be namely mixed with required paste.Use special screen process press by the porcelain tube end face of above-mentioned paste application at ready high alumina ceramic pipe, form the metalized film that one deck coating thickness is 10 ~ 12 μm.Be placed in molybdenum boat by above-mentioned coated porcelain tube, in atmosphere protection stove under the wet hydrogen atmosphere of 1400 DEG C, sinter 1.2 hours, after sintering, metalized film thickness is 4 ~ 6 μm.After above-mentioned metalized film sinters, for the benefit of solder scatters, the nickel dam that re-plating one deck is 1 ~ 2 μm.What described wet hydrogen atmosphere was concrete can be N2/H2 gas mixture or Ar/H2 gas mixture.During concrete enforcement, in protective atmosphere, the content of water is 3.2 ~ 4vol%, and the content of hydrogen is 1.6 ~ 2vol%.
Embodiment two: weigh the ultrafine tungsten powder 750 grams that commercially available median size is 0.6 μm, median size is 250 grams, the porcelain powder of 1.5 μm, the two is placed in ball milling bottle ball milling 24 hours, for subsequent use as cream powder with 300 mesh screen.Terpineol 350 is mixed by 10:1 with ethyl cellulose, is mixed with ethyl cellulose solution.Weigh 570 grams, the good cream powder of above-mentioned outfit, ethyl cellulose solution gets 190 grams, the two is placed in ball milling bottle ball milling 30 hours, uses 300 mesh screen, be namely mixed with required paste.Use the mode of machinery printing by the end face of above-mentioned paste application at ready high alumina ceramic pipe, form the metalized film that one deck coating thickness is 13 ~ 15 μm.Be placed in molybdenum boat by above-mentioned coated porcelain tube, in atmosphere protection stove under the wet hydrogen atmosphere of 1450 DEG C, sinter 100 minutes, after sintering, metalized film thickness is 6 ~ 8 μm.After above-mentioned metalized film sinters, for the benefit of solder scatters, the nickel dam that re-plating one deck is 2 ~ 4 μm.What described wet hydrogen atmosphere was concrete can be N2/H2 gas mixture or Ar/H2 gas mixture.In protective atmosphere, the content of water is 3.5 ~ 5vol%, and the content of hydrogen is 1.8 ~ 2.5vol%.
Embodiment three: weigh the ultrafine tungsten powder 355 grams that commercially available median size is 0.5 ~ 0.7 μm, median size is 145 grams, the porcelain powder of 1.3 ~ 1.5 μm, the two is placed in ball milling bottle ball milling 24 hours, for subsequent use as cream powder with 300 mesh screen.Terpineol 350 is mixed by 10:1 with ethyl cellulose, is mixed with ethyl cellulose solution.Weigh 300 grams, the good cream powder of above-mentioned outfit, ethyl cellulose solution gets 100 grams, the two is placed in ball milling bottle ball milling 30 hours, uses 300 mesh screen, be namely mixed with required paste.Use silk-screen printing machine special by the end face of above-mentioned paste application at ready high alumina ceramic pipe, form the metalized film that one deck coating thickness is 10 ~ 12 μm.Be placed in molybdenum boat by above-mentioned coated porcelain tube, in atmosphere protection stove under the wet hydrogen atmosphere of 1420 DEG C, sinter 60 minutes, after sintering, metalized film thickness is 4 ~ 7 μm.After above-mentioned metalized film sinters, for the benefit of solder scatters, the nickel dam that re-plating one deck is 2.5 ~ 3.5 μm.What described wet hydrogen atmosphere was concrete can be N2/H2 gas mixture or Ar/H2 gas mixture.In protective atmosphere, the content of water is 3.5 ~ 5vol%, and the content of hydrogen is 1.8 ~ 2.5vol%.
