WO2023026771A1 - ガラス組成物及び封着材料 - Google Patents
ガラス組成物及び封着材料 Download PDFInfo
- Publication number
- WO2023026771A1 WO2023026771A1 PCT/JP2022/029329 JP2022029329W WO2023026771A1 WO 2023026771 A1 WO2023026771 A1 WO 2023026771A1 JP 2022029329 W JP2022029329 W JP 2022029329W WO 2023026771 A1 WO2023026771 A1 WO 2023026771A1
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- Prior art keywords
- glass
- content
- sealing material
- glass composition
- tends
- Prior art date
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- 239000011521 glass Substances 0.000 title claims abstract description 148
- 239000003566 sealing material Substances 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title description 2
- 239000000203 mixture Substances 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims description 51
- 239000000945 filler Substances 0.000 claims description 28
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 12
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 abstract description 8
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 abstract description 3
- 229910003069 TeO2 Inorganic materials 0.000 abstract 1
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 abstract 1
- 238000007789 sealing Methods 0.000 description 38
- 238000010304 firing Methods 0.000 description 22
- 238000004017 vitrification Methods 0.000 description 20
- 238000002844 melting Methods 0.000 description 19
- 230000008018 melting Effects 0.000 description 19
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 238000005259 measurement Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- -1 flat display devices Substances 0.000 description 3
- ZPPSOOVFTBGHBI-UHFFFAOYSA-N lead(2+);oxido(oxo)borane Chemical compound [Pb+2].[O-]B=O.[O-]B=O ZPPSOOVFTBGHBI-UHFFFAOYSA-N 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910018162 SeO2 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000005385 borate glass Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000004031 devitrification Methods 0.000 description 2
- 238000004455 differential thermal analysis Methods 0.000 description 2
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000006060 molten glass Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- JPJALAQPGMAKDF-UHFFFAOYSA-N selenium dioxide Chemical compound O=[Se]=O JPJALAQPGMAKDF-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- CYSGHNMQYZDMIA-UHFFFAOYSA-N 1,3-Dimethyl-2-imidazolidinon Chemical compound CN1CCN(C)C1=O CYSGHNMQYZDMIA-UHFFFAOYSA-N 0.000 description 1
- BUUSNVSJZVGMFY-UHFFFAOYSA-N 4-ethylheptane-3,3-diol Chemical compound CCCC(CC)C(O)(O)CC BUUSNVSJZVGMFY-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 1
- 229910020203 CeO Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 239000002202 Polyethylene glycol Chemical class 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 125000005396 acrylic acid ester group Chemical group 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910000174 eucryptite Inorganic materials 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229940117955 isoamyl acetate Drugs 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001223 polyethylene glycol Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052844 willemite Inorganic materials 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
- 229910000500 β-quartz Inorganic materials 0.000 description 1
- 229910052644 β-spodumene Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
-
- 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
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/14—Silica-free oxide glass compositions containing boron
-
- 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
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/14—Silica-free oxide glass compositions containing boron
- C03C3/145—Silica-free oxide glass compositions containing boron containing aluminium or beryllium
-
- 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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
-
- 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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
-
- G—PHYSICS
- G04—HOROLOGY
- G04G—ELECTRONIC TIME-PIECES
- G04G3/00—Producing timing pulses
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/02—Containers; Seals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/02—Containers; Seals
- H01L23/10—Containers; Seals characterised by the material or arrangement of seals between parts, e.g. between cap and base of the container or between leads and walls of the container
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/31—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the arrangement or shape
-
- H—ELECTRICITY
- H03—ELECTRONIC CIRCUITRY
- H03H—IMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
- H03H9/00—Networks comprising electromechanical or electro-acoustic devices; Electromechanical resonators
- H03H9/02—Details
Definitions
- the present invention relates to a glass composition and a sealing material that are weather resistant and hermetically sealed at low temperatures.
