CN1398805A - Glass ceramics for insulating electronic device - Google Patents

Glass ceramics for insulating electronic device Download PDF

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Publication number
CN1398805A
CN1398805A CN 01108662 CN01108662A CN1398805A CN 1398805 A CN1398805 A CN 1398805A CN 01108662 CN01108662 CN 01108662 CN 01108662 A CN01108662 A CN 01108662A CN 1398805 A CN1398805 A CN 1398805A
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China
Prior art keywords
glass
electronic device
devitrified glass
strength
insulating
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CN 01108662
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Chinese (zh)
Inventor
黄宗家
陈军平
倪世龙
陈晓林
郑超
方超
欧阳彬
王学斌
黄艳
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CHENGDU XUGUANG ELECTRONICS Co Ltd
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CHENGDU XUGUANG ELECTRONICS Co Ltd
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Priority to CN 01108662 priority Critical patent/CN1398805A/en
Publication of CN1398805A publication Critical patent/CN1398805A/en
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0018—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents
    • C03C10/0027—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents containing SiO2, Al2O3, Li2O as main constituents
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0054—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing PbO, SnO2, B2O3

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

The present invention is a glass ceramics for insulating electronic device and relates to the insulating material for electronic device. The glass ceramic consists of Li2O 8.0-20.0 wt%, Al2O3 4.0-8.0 wt%, SiO2 64.0-78.0 wt%, K2O 0.5-4.5 wt%, B2O3 1.0-5.0 wt% and P2O5 0.5-4.0 wt%, and is prepared through mixing the said components, smelting and then molding at 1350-1500 deg.c, nucleation at 460-660 deg.C for 0.5-12 hr, crystallization at 660-880 deg.C for 0.5-24 hr, and cooling. It has flexural strength of 240-400 MPa, puncture strength of 23-30 KV/mm, expansion coefficient (90-120)E(-7)/deg.C. It is especially suitable for use in producing insulating part for electronic device and also is especially suitable for matching with Fe-Ni alloy, Fe-Cr alloy, Fe-Ni-Cr alloy, etc. in encapsulation.

