CN101439982A - Process for sealing ceramic-stainless steel - Google Patents
Process for sealing ceramic-stainless steel Download PDFInfo
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- CN101439982A CN101439982A CNA2007101503099A CN200710150309A CN101439982A CN 101439982 A CN101439982 A CN 101439982A CN A2007101503099 A CNA2007101503099 A CN A2007101503099A CN 200710150309 A CN200710150309 A CN 200710150309A CN 101439982 A CN101439982 A CN 101439982A
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Abstract
The invention provides a ceramic-to-stainless steel seal process. The process comprises the steps of processing a ceramic sheet and a stainless steel sheet, preparing a bonding agent, preparing a glass paste, coating the paste, oxidizing the stainless steel sheet, and sealing. The process has the advantages that the process improves a low-temperature oxide solder method for adapting ceramic-stainless steel seal, and achieves good seal performance, airtight performance and seal strength in terms of influences of the glass paste on the impregnation of a 95 aluminum oxide ceramic sheet and stainless steel sheet, the influences of the thickness of an oxidation film of the stainless steel sheet on the seal performance and the interface conditions of a seal piece. A proper thickness of an oxidation film on the surface of the stainless steel is more favorable for seal.
Description
Technical field
The present invention relates to a kind of weldprocedure, particularly a kind of pottery-stainless sealing process.
Background technology
At today function ceramics, engineering ceramics, under the situation that high-temperature structural ceramics and biological ceramics etc. develops rapidly, alumina-ceramic still has one seat, does not also see having what material can replace its possibility in a large number at present.Particularly all the more so in Application Areass such as vacuum switch, microwave tube, power electronics and discharge tube shell.
Over more than 20 year, high-alumina ceramic does not have too big changes and improvements on prescription and component, although in recent years, some experts have done a little discussions on additive both at home and abroad, and benefiting to some extent on the performance or on the sintering temperature, is limited after all yet.
The metal current temperature has two kinds of tendencies, and the one, American and Britain, the Germany man high temperature metallizations that adopt more, general temperature is 1500-1550 ℃; The one, country such as the Japan and Korea S. low temperature metalizations that adopt more, general temperature is 1300-1400 ℃, the advantage of low temperature metalization is a save energy, porcelain spare is not easy distortion, and metallizing temperature and the relatively good processing of glaze maturing temperature, American-European countries thinks that then high temperature metallization can improve sealing strength, thereby adopts high melting glaze or glaze, the once sintered operational path of metallization.
Sealing process commonly used at present is the metal-powder method, and the sealing-in quality of this sealing-in method is higher, but the sealing-in cost is very high, the control of sealing-in difficult quality.The low temperature oxide solder method generally is usually used in the sealing-in of glass and glass, if can to make it be adapted to pottery-stainless sealing-in will be to have very to be badly in need of by improving its technology.Because high-alumina ceramic has high mechanical strength, low high-frequency loss, high insulation resistance and good thermal characteristics, particularly abundant raw material, technical maturity, cheap, so Application Areas is very broad, market outlook are still good.
Summary of the invention
The purpose of this invention is to provide a kind of pottery-stainless sealing process, its preparation method technology is simple, helps realizing the improvement to the water environment pollution situation.
