SG188093A1 - Siliceous powder, process for production of the same, and use thereof - Google Patents
Siliceous powder, process for production of the same, and use thereof Download PDFInfo
- Publication number
- SG188093A1 SG188093A1 SG2013007372A SG2013007372A SG188093A1 SG 188093 A1 SG188093 A1 SG 188093A1 SG 2013007372 A SG2013007372 A SG 2013007372A SG 2013007372 A SG2013007372 A SG 2013007372A SG 188093 A1 SG188093 A1 SG 188093A1
- Authority
- SG
- Singapore
- Prior art keywords
- silica powder
- powder
- silica
- resin
- mass
- Prior art date
Links
- 239000000843 powder Substances 0.000 title claims abstract description 169
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 268
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 128
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000004065 semiconductor Substances 0.000 claims abstract description 48
- 239000000463 material Substances 0.000 claims abstract description 44
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 239000003566 sealing material Substances 0.000 claims abstract description 29
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 28
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims abstract description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052796 boron Inorganic materials 0.000 claims abstract description 21
- 239000011342 resin composition Substances 0.000 claims abstract description 21
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 38
- 239000003822 epoxy resin Substances 0.000 claims description 32
- 229920000647 polyepoxide Polymers 0.000 claims description 32
- 238000001179 sorption measurement Methods 0.000 claims description 19
- 229920005989 resin Polymers 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 abstract description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 20
- 229910000679 solder Inorganic materials 0.000 description 20
- 238000005336 cracking Methods 0.000 description 17
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 12
- 239000002253 acid Substances 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 11
- 238000005259 measurement Methods 0.000 description 11
- 229910052697 platinum Inorganic materials 0.000 description 10
- 239000012086 standard solution Substances 0.000 description 10
- -1 aluminum organic compound Chemical class 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 6
- 229910002026 crystalline silica Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
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- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 239000006087 Silane Coupling Agent Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229930185605 Bisphenol Natural products 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 238000011088 calibration curve Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000004611 spectroscopical analysis Methods 0.000 description 4
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 4
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
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- 125000005843 halogen group Chemical group 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
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- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- GLTDLAUASUFHNK-UHFFFAOYSA-N n-silylaniline Chemical compound [SiH3]NC1=CC=CC=C1 GLTDLAUASUFHNK-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 2
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- 229910052709 silver Inorganic materials 0.000 description 2
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- YUSCRGFYKCAQHE-HQFNMCNFSA-N (8r,9s,13s,14s,17s)-13-methyl-6,7,8,9,11,12,14,15,16,17-decahydrocyclopenta[a]phenanthrene-3,17-diol;(8r,9s,13s,14s,16r,17r)-13-methyl-6,7,8,9,11,12,14,15,16,17-decahydrocyclopenta[a]phenanthrene-3,16,17-triol Chemical compound OC1=CC=C2[C@H]3CC[C@](C)([C@H](CC4)O)[C@@H]4[C@@H]3CCC2=C1.OC1=CC=C2[C@H]3CC[C@](C)([C@H]([C@H](O)C4)O)[C@@H]4[C@@H]3CCC2=C1 YUSCRGFYKCAQHE-HQFNMCNFSA-N 0.000 description 1
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- WJQOZHYUIDYNHM-UHFFFAOYSA-N 2-tert-Butylphenol Chemical compound CC(C)(C)C1=CC=CC=C1O WJQOZHYUIDYNHM-UHFFFAOYSA-N 0.000 description 1
- LVNLBBGBASVLLI-UHFFFAOYSA-N 3-triethoxysilylpropylurea Chemical compound CCO[Si](OCC)(OCC)CCCNC(N)=O LVNLBBGBASVLLI-UHFFFAOYSA-N 0.000 description 1
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 description 1
- BSFODEXXVBBYOC-UHFFFAOYSA-N 8-[4-(dimethylamino)butan-2-ylamino]quinolin-6-ol Chemical compound C1=CN=C2C(NC(CCN(C)C)C)=CC(O)=CC2=C1 BSFODEXXVBBYOC-UHFFFAOYSA-N 0.000 description 1