Description

Glass ceramics for insulating electronic device
Technical field
The present invention relates to insulating material, especially for the devitrified glass of making insulating electronic device, insulated shell.
Background technology
Existing glass ceramics for insulating such as lithium are photosensitive glass-ceramics.Its component has Li 2O, Al 2O 3, SiO 2, K 2O, Ag, Cu or Au.By found, moulding, uviolizing, nucleus crystallization handle, obtaining the coefficient of expansion is 100 * 10 -7/ ℃, folding strength is about the devitrified glass of 200Mpa.Its performance sees Table one.There are the following problems for this devitrified glass, and the first, intensity is lower, can only make the not high insulating parts such as insulated substrate of antagonism folding requirement of strength, and discomfort is fit to do insulating parts such as the higher insulator of antagonism folding requirement of strength, large-scale insulated shell; The second, lower with the resistance to air loss and the intensity of metal sealing, be not suitable for making to sealing-in resistance to air loss and the high insulating electronic device spare of requirement of strength.
Summary of the invention
Given this, the object of the present invention is to provide a kind of insulating electronic device usefulness, folding strength height, with the resistance to air loss and the high devitrified glass of intensity of metal sealing.
The present invention adopts on the basis of existing devitrified glass, adds B in prescription 2O 3, with the nucleus agent P in the prescription 2O 5Replace Ag, Cu or Au, adjust the each component dosage, adopt found, moulding, coring processing, crystallization handle manufacturing process and realize its purpose.
Glass ceramics for insulating electronic device of the present invention, the following component that has weight part to measure: Li 2O8.0～20.0, Al 2O 34.0～8.0, SiO 264.0～78.0, K 2O 0.5～4.5, B 2O 31.0～5.0, P 2O 50.5～4.0, above-mentioned each component is mixed, found moulding through 1350～1500 ℃; Handled 0.5～12 hour through 460～660 ℃ of coring again, be warming up to 660～880 ℃ of crystallization then and handled 0.5～24 hour, obtain folding strength 240～400Mpa after the cooling, anti-electric breakdown strength is that 23～30kv/mm, the coefficient of expansion are 90 * 10 -7～120 * 10 -7/ ℃ devitrified glass.
Li preferably in the above-mentioned prescription 2O 10.0～16.0, Al 2O 34.0～7.0, SiO 268.0～76.0, K 2O 1.0～4.0, B 2O 31.0～4.0, P 2O 51.0～3.0.
In the above-mentioned prescription As can be arranged 2O 3, Sb 2O 3Deng glass industry finings commonly used.
Above-mentioned Li 2O is a major ingredient, with SiO 2Form the lithium silicate crystal, improve the folding strength of devitrified glass.When content was low, the glass smelting temperature drift can only generate a small amount of silicic acid crystalline lithium, is difficult to obtain the devitrified glass of high breaking strength; When content improved, the devitrified glass refractoriness reduced, and electron device heat resistance in process of production reduces.
Above-mentioned Al 2O 3Be mainly used in the coefficient of expansion of adjusting devitrified glass.When content reduced, the coefficient of expansion of devitrified glass improved; When content increased, the coefficient of expansion of devitrified glass reduced.
Above-mentioned SiO 2Be major ingredient.Such as 66 weight parts, the refractoriness and the coefficient of expansion of devitrified glass were on the low side when content was low; When content is higher, be easy to generate silica crystals in the devitrified glass, cause the folding strength of devitrified glass to reduce; When content was moderate, the folding strength of devitrified glass improved, and when the 74 weight part left and right sides, the folding strength of devitrified glass is more than 280Mpa such as content.
Above-mentioned K 2The effect one of O is the folding strength that improves devitrified glass, the 2nd, reduce glass melting temperature.When content was higher, the refractoriness of devitrified glass, chemical stability and anti-electric breakdown strength reduced; Content is lower, and the intensity of devitrified glass is lower.
Above-mentioned B 2O 3Main effect one be by introducing B 2O 3Reduce SiO 2Content prevents to generate in the devitrified glass silica crystals, improves the folding strength of devitrified glass with this, reduces SiO if introduce other 2The component of consumption can cause the deterioration of devitrified glass performance; The 2nd, B 2O 3Can with the oxide compound NiO or the Cr of sealing-in metal 2O 3Chemical reaction takes place, thereby improves the resistance to air loss and the intensity of devitrified glass and metal sealing.B 2O 3Content when higher, the refractoriness of devitrified glass reduces; B 2O 3When content was low, the folding strength of devitrified glass was lower and relatively poor with the resistance to air loss and the intensity of metal sealing.
Above-mentioned P 2O 5Play the nucleus agent.P 2O 5When content was higher, the crystallization velocity of glass was too fast, is unfavorable for forming operation, was difficult to obtain the high strength micro-crystalline glass of even fine crystalline structure; P 2O 5When content is low, when coring and crystallization and thermal treatment, can only obtain small number of coarse crystalline devitrified glass, be difficult to obtain many and little, equally distributed high-intensity devitrified glass.
Above-mentioned As 2O 3Or Sb 2O 3Be the finings of glass smelting, general add-on is 0.3～0.8 just can reach clarifying effect preferably.
When adopting above-mentioned prescription to make devitrified glass, earlier each component is mixed, adopts the melting technology of traditional glass, in 1350～1500 ℃ in glass-melting furnace such as crucible oven or tank furnace, found into glass with electrically heated or flame heating.The moulding process that adopts traditional glass then is as centrifugal casting, cast, and compacting or blowing etc. are above-mentioned glass ware forming.At last formed glass being carried out coring at 460～660 ℃ handled 0.5～12 hour, then be warmed up to 660～880 ℃ and carry out crystallization processing 0.5～24 hour, after the cooling, obtaining folding strength is that 240～400MPa, anti-electric breakdown strength are that 23～30kv/mm, the coefficient of expansion are 90 * 10 -7～120 * 10 -7/ ℃ devitrified glass.