For achieving the above object, technical solution of the present invention provides a kind of pottery-stainless sealing process, and this method may further comprise the steps:
(1) processing of ceramic plate and stainless steel substrates
Preparation scavenging solution: yellow soda ash 10g, tertiary sodium phosphate 6g, OP emulsifying agent 1.2g and water 40ml; Ceramic plate and stainless steel substrates are put into the beaker that above-mentioned scavenging solution is housed, in ultrasonic cleaner, clean 30min, in 70-80 ℃, soak 10min; Use distilled water cleaning ceramic sheet 3-5 times again, and then clean with dehydrated alcohol, oven dry at last, the ceramic plate that is about to wash is prevented drying under 120 ℃ in the baking oven;
(2) preparation of binding agent
Ethyl cellulose with 6%, the heating of 94% Terpineol 350 mix, and it is standby to put into vial;
(3) preparation of glass paste
General window glass is pulverized the back on planetary ball mill, carry out wet-milling, the condition of wet-milling is material: ball: water=1:2:1, after the wet-milling, in the electric heating constant temperature air dry oven, carry out drying, temperature is 120 ℃, the median size of analyzing glass powder through laser particle size analyzer is below the 5 μ m, deposits standbyly, is 680-790 ℃ with high temperature rerum natura determinator mensuration glass melting temperature range; A certain amount of glass powder for preparing is poured in the agate mortar, slowly added in the above-mentioned binding agent, fully grind evenly standby then;
(4) coating of paste
Pick above-mentioned glass paste with writing brush, spread upon above-mentioned ceramic plate surface equably, after being coated with ceramics being put into baking oven dries, temperature is controlled at about 120 ℃, keep the coatingsurface quality, parch taking-up fully up to paste, the ceramic plate surface after oven dry evenly is coated with the above-mentioned glass paste of one deck again, again oven dry;
(5) oxide treatment of stainless steel substrates
Stainless steel substrates to above-mentioned cleaning before sealing-in carries out oxide treatment, make its surface form the oxide film of one deck Slate grey band metalluster, method for oxidation is that stainless steel substrates is placed in the stainless steel box, places in 700 ℃ the retort furnace, behind the insulation 10min-30min, take out and rock air cooling to room temperature;
(6) sealing-in
The stainless steel substrates of oxide treatment is placed on the ceramic plate that scribbles the glass paste, presses a weight to carry out sintering at it; Then, be incubated after being warmed up to sealing temperature, again furnace cooling.
To be this method make it be adapted to pottery-stainless sealing-in by improving low temperature oxide solder method technology to effect of the present invention, studies a kind of low cost, sealing process that performance is high.Studied the wetting property of glass glaze to 95 alumina ceramic chips and stainless steel substrates, the thickness of the oxide film of stainless steel substrates is to the influence of sealing property and the interface conditions of closure.This glass glaze has sealing-in preferably to changing system, and the oxide film of stainless steel surface suitable thickness is favourable to sealing-in.This experiment is the sealing-in scolder with the glass glaze, has obtained certain sealing strength and bubble-tight closure.
Description of drawings
Fig. 1 is the wetting situation of glass paste of the present invention to ceramic plate;
Fig. 2 is the wetting situation of glass paste of the present invention to stainless steel substrates;
Fig. 3 carries out the oxidized surface situation of oxide treatment for stainless steel substrates of the present invention;
Fig. 4 is zone of oxidation of the present invention/glass paste/stainless interface conditions;
Fig. 5 is the energy spectrogram of glass layer of paste in the closure of the present invention.
Embodiment
In conjunction with the accompanying drawings pottery of the present invention-stainless sealing process is described in detail:
Technical solution of the present invention provides a kind of pottery-stainless sealing process, and this method may further comprise the steps: with 95 alumina ceramic plates and 1Cr18Ni9Ti stainless steel substrates is example
(1) processing of ceramic plate and stainless steel substrates
95 alumina ceramic plates and 1Cr18Ni9Ti stainless steel substrates are put into the beaker that scavenging solution is housed, in ultrasonic cleaner, clean 30min.The prescription of scavenging solution: yellow soda ash 10g, tertiary sodium phosphate 6g, OP emulsifying agent 1.2g, water 40ml soaks 10min in 70-80 ℃.Use distilled water cleaning ceramic sheet 3-5 times again, and then clean with dehydrated alcohol.Oven dry at last, the ceramic plate that is about to wash is prevented drying under 120 ℃ in the baking oven.
(2) preparation of binding agent
The heating of 6% ethyl cellulose, 94% Terpineol 350 mixes that to put into vial standby.