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- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 150000007519 polyprotic acids Polymers 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 238000011417 postcuring Methods 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 208000029340 primitive neuroectodermal tumor Diseases 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 229940079877 pyrogallol Drugs 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920006132 styrene block copolymer Polymers 0.000 description 1
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 125000002256 xylenyl group Chemical class C1(C(C=CC=C1)C)(C)* 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
-
- 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
- H01L23/293—Organic, e.g. plastic
- H01L23/295—Organic, e.g. plastic containing a filler
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/0001—Technical content checked by a classifier
- H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
- H05K2201/0203—Fillers and particles
- H05K2201/0206—Materials
- H05K2201/0209—Inorganic, non-metallic particles
Landscapes
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Compounds (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
:To provide a silica powder useful for preparation of a sealing material for semiconductors, and a process for its production.5 It is a silica powder which has a Freundlichadsorption constant K of pyridine of from 1.3 to 5.0. It is particularly preferred that the total of contents (as calculated as oxides) of Si02, Al203 and 13203 is at least 99.5 mass%, and the total of contents of Al203 and 33303 is10 from 0.1 to 20 mass%. The process for producing the silica powder is such that at least two burners are disposed in a furnace body with an angle of from 2 to 10ºto the central axis of the furnace body, and from one burner, a raw material silica powder is sprayed and from15 at least one burner, an aluminum source material and/or a boron source material is sprayed, into a flame. A resin composition is further provided which contains the above silica powder or inorganic powder.
Description
SILICA POWDER, PROCESS FOR ITS PRODUCTION AND ITS USE + TECHNICAL FIELD
The present invention relates to a silica powder, a process for its production and its use.
To meet requirements for downsizing, weight saving and high performance of electronic equipment, downsizing, reduction in thickness and high densification of semiconductors are rapidly in progress. Further, with respect to the mounting method for semiconductors, surface mounting suitable for high density mounting on a printed board or the like ig predominant. In recent years, for a semiconductor of such a surface mounting type, an ultrathin semiconductor package has been used to lower the mounting height on a printed board, whereby the thickness of the package has become very thin. More recently, a PoP (Package on Package) mounting method to mount another semiconductor on a semiconductor, has been practically used, whereby reduction in thickness of semiconductors has been in progress more than ever.
On the other hand, from an increasing consciousness about environmental problems in recent years, it has been commen: to use a lead-free solder which does not contain lead having a large environmental load, for mounting a semiconductor on a circuit board, and the temperature at the time of mounting has become higher by a few tens degrees in centigrade than ever. Namely, a semiconductor package which has become thinner than ever, is mounted as exposed to a temperature higher than ever, whereby a problem of package cracking has become frequented, and a sealing material for semiconductors is required to have the flexural strength, solder cracking resistance, etc. further improved.
In order to satisfy such requirements, it has been attempted to improve the flexural strength or to reduce the stress by such a means to improve e.g. an epoxy resin or phenol resin curing agent to be used for the sealing 1s material for semiconductors (Patént Documents 1 and 23.
However, the effects to improve the flexural strength by such means have been inadequate, and there has been no sealing material for semiconductors whereby a package thinner than ever is durable at a mounting temperature with a lead-free solder and the solder cracking resistance can be remarkably improved.
Further, as a method of modifying a ceramic powder, a case may be mentioned wherein for the purpose of improving the high temperature storage property 28 (reliability) of a sealing material for semiconductors, the chemical adsorption of ammonia is controlled, and impurities in the sealing material for semiconductors are trapped (Patent Document 3).
Patent Document 1: JP-A-2001-233937
Patent Document 2: JP-A-10-279669 ‘Patent Document 3: WO/2007/132771 . DISCLOSURE OF THE INVENTION Cee
It is an object of the present invention to provide a silica powder useful for preparing e.g. a sealing 16 material for semiconductors having the flexural strength improved and having solder cracking resistance further improved.
