CN103332872A - Direct matched sealing method of high borosilicate hard glass and kovar alloy - Google Patents

Direct matched sealing method of high borosilicate hard glass and kovar alloy Download PDF

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Publication number
CN103332872A
CN103332872A CN2013102416159A CN201310241615A CN103332872A CN 103332872 A CN103332872 A CN 103332872A CN 2013102416159 A CN2013102416159 A CN 2013102416159A CN 201310241615 A CN201310241615 A CN 201310241615A CN 103332872 A CN103332872 A CN 103332872A
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kovar alloy
sealing
glass
boron
hard glass
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CN2013102416159A
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CN103332872B (en
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阚存东
李晓勇
张沪基
刑胜平
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Beijing leyfond Vacuum Technology Co., Ltd.
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Nanjing Sanle Electronic Information Industry Group Co Ltd
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Abstract

The invention discloses a direct matched sealing method of high borosilicate hard glass and kovar alloy. The direct matched sealing method comprises the following steps of: (1) firstly, carrying out surface sand blasting texturing treatment on the kovar alloy with the expansion coefficient of 3.0*10<-6>/K, and then placing the kovar alloy subjected to the sand blasting texturing treatment in a hydrogen burning furnace so as to carry out hydrogen burning treatment; sealing the kovar alloy subjected to the hydrogen burning treatment and the high borosilicate glass at 120-130 DEG C high temperature. The direct matched sealing method provided by the invention has the advantages that the operability is strong, the technological design is reasonable, the direct matched sealing of the high borosilicate hard glass and the kovar alloy can be realized, a step of using four transitional glass with the expansion coefficient between a 3.3 high borosilicate glass outer tube and 4J29 kovar alloy for transitional sealing in an original sealing technology can be greatly simplified, the production efficiency is high, the product quality is high, and the production cost is low.