Embodiment four: weigh the ultrafine tungsten powder 740 grams that commercially available median size is 0.6 ~ 0.8 μm, median size is 260 grams, the porcelain powder of 1.5 ~ 1.8 μm, the two is placed in ball milling bottle ball milling 24 hours, for subsequent use as cream powder with 300 mesh screen.Terpineol 350 is mixed by 10:1 with ethyl cellulose, is mixed with ethyl cellulose solution.Weigh 480 grams, the good cream powder of above-mentioned outfit, ethyl cellulose solution gets 160 grams, the two is placed in ball milling bottle ball milling 22 hours, uses 300 mesh screen, be namely mixed with required paste.Use the mode of machinery printing by the end face of above-mentioned paste application at ready high alumina ceramic pipe, form the metalized film that one deck coating thickness is 13 ~ 15 μm.Be placed in molybdenum boat by above-mentioned coated porcelain tube, in atmosphere protection stove under the wet hydrogen atmosphere of 1420 DEG C, sinter 150 minutes, after sintering, metalized film thickness is 5 ~ 6 μm.After above-mentioned metalized film sinters, for the benefit of solder scatters, the nickel dam that re-plating one deck is 3 ~ 5 μm.What described wet hydrogen atmosphere was concrete can be N2/H2 gas mixture or Ar/H2 gas mixture.In protective atmosphere, the content of water is 4vol%, and the content of hydrogen is 2.6vol%.
The tungsten metallization technique of the effective porcelain tube of ceramic discharge of the present invention has the following advantages relative to existing Activated Molybdenum manganese method metallization process:
The first, metallization cost reduces: conventional activation molybdenum manganese method metallized painting cream operation needs 2 ~ 3 coatings, and thickness reaches 40 ~ 80 μm, and some also needs twice metallization to sinter; The tungsten metallization technique of the effective porcelain tube of ceramic discharge of the present invention only needs primary coating thickness to be 10 ~ 15 μm, and the sintering that once metallizes completes.Therefore, two techniques are compared, and tungsten metallization technique had both saved paste cost, again save energy cost, cost of labor.
The second, production efficiency improves: tungsten metallization technique only needs primary coating, once sintered; And traditional molybdenum manganese method needs repeatedly to apply, repeatedly sinter.
3rd, good welding performance: the ceramic metallized layer that the tungsten metallization technique of the effective porcelain tube of ceramic discharge of the present invention obtains is smooth, and metalized film thickness is little, and size control is good, and the amount of solder used during soldering is few, good welding performance; Conventional activation molybdenum manganese method metal layer planeness is relatively poor, and metalized film is thicker, and weld interval, gap was comparatively large, used solder many, welding property relative mistake.
4th, adopt tungsten and ceramics powder as the formula of cream powder, adaptability is good, and Ceramic bond intensity is good, and metallization quality good stability, quality product is more secure.
5th, this technique is specially adapted to the metallization of compact discharge pipe porcelain tube.Compact discharge pipe usage quantity is large, but due to compact discharge pipe porcelain shell size little, porcelain shell wall is thick only has about 0.3 ~ 1.5mm, and metalized film overweight coating, easily occurs groove, affects metallization quality.And because metallization area is less, require just higher to metallization quality, tungsten metallization technique more can ensure the metallization quality of compact discharge pipe porcelain tube.
Claims (10)
1. a tungsten metallization technique for the effective porcelain tube of ceramic discharge, is characterized in that comprising the following steps:
Step one, prepared by paste, comprise following step: step 1, take tungsten powder and porcelain powder by the weight percent of 68%:32%, and be placed in ball milling bottle ball milling, and being equipped to cream powder, to cross 300 mesh sieves for subsequent use; Step 2, refer to by Terpineol 350 and ethyl cellulose by weight percentage 10:1 be hybridly prepared into ethyl cellulose solution; Step 3, by the cream powder for preparing and ethyl cellulose solution mixing and stirring, and is placed in ball milling bottle 300 mesh sieve ball milling, makes paste, filter for subsequent use;
Step 2, paste applies: the end face mode that the paste screen process press prepared in step one or machinery print being coated in porcelain tube;
Step 3, the metalized film sintering of porcelain tube: porcelain tube coated in step 2 is placed on molybdenum plate, loads in molybdenum boat, in atmosphere protection stove, under wet hydrogen atmosphere, sinter 1 ?2 hours; Step 4, end face re-plating one deck nickel dam of the porcelain tube after metalized film sintering.