MEANS TC ACCOMPLISH THE OBJECT
The present inventors have conducted an extensive study to accomplish the above object and have found a silica powder which accomplishes the object. The present invention is based on suck a discovery and provides the following. (1) A silica powder characterized in that it has a
Freundlich adsorption constant XK of pyridine of from 1.3 to 5.0. {2) The silica powder according to the above (1), wherein the total of contents (as calculated as oxides) of 8i0,, Al.0; and B,0; is at least 99.5 mass%, and the total cf contents of A1,0; and B,0s is from 0.1 to 20 massy.
(3) The silica powder accoxding to the above (1) or (2), which has a specific surface area of from 0.5 to 5 m'/g and an average particle size of from 1 to 60 pra. (4) An inorganic powder characterized in that it contains the silica powder as defined in any one of the above {1} to (3). | : (3) The inorganic powder according to the above (4), wherein the inorganic powder is a silica powder and/or an alumina powder. oo (6) A process for producing the silica powder as defined in any one of the above (1) to (3), characterized in that at least two burners are disposed in a furnace body with an angle of from 2 to 10° to the central axis of the furnace body, and from one burner, a raw material gilica powder is sprayed and from at least one burner, an aluminum source material and/or a boron source material is sprayed, into a flame.
Ce (7) The process for producing the silica powder according to the above (6), wherein the aluminum source 2¢ material is an aluminum oxide powder, and the raw material silica powder has an A1.,0; content of at most 1 mass%. (8) The process for producing the silica powder according to the above (7), wherein the aluminum oxide powder has an average particle size of from 0.01 to 10 a. (8) A resin composition characterized in that it contains the silica powder as defined in any one of the above (L} to (3) or the inorganic powder as defined in the above (4) or (5). (10) The resin composition according to the above (9), wherein the resin in the resin composition is an epoxy 5 resin. (11) 2 sealing material for semiconductors, employing the : resin composition as defined in the above (9) or (10).
The present invention provides a resin composition, particularly a resin composition as a sealing material for semiconductors, having the flexural strength and solder cracking resistance improved, and a silica powder useful for the preparation of such a resin composition.
Now, the present invention will be described in detail.
The silica powder of the present invention is a silica powder which has a Freundlich adsorption constant
K of pyridine of from 1.3 to 5.0. Pyridine as a basic substance will be adsorbed to acid points on the surface of the silica powder. Accordingly, the value of the adsorption constant K of this substance being large means that the number of acid points on the surface of the silica powder is large. When acid points of the silica powder are many, bonding points with a basic silane coupling agent such as aminosilane or phenylaminosilane will be many. Accordingly, the adhesion between the silica powder surface and a resin component such as an epoxy resin or a phencl resin in a sealing agent for semiconductors will be firmer, whereby the flexural strength will be improved, and moisture tends to hardly penetrate into the interface between the silica powder and the resin component, and thus the solder cracking. resistance will alsc be remarkably improved.
If the Freundlich adsorption constant K of pyridine is less than 1.3, bonding points of the silica powder with the silane coupling agent will be less, whereby it ~ becomes impossible to remarkably improve the solder cracking resistance or flexural strength of the sealing material for semiconductors. On the other hand, if the
Freundlich adsorption constant K of pyridine exceeds 5.0, the number of acid points on the surface of the silica powder will be too many, whereby the epoxy resin will be cured. Conseguently, there will be problem such that at the time of packaging a semiconductor by means of a sealing material for semiconductors, the vigcosity of the sealing material increases, and the moldability will be impaired. The value of the Freundlich adsorption constant XK of pyridine is preferably from 1.5 to 4.5, particularly preferably from 2.0 to 4.3. These values : are unique and distinct as compared with from 0.07 to 0.8 i.e. the value of the Freundlich adsorption constant K of conventional silica powder.