Devitrified glass of the present invention and existing electrically insulating material lithium are that the performance of photosensitive glass-ceramics, electric-vacuum glass (DM-308), electrovacuum ceramics (95% alumina-ceramic is called for short ' 95 ' porcelain) relatively sees Table one:
Table one
Performance Lithium is a photosensitive glass-ceramics Glass (DM-308) ' 95 ' porcelain Devitrified glass of the present invention
Shock strength (N.m) ????0.3～0.6 ????0.05～0.1 ????0.25 ????0.3～0.75
Linear expansivity (10 -7/℃)(20～500℃) ????110 ????49 ????70 ????90～120
Folding strength (MPa) ????200 ????60～70 ????272 ????240～400
Working temperature (℃) ????850 ????450 ????1500 ????850
Performance Lithium is a photosensitive glass-ceramics Glass (DM-308) ' 95 ' porcelain Devitrified glass of the present invention
Anti-electric breakdown strength (kV/mm) ????23～30 ????20～25 ????15 ????23～30
Edge flashing strength of electric field (kV/cm) in the air ????6 ????5 8 (glaze layers 5～6) ????6
Surface resistivity (Ω/m2) ????10 +14～+16 ????10 +12 ????10 +14 ????10 +14～+16
Mohs' hardness ????6～7 ????6 ????9 ????6～7
Devitrified glass of the present invention and lithium are that photosensitive glass-ceramics, electric-vacuum glass (DM-308), electrovacuum ceramics (' 95 ' porcelain) are compared, and have following advantage:
One, devitrified glass of the present invention can be done the resistance to air loss matched seal with iron-nickel alloy (4J50), ferrochrome exothermic (4J28), iron-nickel-chromium cheap metals such as (4J49).
Two, devitrified glass of the present invention is that photosensitive glass-ceramics is compared with lithium, and the folding strength height is with the resistance to air loss and the intensity height of metal sealing.
Three, devitrified glass of the present invention is compared with electric-vacuum glass, its folding strength, shock strength, anti-electric breakdown strength and refractoriness height, and with the intensity height of metal sealing.
Four, devitrified glass of the present invention is compared with electrovacuum ceramics, pore-free, anti-electric breakdown strength, folding strength and excellent in cushion effect; Smooth surface need not glazing, and production cycle and flow process are short, and waste product is few; Good with the resistance to air loss of metal sealing.
Devitrified glass of the present invention is specially adapted to make insulating parts such as electron tube insulated shell.And be particularly suitable for using with iron-nickel alloy (4J50), ferrochrome exothermic (4J28), iron-nickel-chromium metals such as (4J49) and do matched seal.
Embodiment
Below, with embodiment the present invention is further described again.
The component of embodiments of the invention 1～8, processing parameter, performance perameter such as table two are listed.
Table two
Component, technical parameter Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Embodiment 7 Embodiment 8
?Li 2O (weight part) ????12.2 ???12.6 ???13.0 ????14.0 ????15.0 ????16.0 ????12.5 ????12.5
?Al 2O 3(weight part) ????4.0 ???4.0 ???4.0 ????4.5 ????4.5 ????5.0 ????5.0 ????6.0
?SiO 2(weight part) ????78.0 ???76.8 ???77.4 ????75.4 ????74.0 ????72.0 ????72.5 ????71.5
?K 2O (weight part) ????2.0 ???3.0 ???2.2 ????1.8 ????2.0 ????2.0 ????4.0 ????4.0
?B 2O 3(weight part) ????2.0 ???1.8 ???2.0 ????2.5 ????2.5 ????3.0 ????3.0 ????3.0
?P 2O 5(weight part) ????1.8 ???1.8 ???1.8 ????1.8 ????2.0 ????2.0 ????3.0 ????3.0
?Sb 2O 3(weight part) ????0.3 ????0.3
?As 2O 3(weight part) ????0.5 ???0.5 ???0.5 ????0.5 ????0.5 ????0.5
Add up to (weight part) ????100.5 ???100.5 ???100.5 ????100.5 ????100.5 ????100.5 ????100.3 ????100.3
Glass melting temperature (℃) ????1500 ???1460 ???1440 ????1420 ????1400 ????1380 ????1420 ????1420
Nucleation temperature (℃) ????560 ????540 ????530 ????520 ????520 ????520 ????560 ????580
Nucleation time (h) ????4.0 ????2.0 ????2.0 ????2.0 ????2.0 ????2.0 ????1.0 ????1.0
Crystallization temperature (℃) ????860 ????840 ????820 ????800 ????800 ????780 ????840 ????840
Crystallization time (h) ????4.0 ????4.0 ????2.0 ????2.0 ????2.0 ????2.0 ????1.0 ????1.0
The coefficient of expansion (10 -7/℃) ??(20～500℃) ????120 ????110 ????110 ????105 ????100 ????100 ????100 ????90
The manufacturing process program of above-mentioned each example of the present invention is basic identical, and just processing parameter is selected slightly different.Illustrated with embodiment 1 and embodiment 4.
The manufacturing process of embodiment 1: Ji Liang component is by weight: Li 2O 12.2, Al 2O 34.0, SiO 278.0, K 2O 2.0, B 2O 32.0, P 2O 51.8, As 2O 30.5; To join in the crucible behind the each component uniform mixing, in electric furnace, founded 6 hours for 1500 ℃, then the glass casting that melts is gone in the previously prepd glass mold, obtain glasswork; Then this glasswork is put into retort furnace, be raised to 560 ℃ of insulations with 4～8 ℃/minute heat-up rates and carried out the coring processing in 4.0 hours, then be raised to 860 ℃ of insulations with 2～3 ℃/minute heat-up rate again and carried out crystallization in 4.0 hours and handle, be cooled to room temperature, obtaining the coefficient of expansion is 120 * 10 -7/ ℃ crystallized glass article.
The manufacturing process of embodiment 4: Ji Liang component is by weight: Li 2O 14.0, Al 2O 34.5, SiO 275.4, K 2O 1.8, B 2O 32.5, P 2O 51.8, As 2O 30.5; To join in the crucible behind the each component uniform mixing, in electric furnace, founded 6 hours for 1420 ℃, then the glass casting that melts is gone in the previously prepd glass mold, obtain glasswork, then this glasswork is put into retort furnace, be raised to 520 ℃ of insulations with 3～6 ℃/minute heat-up rates and carried out coring in 2 hours and handle, then be raised to 800 ℃ of insulations with 1～3 ℃/minute heat-up rate again and carried out crystallization in 2.0 hours and handle, be cooled to room temperature, obtaining the coefficient of expansion is 105 * 10 -7/ ℃ crystallized glass article.