- Sealing materials are used for semiconductor integrated circuits, crystal oscillators, metal members, vacuum insulated glass, flat display devices, and glass terminals for LEDs. Since the sealing material is required to have chemical durability and heat resistance, a glass-based sealing material is used instead of a resin-based adhesive. Sealing materials are further required to have properties such as mechanical strength, fluidity, and weather resistance. In particular, it is required to reduce the sealing temperature as much as possible for the sealing of electronic components on which heat-sensitive elements are mounted. Specifically, it is required that sealing can be performed at a temperature of 400° C. or lower. As a glass that satisfies this property, lead-borate glass containing a large amount of PbO, which has a great effect of lowering the softening point, has been widely used (see, for example, Patent Document 1).
- an object of the present invention is to provide a glass composition and a sealing material that have good weather resistance and can be sealed at low temperatures.
- the glass composition of the present invention contains 0.3 to 25% CuO, 1 to 30% Li 2 O + Na 2 O + K 2 O, 1 to 30% MgO + CaO + SrO + BaO + ZnO, and substantially contains SeO 2 in terms of mol%. preferably not. "Substantially free of SeO2 " means that the content of SeO2 is less than 0.1 mol%.
- the glass composition of the present invention preferably has a ZnO content of 0 to 25 mol%.
- the glass composition of the present invention preferably has a Nb 2 O 5 content of 0 to 10 mol %.
- the glass composition of the present invention has a glass composition of 0 to 10% Fe 2 O 3 , 0 to 10% Al 2 O 3 , 0 to 20% B 2 O 3 , and 0 to 20% WO 3 in terms of mol %. It is preferable to contain
- the sealing material of the present invention preferably contains 40 to 100% by volume of glass powder composed of the above glass composition and 0 to 60% by volume of refractory filler powder.
- the refractory filler powder is preferably substantially spherical.
- the term “substantially spherical” is not limited to a true sphere.
- the value obtained by dividing the shortest diameter passing through the center of gravity of the refractory filler powder by the longest diameter is 0.5. 0.7 or more, preferably 0.7 or more.
- all or part of the refractory filler powder is preferably Zr 2 WO 4 (PO 4 ) 2 .
- the sealing material of the present invention is preferably used for crystal oscillator packages.
- the sealing material of the present invention is preferably used for vacuum insulating glass.
- the sealing material paste of the present invention preferably contains the above sealing material and vehicle.
- the present invention can provide a glass composition and a sealing material that can be sealed at a low temperature while having good weather resistance.
- the glass composition of the present invention has a glass composition of 15 to 80% TeO 2 , 0.1 to 30% MoO 3 +Ag 2 O, 5 to 40% V 2 O 5 and 0.1 to 35 CuO as a glass composition. %, PbO 0-10%.
- the reasons for limiting the glass composition range as described above are as follows. In the description of the content of each component, "%” means “mol %” unless otherwise specified.
- TeO 2 is a component that forms a glass network and enhances weather resistance.
- the content of TeO 2 is 15-80%, preferably 20-70%, especially 25-65%. If the TeO 2 content is too low, the glass becomes thermally unstable and tends to devitrify during melting or firing. On the other hand, if the content of TeO 2 is too high, the viscosity (softening point, etc.) of the glass increases, making low-temperature sealing difficult and the coefficient of thermal expansion tends to increase too much.
- MoO 3 and Ag 2 O are components that form a glass network and lower the viscosity (softening point, etc.) of the glass while maintaining the weather resistance of the glass.
- the content of MoO 3 +Ag 2 O is 0.1-30%, 1-29%, 3-28%, 5-28%, 7-27%, 10-25%, 12-22%, especially 15 ⁇ 20% is preferred. If the content of MoO 3 +Ag 2 O is too small, vitrification becomes difficult and the viscosity (softening point, etc.) of the glass increases, making low-temperature sealing difficult. On the other hand, if the content of MoO 3 +Ag 2 O is too high, the glass becomes thermally unstable, the glass tends to devitrify during melting or firing, and the coefficient of thermal expansion tends to become too high.
- the content of MoO3 is 0-30%, 0.1-29%, 1-29%, 5-28%, 7-27%, 10-25%, 12-22%, especially 15-20%. Preferably.