2. the tungsten metallization technique of the effective porcelain tube of ceramic discharge according to claim 1, is characterized in that: in paste described in step one, the weight percent of cream powder and ethyl cellulose solution is 3:1.
3. the tungsten metallization technique of the effective porcelain tube of ceramic discharge according to claim 1, is characterized in that: in step 3, the metalized film sintering process of porcelain tube is carried out in the hydrogen furnace of 1400 DEG C of ?1450 DEG C.
4. the tungsten metallization technique of the effective porcelain tube of ceramic discharge according to claim 1, is characterized in that: in wet hydrogen atmosphere described in step 3, the content of aqueous vapor is 3.2 ~ 4vol%, and the content of hydrogen is 1.6 ~ 2vol%
5. the tungsten metallization technique of the effective porcelain tube of ceramic discharge according to claim 1, is characterized in that: the median size of described tungsten powder is 0.5 ~ 0.8 μm.
6. the tungsten metallization technique of the effective porcelain tube of ceramic discharge according to claim 5, is characterized in that: the median size of described porcelain powder is 1.3 ~ 1.8 μm.
7. the tungsten metallization technique of the effective porcelain tube of the ceramic discharge according to claim 5 or 6, is characterized in that: the time of the powder of cream described in step 1 ball milling in ball milling bottle is 24 hours, and in step 3, the time of ball milling is at least 20 hours.
8. the tungsten metallization technique of the effective porcelain tube of the ceramic discharge according to any one of Claims 1 to 4, is characterized in that: in step 2, the thickness of paste coating is 10 ~ 15 μm.
9. the tungsten metallization technique of the effective porcelain tube of the ceramic discharge according to any one of Claims 1 to 4, is characterized in that: after sintering, metalized film thickness is about 4 ~ 8 μm.
10. the tungsten metallization technique of the effective porcelain tube of the ceramic discharge according to any one of Claims 1 to 4, is characterized in that: in step 4, the thickness of electroless nickel layer is 1 ~ 5 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347851A (en) * | 2015-11-03 | 2016-02-24 | 孝感正华电真空材料有限责任公司 | Method for metallization sintering of ceramic gas discharge tube dry-pressed porcelain tube |
| CN105384469A (en) * | 2015-11-03 | 2016-03-09 | 孝感正华电真空材料有限责任公司 | Nickel burning method for metallized ceramic tube for ceramic gas discharge tube |
| CN107359499A (en) * | 2017-07-09 | 2017-11-17 | 湖南省众精细陶瓷制造有限公司 | The packaging technology of ceramic discharge tube |
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| 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 |
| CN103189975A (en) * | 2010-11-01 | 2013-07-03 | 日铁住金电设备株式会社 | Package for storing electronic component elements |
| 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 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103189975A (en) * | 2010-11-01 | 2013-07-03 | 日铁住金电设备株式会社 | Package for storing electronic component elements |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347851A (en) * | 2015-11-03 | 2016-02-24 | 孝感正华电真空材料有限责任公司 | Method for metallization sintering of ceramic gas discharge tube dry-pressed porcelain tube |
| CN105384469A (en) * | 2015-11-03 | 2016-03-09 | 孝感正华电真空材料有限责任公司 | Nickel burning method for metallized ceramic tube for ceramic gas discharge tube |
| CN107359499A (en) * | 2017-07-09 | 2017-11-17 | 湖南省众精细陶瓷制造有限公司 | The packaging technology of ceramic discharge tube |
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