(3) preparation of glass paste
General window glass is pulverized the back on planetary ball mill, carry out wet-milling (material: ball: water=1:2:1), after the wet-milling, in the electric heating constant temperature air dry oven, carry out drying, 120 ℃ of temperature, the median size of analyzing glass powder through laser particle size analyzer is below the 5 μ m, deposits standby.Measure the glass melting temperature range with high temperature rerum natura determinator and be 680-790 ℃.A certain amount of glass powder for preparing is poured in the agate mortar, slowly splashed into binding agent (can suitably heat again and drip), fully grind evenly then.
(4) coating of paste
Pick the glass paste with writing brush, spread upon 95 alumina ceramic plate surfaces as far as possible equably, after being coated with ceramics is put into baking oven oven dry (temperature is controlled at about 120 ℃, notes not touching coat side) and parch taking-up fully up to paste, standby.Because coat-thickness has certain influence to the sealing-in quality, when especially coating was too thin, the interface was imperfect, and intensity is for reducing, so this experiment is coated with two-layerly, promptly evenly was coated with one deck paste again after oven dry, again oven dry.
(5) oxide treatment of stainless steel substrates
Before sealing-in, must carry out oxide treatment to the stainless steel substrates that cleaned, make its surface form the oxide film of one deck Slate grey band metalluster, method for oxidation is that part is placed in the stainless steel box, place in 700 ℃ the retort furnace, insulation 10min, 20min behind the 30min, takes out and rocks air cooling rapidly to room temperature.
(6) sealing-in
Stainless steel substrates is placed on the ceramics that scribbles the glass paste, is pressing a weight can carry out sintering.The beginning heat-up rate should not be too fast, to guarantee Terpineol 350, the slowly fully volatilization of ethyl cellulose in the low melting glass cream, then, is incubated certain hour be warmed up to the sealing temperature of low melting glass by certain speed after, again furnace cooling.
1, the glass paste is to 95Al
2O
3The wettability of ceramics and 1Cr18Ni9Ti stainless steel substrates
For making sealing process simple, sealing strength height, resistance to air loss are good, general basic demand to glass solder is: can fusion under the low temperature below 900 ℃, with precise measure that guarantees stainless steel part (heat-drawn wire is general〉1000 ℃) and the energy consumption that reduces sealing-in as far as possible; On the other hand, the glass glaze must all have wettability like this to porcelain spare and stainless steel part, and glass paste fused solution could easily flow in the gap of each parts and go, and forms fine and close glass coating under suitable speed of cooling.
The raw material of preparation glass paste at high temperature generally all can be emitted a certain amount of moisture and gas, if raw material mixing directly carrying out sealing-in, not only be not easy wetting ceramic member and metallic surface, and the glass layer of paste also forms pore easily, cause the reduction of sealing strength, therefore generally all prepare the glass flour earlier, ball milling is made the glass powdered frit again.This experiment usefulness be that common window glass is made glass powder through ball milling.Below be that the glass paste is to 95Al
2O
3The wetting situation of porcelain and 1Cr18Ni9Ti stainless steel substrates.
Can find out that from Fig. 1 and Fig. 2 this glass paste is to 95Al
2O
3The wettability of porcelain is very good, and cohesive strength is also very high, and the glass paste is just relatively poor to the wettability of the 1Cr18Ni9Ti stainless steel substrates that passes through oxide treatment in advance, and the cohesive strength between them is also lower.This mainly is because glass paste and 95Al
2O
3Chemical ingredients very approaching, according to the similar compatibility principle, in certain temperature, can interpenetrate between their composition, form compact transition layer.Although and the 1Cr18Ni9Ti stainless steel substrates has passed through oxide treatment, the surface has had one deck with Fe
2O
3Be main metal oxide film, but oxide film is thin, the composition of composition and glass glaze also has certain difference, so interpenetrating between them is relatively poor, and wettability is relatively poor, and cohesive strength is lower.