Description

The direct matched seal method of high borosilicate hard glass and kovar alloy
Technical field
The present invention designs the method for sealing of a kind of glass and metal, is specifically related to a kind of high borosilicate hard glass and the direct matched seal method of kovar alloy.
Background technology
High-boron-silicon glass (having another name called hard glass) is because coefficient of linear thermal expansion is (3.3 scholar 0.1) * 10 -6/ K also is referred to as " borosilicate glass 3.3 ".It is the specific glass material of a kind of low thermal expansion, high temperature resistant, high strength, high rigidity, high transmission rate and high chemical stability, because of its excellent performance, is widely used in industries such as sun power, chemical industry, medical packaging, electric light source, artwork Ornament.Its superperformance has obtained the extensive approval of world all circles, particularly field of solar energy is used more extensive, high-temperature heat-collection pipe is formed the double wall tube that interlayer is vacuum by pipe in 3.3 high-boron-silicon glass outer tubes and the stainless steel metal in the sun power, therefore, need carry out the sealing-in of 3.3 high-boron-silicon glass outer tubes and metal inner pipe, sealing strength and resistance to air loss are the key influence factors in thermal-collecting tube quality and life-span.Because the coefficient of expansion of glass is about (3.3 scholar 0.1) * 10 -6/ K, excessive with the coefficient of expansion gap of pipe in the stainless steel, generally adopt low expansion alloy 4J29 to cut down, as transition metal, but the coefficient of expansion of 4J29 kovar alloy is 5.3 * 10 -6/ K, and the reliable coefficient of expansion of glass and metal sealing is poor, can not surpass 15%, therefore, the sealing-in of prior art need adopt 4 kinds of coefficients of expansion between the transitional glass of 3.3 high-boron-silicon glass and 4J29 kovar alloy, carries out transition sealing, though the transition sealing quality can meet the demands, but production efficiency is low, the steady quality consistence is poor, the production cost height, is difficult to apply.
Therefore, necessary on the basis of prior art, research and design is a kind of to be approached with the high-boron-silicon glass coefficient of expansion, need not to adopt multiple transition alloy, the high borosilicate hard glass that production efficiency is high and the direct matched seal method of kovar alloy.
Summary of the invention
Goal of the invention: the objective of the invention is in order to solve the deficiencies in the prior art, provide a kind of component proportioning scientific and reasonable, especially the coefficient of expansion is 3.0 * 10 -6/ K, good with the high-boron-silicon glass matched coefficients of thermal expansion, can be directly and the high-boron-silicon glass kovar alloy that carries out matched seal, the coefficient of expansion that adopts the present invention to obtain by a large amount of experiment screenings is 3.0 * 10 -6/ K kovar alloy can carry out direct sealing-in with high-boron-silicon glass, and whole technological operation is strong, and technological design is reasonable, products production efficient height, quality product high conformity.
Technical scheme: in order to realize above purpose, the technical solution used in the present invention is:
A kind of high borosilicate hard glass and the direct matched seal method of kovar alloy, it may further comprise the steps:
(1) get the kovar alloy that the coefficient of expansion is 3.0 * 10-6/K, carry out the surface sand-blasting texturing earlier and handle, the kovar alloy that sandblast texturing was handled places hydrogen-burning stove to burn the wet hydrogen processing then;
(2) kovar alloy and the high-boron-silicon glass of getting the processing of step (1) annealing in hydrogen atmosphere carries out sealing-in under high temperature (1200 ℃~1300 ℃) condition.
The described coefficient of expansion is that the kovar alloy of 3.0 * 10-6/K is become to be grouped into by following weight percent:
Ni 27%~32%, and Co 11%~15%, and Mn 0.3%~0.5%, and Si 0%~0.2%, and Cr 0%~0.2%, and Cu 0.15%~0.2%, and Mo 0.15%~0.2%, and S 0%~0.025%, and P 0%~0.025%, and C 0.05%~0.06%, remains to be Fe;
(3) get the good kovar alloy of step (2) sealing-in and high-boron-silicon glass and under 1000 ℃~1100 ℃ conditions, carry out anneal.
As preferred version, the coefficient of expansion of the present invention is that the kovar alloy of 3.0 * 10-6/K is become to be grouped into by following weight percent:
Ni 27%~32%, and Co 11%~15%, and Mn 0.3%~0.5%, and Si 0.05%~0.2%, and Cr 0.05%~0.2%, and Cu 0.15%~0.2%, and Mo 0.15%~0.2%, and S 0.001%~0.025%, P0.001%~0.025%, and C 0.05%~0.06%, remains to be Fe;
The present invention is according to the physico-chemical property of high-boron-silicon glass and special thermal expansivity, by the moiety of a large amount of experiment screening kovar alloys and the weight proportion of each component, experimental result shows, the coefficient of expansion of the kovar alloy that the present invention preferably obtains is the special kovar alloy of 3.0 * 10-6/K, can realize the direct matched seal of glass and metal, can simplify existing sealing technology greatly adopts 4 kinds of coefficients of expansion to carry out the transition sealing method between the transitional glass of 3.3 high-boron-silicon glass and 4J29 kovar alloy, production efficiency is higher, the constant product quality high conformity of sealing-in, production cost is lower, has obtained extraordinary technique effect.
As preferred version, above-described high borosilicate hard glass and the direct matched seal method of kovar alloy, the temperature that the described burning wet hydrogen of step (1) is handled is 1050 ℃, burning the wet hydrogen time is 60 minutes.The present invention carries out sandblast texturing to the kovar alloy surface earlier and handles, can improve the compactness of kovar alloy and the sealing-in of high borosilicate hard glass, and the present invention is in order further to improve the compactness after kovar alloy and the sealing-in of high borosilicate hard glass, matching, the present invention is 1050 ℃ by the temperature that a large amount of experiment screening kovar alloys burn wet hydrogen, burning the wet hydrogen time is 60 minutes, after burning the wet hydrogen processing, can more thoroughly remove the kovar alloy surface impurity, reduce its internal stress, form compound easy and the high-boron-silicon glass fusion, can better improve and high borosilicate hard glass matched seal quality.
As preferred version, above-described high borosilicate hard glass and the direct matched seal method of kovar alloy, the sealing-in mode of step (2) are that kovar alloy is inserted into and carries out sealing-in or kovar alloy in the high-boron-silicon glass and dock with high-boron-silicon glass and carry out sealing-in.
The present invention is after optimizing the kovar alloy that the coefficient of expansion is 3.0 * 10-6/K and after burning the wet hydrogen treatment process, Heating temperature during again by a large amount of experiment screening sealing-in, by preferred 1200 ℃~1300 ℃ sealing-in Heating temperature of the present invention, can guarantee the perfect sealing-in of high borosilicate hard glass and kovar alloy, not only connect firmly stable, and good stability, long service life.Because temperature is too high, high borosilicate hard glass and kovar alloy are yielding, the quality product that sealing-in obtains is low, stability and consistence are poor, low can not make high borosilicate hard glass and kovar alloy finish tight sealing-in smoothly and cross as temperature, can produce space or bubble, the sealing-in of product is not tight, and quality is lower.
Beneficial effect: high borosilicate hard glass provided by the invention and the direct matched seal method of kovar alloy compared with prior art have the following advantages:
High borosilicate hard glass of the present invention and the direct matched seal method of kovar alloy, workable, technological design is reasonable, the production efficiency height, the quality conformance of the product for preparing is good.
Especially the present invention is by the moiety of a large amount of experiment screening kovar alloys and the weight proportion of each component, experimental result shows, the coefficient of expansion of the kovar alloy that the present invention preferably obtains is 3.0 * 10-6/K, can realize the direct matched seal with high borosilicate hard glass, can simplify existing sealing technology greatly adopts 4 kinds of coefficients of expansion to carry out the transition sealing step between the transitional glass of 3.3 high-boron-silicon glass and 4J29 kovar alloy, obtained extraordinary technique effect, can be widely used in sun power, chemical industry, medical packaging, electric light source, industries such as artwork Ornament have important economic benefit and social benefit.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment only is used for explanation the present invention and is not used in and limits the scope of the invention, after having read the present invention, those skilled in the art all fall within the application's claims institute restricted portion to the modification of the various equivalent form of values of the present invention.
Embodiment 1
A kind of high borosilicate hard glass and the direct matched seal method of kovar alloy, it may further comprise the steps:
(1) get the kovar alloy that the coefficient of expansion is 3.0 * 10-6/K, carry out the surface sand-blasting texturing earlier and handle, the kovar alloy that sandblast texturing was handled places hydrogen-burning stove to burn the wet hydrogen processing then;
(2) kovar alloy and the high-boron-silicon glass of getting the processing of step (1) burning wet hydrogen carries out sealing-in under 1200 ℃ of conditions of high temperature;
The coefficient of expansion of the present invention is that the kovar alloy of 3.0 * 10-6/K is become to be grouped into by following weight percent:
Ni 32%, and Co 15%, and Mn 0.5%, and Si 0.2%, and Cr 0.2%, and Cu 0.2%, and Mo 0.2%, and S 0.025%, P0.025%, and C 0.06%, remains to be Fe;
(3) get the good kovar alloy of step (2) sealing-in and high-boron-silicon glass and under 1000 ℃~1100 ℃ conditions, carry out anneal.
Above-described high borosilicate hard glass and the direct matched seal method of kovar alloy, the temperature that the described burning wet hydrogen of step (1) is handled is 1050 ℃, the annealing in hydrogen atmosphere time is 60 minutes.
Above-described high borosilicate hard glass and the direct matched seal method of kovar alloy, the sealing-in mode of step (2) are that kovar alloy is inserted into and carries out sealing-in in the high-boron-silicon glass.
Embodiment 2
A kind of high borosilicate hard glass and the direct matched seal method of kovar alloy, it may further comprise the steps:
(1) get the kovar alloy that the coefficient of expansion is 3.0 * 10-6/K, carry out the surface sand-blasting texturing earlier and handle, the kovar alloy that sandblast texturing was handled places hydrogen-burning stove to carry out the annealing in hydrogen atmosphere processing then;
(2) kovar alloy and the high-boron-silicon glass of getting the processing of step (1) annealing in hydrogen atmosphere carries out sealing-in under 1300 ℃ of conditions of high temperature;
The coefficient of expansion of the present invention is that the kovar alloy of 3.0 * 10-6/K is become to be grouped into by following weight percent: Ni 27%, and Co 11%, and Mn 0.3%, and Si 0.05%, Cr 0.05%, and Cu 0.15%, and Mo 0.15%, and S 0.001%, P0.001%, C 0.05%, remains to be Fe;
(3) get the good kovar alloy of step (2) sealing-in and high-boron-silicon glass and under 1000 ℃~1100 ℃ conditions, carry out anneal.
Above-described high borosilicate hard glass and the direct matched seal method of kovar alloy, the temperature that the described burning wet hydrogen of step (1) is handled is 1050 ℃, the annealing in hydrogen atmosphere time is 60 minutes.
Above-described high borosilicate hard glass and the direct matched seal method of kovar alloy, the sealing-in mode of step (2) are that kovar alloy docks with high-boron-silicon glass and carries out sealing-in.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (4)