- the content of Ag 2 O is 0-30%, 0.1-29%, 1-29%, 5-28%, 7-27%, 10-25%, 12-22%, especially 15-20% is preferably
- V 2 O 5 is a component that forms a glass network and lowers the viscosity (softening point, etc.) of glass. It is also a component that lowers the coefficient of thermal expansion.
- the content of V 2 O 5 is 5-40%, preferably 7-35%, 8-30%, 10-25%, especially 12-20%. If the V 2 O 5 content is too small, vitrification becomes difficult and the viscosity (softening point, etc.) of the glass increases, making low-temperature sealing difficult. Also, the coefficient of thermal expansion tends to be too high. On the other hand, if the content of V 2 O 5 is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing.
- CuO is a component that lowers the viscosity (softening point, etc.) of glass and lowers the coefficient of thermal expansion. It is also a component that enhances the adhesive strength between glass and metal when sealing metal. Although the mechanism for increasing the adhesive strength is currently unknown in detail, since Cu atoms are highly diffusible, it is believed that the diffusion of Cu atoms from the surface layer of the metal toward the inside facilitates the integration of the glass and the metal. Conceivable. There are no particular restrictions on the type of metal to be sealed, but examples include iron, iron alloys, nickel, nickel alloys, copper, copper alloys, aluminum, and aluminum alloys.
- the content of CuO is 0.1-35%, 0.2-30%, 0.3-25%, 0.4-20%, 0.5-15%, 1-12%, especially 3 ⁇ 11% is preferred. If the CuO content is too low, vitrification becomes difficult and the viscosity (softening point, etc.) of the glass increases, making low-temperature sealing difficult. Also, the coefficient of thermal expansion tends to be too high. If the CuO content is too high, the glass becomes thermally unstable, and metal Cu may precipitate from the glass surface in the sealing process, which may adversely affect the sealing strength and electrical properties. Also, the glass tends to devitrify during melting or firing.
- PbO is a component that lowers the viscosity (softening point, etc.) of glass. 1%, preferably substantially no (less than 0.1%).
- Li 2 O, Na 2 O and K 2 O are components that lower the viscosity (softening point, etc.) of glass.
- the content of Li 2 O+Na 2 O+K 2 O is preferably 0-30%, 1-30%, 5-25%, especially 10-20%. If the content of Li 2 O+Na 2 O+K 2 O is too small, the viscosity (softening point, etc.) of the glass increases, which may make sealing at low temperatures difficult. Moreover, vitrification may become difficult. On the other hand, if the content of Li 2 O+Na 2 O+K 2 O is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing. Moreover, the weather resistance tends to deteriorate, and the coefficient of thermal expansion tends to become too high.
- Li 2 O is a component that significantly lowers the viscosity (softening point, etc.) of glass compared to Na 2 O and K 2 O.
- the content of Li 2 O is preferably 0-30%, 1-20%, 3-15%, especially 5-13%. If the content of Li 2 O is too small, the viscosity (softening point, etc.) of the glass increases, which may make sealing at low temperatures difficult. Moreover, vitrification may become difficult. On the other hand, if the content of Li 2 O is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing. Moreover, the weather resistance tends to deteriorate, and the coefficient of thermal expansion tends to become too high.
- K 2 O is a component that is more effective than Na 2 O in lowering the viscosity (softening point, etc.) of glass.
- the content of K 2 O is preferably 0-30%, 1-20%, 3-15%, especially 5-13%. If the content of K 2 O is too small, the viscosity (softening point, etc.) of the glass increases, and sealing at low temperatures may become difficult. Moreover, vitrification may become difficult. On the other hand, if the K 2 O content is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing. Moreover, the weather resistance tends to deteriorate, and the coefficient of thermal expansion tends to become too high.
- Na 2 O is a component that lowers the viscosity (softening point, etc.) of glass.