The Freundlich adsorption constant XK of pyridine can be measured by the following procedure. (1) Preparation of pyridine standard solutions: 0.1 mol of pyridine for spectrometry is taken into a 500 ml measuring flask and adjusted to the constant volume with n-heptane for spectrometry. Then, 0.25 ml, 0.50 wl and 1.00 ml of such a pyridine solution are, regpectively, taken into 200 ml measuring flasks and adjusted to the constant velume with n-heptane to prepare pyridine standard solutions of 0.25 mmol/l, 0.50 mmol/l and 1.00 mmol /1, (2) Adsorption on silica powder: 4.00 g each of silica powder preliminarily dried under heating at 200°C for 2 hours, followed by cooing in a desiccator, is accurately weighed and put into three 25 ml measuring flasks. Into the respective measuring flasks, 20 ml of the pyridine standard solutions of 0.25% mmol/L, 0.50 mmol/l and 1.00 mmol/l are put and mixed by shaking for 3 minutes. These measuring flasks are immersed in a constant temperature tank set at 25°C for 2 hours to have pyridine adsorbed on the silica powder. (3) Measurement of adsorbed amount of pyridine: From the above measuring flasks having the pyridine standard solutions and silica powders mixed therein, the supernatants were respectively taken and put into measuring cells of an ultraviolet-visible spectrophotometer and the concentration of residual pyridine remaining without being adsorbed is quantified by the absorbance.
(4) Calculation of Freundlich adsorption constant XK of pyridine: The Freundlich adsorption constant K of pyridine is calculated by the Freundlich adsorption formula of logA=logK+ (1l/n)logC.
Namely, when a graph is . drawn so that Y axis represents logh and X axis represents (1/n)logC, logK is obtained from Y-intercept,
whereby K can be calculated.
Here, A is the amount (umol/g) of pyridine adsorbed on 1 g of silica powder, C ig the concentration (pmol/ml}) of residual pyridine in the supernatant, and K and n are constants.
: Here, as an example of the ultraviolet-vigible spectrophotometer to be used for the measurement, “Ultraviolet-visible Spectrophotometer, Model UV-1800*, tradename, manufactured by Shimadzu Corporation may be mentioned.
As examples of the reagents to be used for preparation of the pyridine standard solutions, pyridine
(spectrometry grade) and n-heptane (spectrometry grade), manufactured by Wako Pure Chemical Industries, Ltd., may be mentioned.
Further, the wavelength for measurement of the absorbance was 251 nm, and only n-heptane was measured, and background correction was carried out.
For the preparation of a calibration curve, the pyridine standard solutions of 0.00 mmmol/l, 0.25 mmol/l, 0.50 mmol/l and 1.00 mmol/l were used.
. 2 Co
Further, a characteristic of the silica powder of the present invention is that the total of contents (as calculated as oxides) of Si0,, Al,0; and B;03; is at least 99.5 mass%, and the total of contents of Al,0, and B,0O, is - from 0.1 to 20 mass%. If the total of contents of SiQ,,
Al;0; and B20: is less than 99.5 masss, l.e. if the content other than Si0;, Al;0; and B;0; exceeds 0.5 mass%, when the powder is formed into a sealing material for semiconductors, unnecessary substances will increase as 1¢ impurities, such being undesirable. For example, Na,Q,
Fey0:, etc., are likely to be partially ionized and elute to present damages to semiconductor chips or wirings.
MgO, X;0, Cal, etc. are likely to increase the thermal expansion coefficient of silica powder and thus present an adverse effect to the solder cracking resistance.
The total of contents of 8i0,, Al.0; and B20; is preferably at least 99.6 mass%, more preferably at least 99.7 mass%.
Further, the total of contents of 21,0; and B20; in the silica powder is preferably from 0.1 to 20 mass%.
When Al and B are present in the silica powder, the positions of Al and B will be strong acid points. By such acid points, bonding points of the silica powder surface with the basic silane coupling agent will increase, whereby the flexural strength and the solder cracking resistance will be improved. If the total of contents of Al,0; and B,0s ig less than 0.1 mass%, the increase of acid points tends to be inadeguate. On the other hand, if it exceeds 20 mass%, the thermal expansion coefficient of the silica powder tends to be too large, which is likely to adversely affect the solder cracking resistance. The total of contents of Al,0; and R05; ig more preferably from 0.2 to 18 mass%, further preferably from 0.3 to 15 mass%. or The SiO; content (as calculated as an oxide) in the silica powder of the present invention can be measured by : a mass reduction method, the Al,0; content (as calculated as an oxide} can be measured by an atomic adsorption analysis, and the B,0. content (as calculated as an oxide) can be measured by an ICP emission gpectrometry, © as follows. (1} Measurement of 8i0, content: 2.5 g of silica powder is accurately weighed on a platinum dish, and special grade reagent hydrofluoric acid, special grade reagent sulfuric acid and pure water are added in amounts of 20 ml, 1 ml and 1 ml, respectively. Such a platinum dish is left to stand still for 15 minutes on a sand bath heated at 300°C to let the powder dissolve and be dried.