1. one kind high borosilicate hard glass and the direct matched seal method of kovar alloy is characterized in that it may further comprise the steps:
(1) getting the coefficient of expansion is 3.0 * 10 -6The kovar alloy of/K carries out the surface sand-blasting texturing earlier and handles, and the kovar alloy that sandblast texturing was handled places hydrogen-burning stove to burn the wet hydrogen processing then;
(2) kovar alloy and the high-boron-silicon glass of getting the processing of step (1) burning wet hydrogen carries out sealing-in under 1200 ℃~1300 ℃ hot conditionss;
The described coefficient of expansion is 3.0 * 10 -6The kovar alloy of/K is become to be grouped into by following weight percent:
Ni 27%~32%, and Co 11%~15%, and Mn 0.3%~0.5%, and Si 0%~0.2%, and Cr 0%~0.2%, and Cu 0.15%~0.2%, and Mo 0.15%~0.2%, and S 0% ~ 0.025%, and P 0% ~ 0.025%, and C 0.05% ~ 0.06%, remains to be Fe;
(3) get the good kovar alloy of step (2) sealing-in and high-boron-silicon glass and under 1000 ℃~1100 ℃ conditions, carry out anneal.
2. high borosilicate hard glass according to claim 1 and the direct matched seal method of kovar alloy is characterized in that, the described coefficient of expansion of step (2) is 3.0 * 10 -6The kovar alloy of/K is become to be grouped into by following weight percent:
Ni 27%~32%, and Co 11%~15%, and Mn 0.3%~0.5%, and Si 0.05%~0.2%, and Cr 0.05%~0.2%, and Cu 0.15%~0.2%, and Mo 0.15%~0.2%, and S 0.001% ~ 0.025%, P0.001% ~ 0.025%, and C 0.05% ~ 0.06%, remains to be Fe.
3. high borosilicate hard glass according to claim 1 and the direct matched seal method of kovar alloy is characterized in that, the temperature that the described burning wet hydrogen of step (1) is handled is 1050 ℃, and burning the wet hydrogen time is 60 minutes.
4. high borosilicate hard glass according to claim 1 and the direct matched seal method of kovar alloy, it is characterized in that the sealing-in mode of step (2) is that kovar alloy is inserted into and carries out sealing-in or kovar alloy in the high-boron-silicon glass and dock with high-boron-silicon glass and carry out sealing-in.
CN201310241615.9A 2013-06-19 2013-06-19 High borosilicate hard glass and the direct matched seal method of kovar alloy Expired - Fee Related CN103332872B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104788024A (en) * 2015-03-10 2015-07-22 北京工业大学 Method for improving metal surface wettability by high energy beam texturing
CN107628759A (en) * 2017-10-25 2018-01-26 上海容东激光科技有限公司 A kind of burn-back technique of kovar alloy and hard glass
CN109746455A (en) * 2019-03-19 2019-05-14 湖南恒基粉末科技有限责任公司 A kind of cupric kovar alloy and preparation method thereof
CN110950549A (en) * 2019-12-31 2020-04-03 西安赛尔电子材料科技有限公司 Kovar alloy-glass sealing process for energy storage welding
CN114043029A (en) * 2021-11-05 2022-02-15 天津航空机电有限公司 Brazing method for welding molybdenum alloy and kovar alloy by using copper-platinum solder