2, oxide thickness is to the influence of sealing property
So-called oxide compound is meant the processing of metal before sealing-in, form one deck oxide film in the metallic surface, the sealing-in of glass metal, mainly be to utilize glass suboxide and glass head seal, therefore metal is carried out also will heat-treating after the cleaning, make metallic surface formation one deck oxide compound and reach wetting effect.
The metallic surface of preheating can form metal oxide layer, and the surperficial suboxide of metallic matrix is from chemical bond type angle, and it approaches metal, therefore can combine securely with metal; And the chemical bond of the higher extexine oxide compound of degree of oxidation and glassy phase are seemingly, so can combine with glass, therefore, excessively layer is most important to glass-metal sealing for this.
The time that table 1 stainless steel oxide is handled is to the influence of sealing property
| The time (min) that stainless steel oxide is handled | 10 | 20 | 30 |
| Sealing strength (MPa) | 5.6 | 12 | 10 |
| Resistance to air loss | It is bigger to leak gas | Gas leakage is minimum | It is less to leak gas |
Can find out that from table 1 when oxide film was too thick, oxide film just was easy to all be dissolved in the vitreum, thereby had influence on intensity and resistance to air loss; When oxide film was too thin, the two wettability will be very poor, can not form good sealing-in.
3, the microtexture at closure interface
Can find out from Fig. 3 and Fig. 4, before and after sealing-in, obvious variation does not take place in alumina-ceramic, tangible sealing layer is arranged between ceramic plate and stainless steel substrates, but between ceramic plate and oxide glass paste and the interface between stainless steel substrates and oxide glass paste all has preferably and interpenetrates, and the interface is more complete.Therefore intensity and resistance to air loss are all better.As can be seen from Figure 5, in the middle part of glass paste sealing layer, still keep the component of glass, component is not obvious to the infiltration of glass layer of paste in stainless steel and the ceramic member.
Claims (1)
1, a kind of pottery-stainless sealing process, this method may further comprise the steps:
(1) processing of ceramic plate and stainless steel substrates
Preparation scavenging solution: yellow soda ash 10g, tertiary sodium phosphate 6g, OP emulsifying agent 1.2g and water 40ml; Ceramic plate and stainless steel substrates are put into the beaker that above-mentioned scavenging solution is housed, in ultrasonic cleaner, clean 30min, in 70-80 ℃, soak 10min; Use distilled water cleaning ceramic sheet 3-5 times again, and then clean with dehydrated alcohol, oven dry at last, the ceramic plate that is about to wash is prevented drying under 120 ℃ in the baking oven;
(2) preparation of binding agent
Ethyl cellulose with 6%, the heating of 94% Terpineol 350 mix, and it is standby to put into vial;
(3) preparation of glass paste
General window glass is pulverized the back on planetary ball mill, carry out wet-milling, the condition of wet-milling is material: ball: water=1:2:1, after the wet-milling, in the electric heating constant temperature air dry oven, carry out drying, temperature is 120 ℃, the median size of analyzing glass powder through laser particle size analyzer is below the 5 μ m, deposits standbyly, is 680-790 ℃ with high temperature rerum natura determinator mensuration glass melting temperature range; A certain amount of glass powder for preparing is poured in the agate mortar, slowly added in the above-mentioned binding agent, fully grind evenly standby then;
(4) coating of paste
Pick above-mentioned glass paste with writing brush, spread upon above-mentioned ceramic plate surface equably, after being coated with ceramics being put into baking oven dries, temperature is controlled at about 120 ℃, keep the coatingsurface quality, parch taking-up fully up to paste, the ceramic plate surface after oven dry evenly is coated with the above-mentioned glass paste of one deck again, again oven dry;
(5) oxide treatment of stainless steel substrates