- the content of Na 2 O is preferably 0-30%, 0.1-20%, 1-15%, especially 3-13%. If the content of Na 2 O is too small, the viscosity (softening point, etc.) of the glass increases, which may make sealing at low temperatures difficult. Moreover, vitrification may become difficult. On the other hand, if the content of Na 2 O is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing. Moreover, the weather resistance tends to deteriorate, and the coefficient of thermal expansion tends to become too high.
- the molar ratio Li 2 O/K 2 O is 0.3 to 5, 0.4 to 4, 0.5 to 3, 0.6 to 2, especially 0.3 to 5, 0.4 to 4, 0.5 to 3, 0.6 to 2, in order to lower the softening point due to the alkali mixing effect. It is preferably between 7 and 1.5.
- Li2O / K2O refers to the value obtained by dividing the content of Li2O by the content of K2O .
- the molar ratio Na 2 O/K 2 O is 0.3 to 5, 0.4 to 4, 0.5 to 3, 0.6 to 2, especially 0.3 to 5, 0.4 to 4, 0.5 to 3, 0.6 to 2, in order to lower the softening point due to the alkali mixing effect. It is preferably between 7 and 1.5. If the molar ratio Na 2 O/K 2 O is outside the above range, the glass becomes thermally unstable, and the glass tends to devitrify during melting or firing.
- Na2O / K2O refers to the value obtained by dividing the content of Na2O by the content of K2O .
- MgO, CaO, SrO, BaO and ZnO are components that widen the vitrification range and improve weather resistance.
- MgO+CaO+SrO+BaO+ZnO is preferably 0-30%, 1-30%, 3-20%, especially 5-15%. If the content of MgO+CaO+SrO+BaO+ZnO is too small, the viscosity (softening point, etc.) of the glass increases, which may make sealing at low temperatures difficult. Moreover, vitrification may become difficult. On the other hand, if the content of MgO+CaO+SrO+BaO+ZnO is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing. Moreover, the weather resistance tends to deteriorate, and the coefficient of thermal expansion tends to become too high.
- MgO is a component that expands the vitrification range and improves weather resistance.
- the content of MgO is preferably 0-25%, 0-20%, 0-10%, especially 1-7%. If the content of MgO is small, vitrification may become difficult. In addition, the viscosity (softening point, etc.) of the glass increases, which may make sealing at low temperatures difficult. On the other hand, if the content of MgO is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing. Moreover, the weather resistance tends to deteriorate, and the coefficient of thermal expansion tends to become too high.
- CaO is a component that expands the vitrification range and improves weather resistance.
- the content of CaO is preferably 0-25%, 0-20%, 0-10%, especially 1-7%.
- vitrification may become difficult.
- viscosity (softening point, etc.) of the glass increases, which may make sealing at low temperatures difficult.
- the content of CaO is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing.
- the weather resistance tends to deteriorate, and the coefficient of thermal expansion tends to become too high.
- SrO is a component that expands the vitrification range and improves weather resistance.
- the content of SrO is preferably 0-25%, 0-20%, 0-10%, particularly 1-7%.
- vitrification may become difficult.
- viscosity (softening point, etc.) of the glass increases, which may make sealing at low temperatures difficult.
- the content of SrO is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing.
- the weather resistance tends to deteriorate, and the coefficient of thermal expansion tends to become too high.
- BaO is a component that expands the vitrification range and improves weather resistance.
- the content of BaO is preferably 0-25%, 0.1-20%, 0.5-10%, especially 1-7%.
- vitrification may become difficult.
- viscosity (softening point, etc.) of the glass increases, which may make sealing at low temperatures difficult.
- the content of BaO is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing.
- the weather resistance tends to deteriorate, and the coefficient of thermal expansion tends to become too high.
- ZnO is a component that expands the vitrification range and improves weather resistance.
- the content of ZnO is preferably 0-25%, 0.1-22%, 1-20%, especially 2-15%. If the ZnO content is too low, vitrification becomes difficult. In addition, the viscosity (softening point, etc.) of the glass increases, making low-temperature sealing difficult. On the other hand, if the ZnO content is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing. Moreover, the weather resistance tends to deteriorate, and the coefficient of thermal expansion tends to become too high.