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1040395A (en) * 1988-08-18 1990-03-14 陕西钢铁研究所 Siliconized fernico
EP0683502A1 (en) * 1994-05-16 1995-11-22 Yusuke Shida Method of producing frit-sealed x-ray tube
CN102515522A (en) * 2011-12-08 2012-06-27 山东力诺新材料有限公司 Borosilicate glass, glass-metal coupled sealing connection member, and preparation method and use of the glass-metal coupled sealing connection member

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1040395A (en) * 1988-08-18 1990-03-14 陕西钢铁研究所 Siliconized fernico
EP0683502A1 (en) * 1994-05-16 1995-11-22 Yusuke Shida Method of producing frit-sealed x-ray tube
CN102515522A (en) * 2011-12-08 2012-06-27 山东力诺新材料有限公司 Borosilicate glass, glass-metal coupled sealing connection member, and preparation method and use of the glass-metal coupled sealing connection member

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104788024A (en) * 2015-03-10 2015-07-22 北京工业大学 Method for improving metal surface wettability by high energy beam texturing
CN107628759A (en) * 2017-10-25 2018-01-26 上海容东激光科技有限公司 A kind of burn-back technique of kovar alloy and hard glass
CN109746455A (en) * 2019-03-19 2019-05-14 湖南恒基粉末科技有限责任公司 A kind of cupric kovar alloy and preparation method thereof
CN110950549A (en) * 2019-12-31 2020-04-03 西安赛尔电子材料科技有限公司 Kovar alloy-glass sealing process for energy storage welding
CN114043029A (en) * 2021-11-05 2022-02-15 天津航空机电有限公司 Brazing method for welding molybdenum alloy and kovar alloy by using copper-platinum solder

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