Then, into a muffle furnace heated at 1,000, the platinum dish is put and heated for 10 minutes to let fluosilicic acid evaporate. In a desiccator, the platinum dish ig left to cool to room temperature, and ‘then, the mass of the platinum dish is accurately weighed, whereupon the content of $i0, in the silica powder ig calculated from the mass reduction. (2) Measurement of Al.O; content: 1 g of gilica powder is accurately weighed on a platinum dish, and special reagent hydrofluoric acid and special reagent oo perchloric acid are added in amounts of 20 ml and 1 ml, respectively. Such a platinum dish is left to stand : : still for 15 minutes on a sand bath heated at 300°C and then cooled to room temperature, and the content is transferred to a 25 ml measuring flask and adjusted to the constant volume with pure water. The Al amount in this solution is quantified by a calibration method by means of an atomic absorption photometer. The 21 amount ig calculated into Al.0. to obtain the content in the silica powder. As an example of the atomic absorption photometer, “Atomic Absorption Photometer Model AR-96en, tradename, manufactured by Nippon Jarrel-Ash may be mentioned. As an example of the standard solution to ke used for preparing the calibration curve, Al standard solution for atomic absorption (concentration: 1,000 ppm) manufactured by Kanto Chemical Co., Ltd. may be mentioned.
Further, at the time of the measurement, as the frame, an acetylene/nitrous oxide frame was used, and the absorbance at a wavelength of 209.3 nm was measured for quantitative determination. (3) Measurement of B,0; content: 1 g of silica powder is accurately weighed on a platinum dish, and special grade hydrofluoric acid, special grade nitric acid and a 1% aqueous solution of special grade mannitol are added in amounts of 20 ml, I ml and 1 ml, respectively, and the platinum dish was left to stand still for 15 minutes on a sand bath heated at 300°C to let the powder dissolve and be dried. Then, to the dried product on the platinum dish, special reagent grade nitric acid and pure water are added in an amount of 1 ml each for redissclution, and then, the solution is transferred to a 25 ml measuring flask and adjusted to the constant volume with pure water. The B amount in this solution is quantified by a calibration curve method by means of an ICP emission spectrophotoanalyzer. Such a
B amount is calculated into B,0; to cbtain the content in the silica powder. As an example of the ICP emission 18 spectrophotoanalyzer, “Model SPS-1700R", tradenams, manufactured by Seiko Instruments Inc. may be mentioned, and the emission intensity at a wavelength of 249.8 nm is measured. As an example of a standard solution to be used for preparing the calibration curve, B-standard solution for atomic absorption (concentration: 1,000 ppm) : manufactured by Kanto Chemical Co., Ltd. may be mentioned.
The effect for improving the flexural strength and the solder cracking resistance by the resin composition of the present invention will be further increased when the specific surface area of the silica powder is within a range of from 0.5 to 5 m’/g, and the average particle size is within a range of from 1 to 60 um. If the specific surface area is less than 0.5 m?/g, the bonding area of the silica powder surface with the silane 3 coupling agent tends to be too small, whereby the flexural strength or the solder cracking resistance tends to be hardly improved. On the other hand, if the specific surface area exceeds 5 m’/g, such means that the silica powder contains a large amount of fine particles, . or a part or whole of the particle surface has irregularities, whereby at the time of packaging a semiconductor by means of a sealing agent for semiconductors, the viscosity of the sealing material increases to impair the moldability. The range of the specific surface area is preferably from 0.6 to 4.8 m*/g, more preferably from 0.7 to 4.7 m?/qg.