- AgI is a component that lowers the viscosity (softening point, etc.) of glass.
- the AgI content is preferably 0 to 3%, 0 to 2%, particularly 0 to 1%. If the AgI content is too high, the coefficient of thermal expansion tends to be too high.
- SeO 2 is a component that lowers the viscosity (softening point, etc.) of glass. 1%, preferably substantially no (less than 0.1%).
- Fe 2 O 3 is a component that enhances reactivity with the object to be sealed.
- the content of Fe 2 O 3 is preferably 0-10%, 0-8%, 0.1-10%, especially 1-7%. If the content of Fe 2 O 3 is too high, vitrification becomes difficult and the viscosity (softening point, etc.) of the glass increases, making low-temperature sealing difficult.
- Al 2 O 3 is a component that improves weather resistance.
- the content of Al 2 O 3 is preferably 0-10%, 0-8%, 0-6%, especially 0.1-5%. If the content of Al 2 O 3 is too high, the viscosity (softening point, etc.) of the glass increases, making low-temperature sealing difficult.
- B 2 O 3 is a component that forms a glass network.
- the content of B 2 O 3 is 0-20%, preferably 0-10%, especially 0.1-5%. If the content of B 2 O 3 is too high, the viscosity (softening point, etc.) of the glass increases, making low-temperature sealing difficult and the glass more likely to undergo phase separation. Moreover, it becomes difficult to vitrify.
- WO3 is a component that lowers the coefficient of thermal expansion.
- the content of WO 3 is preferably 0-20%, 0-10%, 0-5%, especially 0.1-3%. If the content of WO3 is too high, the glass becomes thermally unstable, the glass tends to devitrify during melting or firing, and the viscosity (softening point, etc.) of the glass increases, making low-temperature sealing difficult. become difficult.
- P 2 O 5 is a component that forms a glass network and thermally stabilizes the glass.
- the content of P 2 O 5 is preferably 0-10%, 0-5%, 0-2%, especially 0-1%. If the content of P 2 O 5 is too high, the viscosity (softening point, etc.) of the glass increases, making low-temperature sealing difficult and weather resistance more likely to decrease.
- Nb 2 O 5 is a component that thermally stabilizes glass and enhances weather resistance.
- the content of Nb 2 O 5 should be 0-10%, 0-5%, 0.1-4%, 0.5-3.5%, 1-3%, especially 1-2.5% is preferred. If the content of Nb 2 O 5 is too small, the glass becomes thermally unstable and tends to devitrify during melting or firing. On the other hand, if the content of Nb 2 O 5 is too high, the viscosity (softening point, etc.) of the glass increases, and low-temperature sealing tends to become difficult.
- La 2 O 3 is a component that thermally stabilizes glass and suppresses devitrification.
- the content of La 2 O 3 is preferably 0-10%, 0-5%, 0-2%, especially 0.1-1%. If the content of La 2 O 3 is too high, the viscosity (softening point, etc.) of the glass increases, and low-temperature sealing tends to become difficult.
- Ga 2 O 3 is a component that thermally stabilizes glass and enhances weather resistance, but is very expensive, so its content is preferably less than 0.01%.
- TiO 2 , GeO 2 , CeO 2 and Sb 2 O 3 are components for thermally stabilizing the glass and suppressing devitrification, and each can be added up to less than 5%. If the content of these elements is too high, the glass becomes thermally unstable and tends to devitrify during melting or firing.
- the sealing material of the present invention contains glass powder made from the above glass composition.
- the sealing material of the present invention may contain refractory filler powder in order to improve the mechanical strength or adjust the coefficient of thermal expansion.
- the mixing ratio is 40 to 100% by volume of glass powder, 0 to 60% by volume of refractory filler powder, 50 to 99% by volume of glass powder, 1 to 50% by volume of refractory filler powder, 60 to 95% by volume of glass powder, and refractory. 5 to 40% by volume of the refractory filler powder, particularly 70 to 90% by volume of the glass powder, and 10 to 30% by volume of the refractory filler powder. If the content of the refractory filler powder is too high, the proportion of the glass powder is relatively low, making it difficult to ensure desired fluidity.