Stainless steel substrates to above-mentioned cleaning before sealing-in carries out oxide treatment, make its surface form the oxide film of one deck Slate grey band metalluster, method for oxidation is that stainless steel substrates is placed in the stainless steel box, places in 700 ℃ the retort furnace, behind the insulation 10min-30min, take out and rock air cooling to room temperature;
(6) sealing-in
The stainless steel substrates of oxide treatment is placed on the ceramic plate that scribbles the glass paste, presses a weight to carry out sintering at it; Then, be incubated after being warmed up to sealing temperature, again furnace cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101503099A CN101439982A (en) | 2007-11-22 | 2007-11-22 | Process for sealing ceramic-stainless steel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101503099A CN101439982A (en) | 2007-11-22 | 2007-11-22 | Process for sealing ceramic-stainless steel |
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| CN101439982A true CN101439982A (en) | 2009-05-27 |
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| CNA2007101503099A Pending CN101439982A (en) | 2007-11-22 | 2007-11-22 | Process for sealing ceramic-stainless steel |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857457A (en) * | 2010-05-19 | 2010-10-13 | 中国电子科技集团公司第四十三研究所 | Transition layer for combination of ceramic composite substrate and metal and preparation method thereof |
| CN102875180A (en) * | 2012-11-07 | 2013-01-16 | 王向阳 | Method for connecting ceramics and aluminum metal |
| CN104276836A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Sealing method based on negative thermal expansion sealing medium |
| CN104276837A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Metal vitrification sealing method |
| CN104276838A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Double vitrifying sealing method of ceramic and metal |
| CN104276839A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Sealing method for ceramic vitrification |
| CN106735728A (en) * | 2016-11-29 | 2017-05-31 | 长春工业大学 | A kind of connection method of ceramic-lined composite steel tube |
| CN107285648A (en) * | 2017-05-15 | 2017-10-24 | 淮北蓄煌新能源科技有限公司 | A kind of method for welding between nonmetallic materials and metal material |
| CN111689690A (en) * | 2019-03-13 | 2020-09-22 | 陆焕炯 | Production process of silicate coating inside and outside stainless steel utensil |
-
2007
- 2007-11-22 CN CNA2007101503099A patent/CN101439982A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857457A (en) * | 2010-05-19 | 2010-10-13 | 中国电子科技集团公司第四十三研究所 | Transition layer for combination of ceramic composite substrate and metal and preparation method thereof |
| CN102875180A (en) * | 2012-11-07 | 2013-01-16 | 王向阳 | Method for connecting ceramics and aluminum metal |
| CN104276836A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Sealing method based on negative thermal expansion sealing medium |
| CN104276837A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Metal vitrification sealing method |
| CN104276838A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Double vitrifying sealing method of ceramic and metal |
| CN104276839A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Sealing method for ceramic vitrification |
| CN104276838B (en) * | 2013-07-12 | 2016-01-06 | 中国科学院上海硅酸盐研究所 | Pottery vitrified method for sealing two with metal |
| CN104276839B (en) * | 2013-07-12 | 2016-05-18 | 中国科学院上海硅酸盐研究所 | The method for sealing of glass-ceramic |
| CN104276836B (en) * | 2013-07-12 | 2016-08-10 | 中国科学院上海硅酸盐研究所 | Method for sealing based on negative expansion sealing medium |
| CN104276837B (en) * | 2013-07-12 | 2016-09-07 | 中国科学院上海硅酸盐研究所 | The method for sealing of glassy metal |
| CN106735728A (en) * | 2016-11-29 | 2017-05-31 | 长春工业大学 | A kind of connection method of ceramic-lined composite steel tube |
| CN107285648A (en) * | 2017-05-15 | 2017-10-24 | 淮北蓄煌新能源科技有限公司 | A kind of method for welding between nonmetallic materials and metal material |
| CN111689690A (en) * | 2019-03-13 | 2020-09-22 | 陆焕炯 | Production process of silicate coating inside and outside stainless steel utensil |
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Open date: 20090527 |