Further, if the average particle gize of the silica powder is less than 1 um, likewiee, at the time of packaging a semiconductor by means of a sealing material for semiconductors, the viscosity of the sealing material increases to impair the moldability, such being undesirable. On the other hand, if the average particle size exceeds 60 um, since the thickness of the semiconductor package is very thin, there will be a problem that a semiconductor chip will thereby be damaged by scratching, or it tends to be difficult to obtain a uniform package free from irregularities. The range of the average particle size is preferably from 2 to 55 um, more preferably within a range of from 2 to 50 um.
Further, the maximum particle size is preferably at most 196 pm, more preferably at most 128 pum.
The average particle size of the silica powder of the present invention is measured based on the particle size measurement by a laser diffraction scattering method.
As the measuring machine to be used, for example, “Cirrus
Granulometer Model 920”, tradename, manufactured by
CIRRUS, is used, and silica powder is dispersed in water 7 and further subjected to dispersion treatment by an ultrasonic homogenizer at an output of 200 W for 1 minute, followed by measurement . Here, the measurement of the particle size distribution is carried out by particle size channels of 0.3, 1, 1.5, 2, 3, 4, 6, 8, 12, 16, 24, 32, 48, 64, 96, 128 and 196 pm. In the measured particle size distribution, the particle size where the cumulative } mass becomes 50%, is the average particle gize, and the particle size where the cumulative mass becomes 100%, is the maximum particle size.
The specific surface area of the silica powder of the present invention is measured based on the specific surface area measurement by a BET method. The specific surface area measuring apparatus may, for example, be “Macsorb Model HM-1208", tradename, manufactured by
Mountech Co., Ltd.
The gilica powder of the present invention is able to exhibit its effects even when mixed to another inorganic powder. The content of the silica powder of the present invention in such an inorganic powder is preferably at least 0.5 mass%, more preferably at least 2 mass%. The type of the inorganic powder is preferably a silica powder and/or an alumina powder. These powders may be used alone or in combination as a mixture of two of them. In order to lower the thermal expansion coefficient of the sealing material for semiconductors or to reduce the abrasion of a mold, a silica powder is selected for use, and in order to impart thermal 1c conductivity, an alumina powder is selected for use.
Here, the silica powder is preferably such that the value of the amorphous ratio as measured by the after-mentioned method is at least 95%.
The silica powder of the present invention is such 1s that the amorphous ratio measured by the following method is preferably at least 95%, particularly preferably at ~ least 98%. The amorphous ratio is obtained from the intensity ratio of specific diffraction peaks by carrying out an X-ray diffraction analysis by means of a powder X- ray diffraction apparatus (such as “Model Mini Flex”, tradename, manufactured by RIGAKU K.K.) within such a range that 28 of CuKo-line is within a range of from 26° to 27.5°. In the case of the silica powder, crystalline silica has the main peak at 26.7°, while amorphous silica has no peak. When amorphous silica and crystalline silica are present in a mixed state, a peak height at 26.7° corresponding to the proportion of the crystalline gilica is obtained, and from the ratio of the X-ray intensity of a sample to the X-ray intensity of the crystalline silica standard sample, the mixed ratio of the crystalline silica (X-ray diffraction intensity of the sample/X-ray diffraction intensity of crystalline silica) is calculated, and the amorphous ratio is obtained by the formula, amorphous ratio (%) = (l-mixed ratio of crystalline silica) x 100.
The average sphericity of each of the silica powder cf the present invention, the inorganic powder and the alumina powder is preferably at least 0.80, particularly preferably at least 0.85. It is thereby possible to lower the viscosity of the resin composition and to improve the moldability. For the average sphericity, a particle image photographed by e.g. a stereoscopic microscope (such as “Model 8MZ-107, tradename, : manufactured by Nikon Corporation) is taken into an image analyzer (such as “MacView”, tradename, manufactured by
Mountech Co., Ltd.), and from the photograph, the projected area (A) and the periphery length (PM) of a particle are measured. When the area of a perfect circle corresponding to the peripheral length (PM) is represented by (B), the sphericity of the particle is represented by A/B. Accordingly, when a perfect circle having the same peripheral length as the peripheral ~ length (PM) of a sample is assumed, PM=27r and B=mr?, and thus, B=ax(PM/27)?. The sphericity of an individual particle will be sphericity=A/B=Ax47/(PM)2. Sphericities of optional 200 particles thus obtained, were determined, and the average value was taken as the average sphericity.