- the refractory filler powder preferably contains Zr2WO4 ( PO4 ) 2 .
- Zr 2 WO 4 (PO 4 ) 2 hardly reacts with the glass powder according to the present invention, and further has the property of significantly lowering the thermal expansion coefficient of the sealing material.
- a refractory filler powder other than Zr 2 WO 4 (PO 4 ) 2 can be used as the refractory filler powder.
- Other refractory filler powders include NbZr( PO4 ) 3 , Zr2MoO4 ( PO4) 2 , Hf2WO4 ( PO4 ) 2 , Hf2MoO4 ( PO4 ) 2 , zirconium phosphate, Zircon, zirconia, tin oxide, aluminum titanate, quartz, ⁇ -spodumene, mullite, titania, quartz glass, ⁇ -eucryptite, ⁇ -quartz, willemite, cordierite, Sr 0.5 Zr 2 (PO 4 ) 3 and the like can be used alone or in combination of two or more.
- the refractory filler powder is preferably approximately spherical.
- the refractory filler powder is preferably approximately spherical.
- the fluidity of the glass powder is less likely to be hindered by the refractory filler powder, and as a result, the fluidity of the sealing material is improved.
- the stress in this part is dispersed because the refractory filler powder is substantially spherical. As a result, even if the object to be sealed comes into contact with the glaze layer during sealing, undue stress is less likely to be applied to the object to be sealed, making it easier to ensure airtightness.
- the average particle size D 50 of the refractory filler powder is preferably 0.2-20 ⁇ m, especially 2-15 ⁇ m. If the average particle diameter D50 is too large, the sealing layer tends to be thick. On the other hand, if the average particle diameter D50 is too small, the refractory filler powder is eluted into the glass during sealing, and the glass tends to devitrify.
- the sealing material of the present invention has a softening point of 360° C. or lower, 350° C. or lower, 340° C. or lower, 330° C. or lower, 320° C. or lower, 310° C. or lower, 300° C. or lower, 295° C. or lower, particularly 290° C. or lower. is preferred. If the softening point is too high, the viscosity of the glass increases, so that the sealing temperature rises and the element may be deteriorated by heat during sealing. Although the lower limit of the softening point is not particularly limited, it is practically 180° C. or higher.
- the “softening point” refers to a value measured with a macro-type differential thermal analysis device using a sealing material having an average particle diameter D50 of 0.5 to 20 ⁇ m as a measurement sample. As for the measurement conditions, the measurement is started at room temperature, and the temperature rise rate is 10° C./min.
- the softening point measured by the macro-type differential thermal analyzer refers to the temperature (Ts) at the fourth inflection point in the measurement curve shown in FIG.
- the thermal expansion coefficient in the temperature range of 30 to 150°C is preferably 20 ⁇ 10 -7 /°C to 200 ⁇ 10 -7 /°C, more preferably 30 ⁇ 10 -7 /°C. 160 ⁇ 10 -7 /°C, more preferably 40 ⁇ 10 -7 /°C to 140 ⁇ 10 -7 /°C, particularly preferably 50 ⁇ 10 -7 /°C to 120 ⁇ 10 -7 /°C. If the coefficient of thermal expansion is out of the above range, the sealing portion is likely to be damaged during or after sealing due to the difference in thermal expansion with the material to be sealed.
- a raw material powder prepared to give a desired glass composition is melted at 700 to 1000° C. for 1 to 2 hours until a homogeneous glass is obtained.
- the obtained molten glass is shaped into a film or the like, and then pulverized and classified to prepare glass powder.
- the average particle diameter D50 of the glass powder is preferably about 1 to 20 ⁇ m. If necessary, various refractory filler powders are added to the glass powder and mixed to obtain a sealing material.
- a sealing material paste is prepared by adding a vehicle to the sealing material and kneading the mixture.
- the vehicle mainly consists of an organic solvent and a resin, and the resin is added for the purpose of adjusting the viscosity of the paste.