Claims (2)

1, glass ceramics for insulating electronic device is characterized in that having the following component of metering: Li by weight 2O8.0～20.0, Al 2O 34.0～8.0, SiO 264.0～78.0, K 2O 0.5～4.5, B 2O 31.0～5.0, P 2O 50.5～4.0, above-mentioned each component is mixed, found moulding through 1350～1500 ℃; Handled 0.5～12 hour through 460～660 ℃ of coring again, be warming up to 660～880 ℃ of crystallization then and handled 0.5～24 hour, obtain folding strength 240～400Mpa after the cooling, anti-electric breakdown strength is that 23～30kv/mm, the coefficient of expansion are 90 * 10 -7～120 * 10 -7/ ℃ devitrified glass.
2, glass ceramics for insulating electronic device according to claim 1 is characterized in that Li wherein 2O10.0～16.0, Al 2O 34.0～7.0, SiO 268.0～76.0, K 2O 1.0～4.0, B 2O 31.0～4.0, P 2O 51.0～3.0.
CN 01108662 2001-07-24 2001-07-24 Glass ceramics for insulating electronic device Pending CN1398805A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1944304B (en) * 2006-11-09 2010-09-01 北京科技大学 Sealing micro crystal glass and its sealing method
CN101152973B (en) * 2006-09-28 2010-09-22 中南大学 Crystallizing glass material for 4J29 kovar alloy sealing-in and method of producing the same
CN102060440A (en) * 2010-11-30 2011-05-18 法库县矿产资源研究发展中心 High-pressure-resistant sealing glass ceramic and use thereof
CN105742056A (en) * 2016-01-29 2016-07-06 桂林电子科技大学 High-energy borophosphate microcrystalline glass dielectric material and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101152973B (en) * 2006-09-28 2010-09-22 中南大学 Crystallizing glass material for 4J29 kovar alloy sealing-in and method of producing the same
CN1944304B (en) * 2006-11-09 2010-09-01 北京科技大学 Sealing micro crystal glass and its sealing method
CN102060440A (en) * 2010-11-30 2011-05-18 法库县矿产资源研究发展中心 High-pressure-resistant sealing glass ceramic and use thereof
CN102060440B (en) * 2010-11-30 2012-12-26 法库县矿产资源研究发展中心 High-pressure-resistant sealing microcrystalline glass and use thereof
CN105742056A (en) * 2016-01-29 2016-07-06 桂林电子科技大学 High-energy borophosphate microcrystalline glass dielectric material and preparation method thereof

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