- a surfactant, a thickening agent, etc. can also be added as needed.
- the organic solvent preferably has a low boiling point (for example, a boiling point of 300° C. or lower), leaves little residue after firing, and does not degrade the glass, and its content is preferably 10 to 40% by mass. preferable.
- Organic solvents include propylene carbonate, toluene, N,N'-dimethylformamide (DMF), 1,3-dimethyl-2-imidazolidinone (DMI), dimethyl carbonate, butyl carbitol acetate (BCA), isoamyl acetate, It is preferred to use dimethyl sulfoxide, acetone, methyl ethyl ketone and the like. Further, it is more preferable to use a higher alcohol as the organic solvent.
- Pentanediol and its derivatives specifically diethylpentanediol (C 9 H 20 O 2 ), can also be used as the solvent because of their excellent viscosity.
- the resin preferably has a low decomposition temperature, leaves little residue after firing, and does not easily degrade the glass, and its content is preferably 0.1 to 20% by mass.
- the resin it is preferable to use nitrocellulose, polyethylene glycol derivatives, polyethylene carbonate, acrylic acid ester (acrylic resin), and the like.
- the sealing material paste is applied to the sealing portion of the object to be sealed made of metal, ceramic, or glass using an applicator such as a dispenser or a screen printer, dried, and glazed at 280 to 320 ° C. do.
- an applicator such as a dispenser or a screen printer
- another object to be sealed is brought into contact with the object and heat-treated at 300 to 400° C., so that the glass powder softens and flows to seal the two.
- the glass powder according to the present invention can be used for purposes other than sealing, such as coating and filling. It can also be used in forms other than paste, specifically in the form of powder, green sheet, tablet (a powder material sintered into a predetermined shape), and the like.
- Tables 1 to 3 show examples of the present invention (Sample Nos. 1 to 9, 13 to 27) and Comparative Examples (Sample Nos. 10 to 12).
- raw material powders prepared to give the glass composition shown in the table were placed in a platinum crucible and melted in air at 700 to 1000° C. for 1 to 2 hours. After that, the molten glass was formed into a film with a water-cooled roller, and the film-shaped glass was pulverized with a ball mill and passed through a sieve with an opening of 75 ⁇ m to obtain a glass powder having an average particle diameter D50 of about 10 ⁇ m.
- the obtained glass powder and refractory filler powder were mixed to obtain a mixed powder.
- the average particle size D50 of the refractory filler powder was about 10 ⁇ m.
- Sample No. 1 to 27 were evaluated for glass transition point, thermal expansion coefficient, softening point, fluidity and weather resistance.
- the glass transition point and thermal expansion coefficient in the temperature range of 30 to 150°C were evaluated as follows. First, the mixed powder was placed in a rod-shaped mold, press-molded, and then fired at 280 to 350° C. for 10 minutes on an alumina substrate coated with a release agent. After that, the sintered body was processed into a predetermined shape and measured with a TMA apparatus.
- the softening point was measured with a macro-type differential thermal analyzer, and the softening point was defined as the fourth inflection point.
- the measurement atmosphere was the air, the rate of temperature increase was 10° C./min, and the measurement was started from room temperature.
- Liquidity is evaluated as follows. A mass corresponding to the composite density of the mixed powder was placed in a mold with a diameter of 20 mm and press-molded. After that, sample no. 1 to 12 and 17 to 27 were baked on a glass substrate at 350° C. for 10 minutes. Sample no. 13 to 16 were baked on a glass substrate at 300° C. for 10 minutes. When the flow diameter of the sintered body was 19 mm or more, it was evaluated as " ⁇ ", and when it was less than 19 mm, it was evaluated as "x".
- the weather resistance was evaluated by an accelerated deterioration test by PCT (Pressure Cooker Test). Specifically, after holding the fired body prepared above for 24 hours in an environment of 121 ° C., 2 atm, and 100% relative humidity, visually observed, if there is no precipitate from the fired body surface, "O". , and others were marked with "x".
- PCT Pressure Cooker Test
- sample no. Samples 1 to 9 and 13 to 27 were evaluated as good in fluidity and weather resistance.
- sample no. No. 10 had a low V 2 O 5 content in the glass composition and did not contain CuO, so it had a high softening point and poor fluidity.
- Sample no. No. 11 had a high softening point and poor fluidity due to the low content of V 2 O 5 in the glass composition.
- the glass composition of the present invention is suitable for sealing crystal resonator packages, and is also suitable for sealing airtight packages such as semiconductor integrated circuits, flat display devices, glass terminals for LEDs, and aluminum nitride substrates. is. It can also be used as a sealing material for metals and vacuum insulating glass.
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Abstract
Description
Claims (11)
- ガラス組成として、モル%で、TeO2 15~80%、MoO3+Ag2O 0.1~30%、V2O5 5~40%、CuO 0.1~35%、PbO 0~10%を含有することを特徴とするガラス組成物。
- ガラス組成として、モル%で、CuO 0.3~25%、Li2O+Na2O+K2O 1~30%、MgO+CaO+SrO+BaO+ZnO 1~30%を含有し、実質的にSeO2を含有しないことを特徴とする請求項1に記載のガラス組成物。
- ZnOの含有量が0~25モル%であることを特徴とする請求項1又は2に記載のガラス組成物。
- Nb2O5の含有量が0~10モル%であることを特徴とする請求項1~3の何れかに記載のガラス組成物。
- ガラス組成として、モル%で、Fe2O3 0~10%、Al2O3 0~10%、B2O3 0~20%、WO3 0~20%を含有することを特徴とする請求項1~4の何れかに記載のガラス組成物。
- 請求項1~5の何れかに記載のガラス組成物からなるガラス粉末 40~100体積%と、耐火性フィラー粉末 0~60体積%とを含有することを特徴とする封着材料。
- 耐火性フィラー粉末が略球状であることを特徴とする請求項6に記載の封着材料。
- 耐火性フィラー粉末の全部又は一部がZr2WO4(PO4)2であることを特徴とする請求項6又は7に記載の封着材料。
- 水晶振動子パッケージに用いることを特徴とする請求項6~8の何れかに記載の封着材料。
- 真空断熱ガラスに用いることを特徴とする請求項6~8の何れかに記載の封着材料。
- 請求項6~10の何れかに記載の封着材料とビークルとを含有することを特徴とする封着材料ペースト。
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02293344A (ja) * | 1989-04-19 | 1990-12-04 | Natl Starch & Chem Corp | 電子的用途に使用するのに好適な低軟化点金属酸化物ガラス |
JP2018203549A (ja) * | 2017-05-31 | 2018-12-27 | 日立化成株式会社 | 真空断熱部材及びその製造方法 |
JP2019142725A (ja) * | 2018-02-16 | 2019-08-29 | 日本電気硝子株式会社 | ガラス組成物及び封着材料 |
JP2019202921A (ja) | 2018-05-25 | 2019-11-28 | 日本電気硝子株式会社 | ガラス組成物及び封着材料 |
JP2020059615A (ja) * | 2018-10-05 | 2020-04-16 | 日本電気硝子株式会社 | ガラス組成物及び封着材料 |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH02293344A (ja) * | 1989-04-19 | 1990-12-04 | Natl Starch & Chem Corp | 電子的用途に使用するのに好適な低軟化点金属酸化物ガラス |
JP2018203549A (ja) * | 2017-05-31 | 2018-12-27 | 日立化成株式会社 | 真空断熱部材及びその製造方法 |
JP2019142725A (ja) * | 2018-02-16 | 2019-08-29 | 日本電気硝子株式会社 | ガラス組成物及び封着材料 |
JP2019202921A (ja) | 2018-05-25 | 2019-11-28 | 日本電気硝子株式会社 | ガラス組成物及び封着材料 |
JP2020059615A (ja) * | 2018-10-05 | 2020-04-16 | 日本電気硝子株式会社 | ガラス組成物及び封着材料 |
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