Now, the process for producing the silica powder of the present invention will be described. :
The process of the present invention is a process for producing the silica powder, characterized in that at least two burners are disposed in a furnace body with an angle of from 2 to 10° to the central axis of the furnace body, and from one burner, a raw material silica powder is sprayed and from at least one burner, an aluminum source material and/or a boron source material is sprayed, into a flame. If the raw material silica powder, and the aluminum source material and/or the boron source material, are sprayed from the same one burner, the sprayed ) materials necessarily spread in a conical shape, whereby . the proportion of the aluminum source material and/or the boron source material fused on the surface of the raw material silica powder tends to be small, and it becomes impossible to produce the silica powder of the present invention wherein the total of contents of Al,0; and BQ; ig from 0.1 to 20 mass%. Further, even in a case where the raw material silica powder, and the aluminum source material and/or the boron source material, are preliminarily mixed, they will be spread in a conical shape at the time of spraying and will be dispersed and separated, whereby the composition will be non-uniform.
At least two burners are disposed in a furnace body with an angle of from 2 to 10° to the central axis of the furnace body, to form a focal point, and from one burner, a raw material silica powder is sprayed and from at least one burner, an aluminum source material and/or a boron source material is sprayed, into a flame, whereby the silica powder of the present invention can be produced very efficiently.
By using a plurality of burners to spray the aluminum source material and/or the boron 1¢ source material, it is possible to further increase the uniformity of the conposition of the silica powder of the present invention.
A preferred number of burners is two burners to spray the aluminum source material and/or the boron source material per one burner to spray the raw material silica powder.
Here, the disposed angle of burners is required to be from 2 to 10° to the central axis of the furnace body.
If the disposed angle of burners is less than 2°, the focal point will be out of ‘the flame, and the proportion of the aluminum source material and/or the boron source material £0 be fused on the surface of the raw material silica powder tends to be small.
On the other hand, if the disposed angle of burners exceeds 10°, the focal point will be formed before the aluminum source material and/or the boron source material ig fused on the surface of the raw material silica powder, such being undesirable.
The disposed angle of burners is more preferably within a range of from 3 to 8°.
In the present invention, the aluminum source material is preferably an aluminum oxide powder. The aluminum source material may, for example, be aluminum : 5 oxide, aluminum hydroxide, aluminum sulfate, aluminum chloride or an aluminum organic compound. However, aluminum oxide is most preferred, since it is close to the melting point of the raw material silica powder, so that it is readily fused on the surface of the raw material silica powder when sprayed from a burner, and the impurity content is also small. Here, the average particle size of the aluminum oxide powder is preferably from 0.01 to 10 um. If the average particle size is less than 0.01 pm, the powder tends to be agglomerated, and the composition when fused with the silica powder tends . to be non-uniform, and likewise, 1f it exceeds 10 um, the composition when fused with the silica powder tends to be non-uniform. The range of the average particle size is preferably from 0.032 to 8 um, more preferably from 0.05 to 5 um. in the present invention, the Al1.0, content in the raw material silica powder is preferably at most 1 mass%.
Among Al and B in the silica powder, only one located on the surface of the powder will form a strong acid point and is capable of bonding to a basic silane coupling agent. Thus, Al,0; present in the interior of the raw material silica powder will present an adverse effect to increase the thermal expansion coefficient of the silica powder. Accordingly, the Al,0. content in the raw material silica powder is more preferably at most 0.8 mass%, further preferably at mest 0.5 mass%. - The raw material silica powder may contain Fes0,,
Na,0, MgO, CaO, B;0;, etc. in addition to the above- mentioned Al,0,. However, the 810; content in the raw material silica powder is preferably at least 97 masst, more preferably at least 98 mass%.
As an apparatus to spray the raw material silica powder and the aluminum source material and/or the boron source material to the flame thereby to fuse them and collect them, one having a collecting device connected to the furnace body equipped with the burners may be used.
The furnace body may be an open or closed type or a vertical or horizontal type. The collecting device is provided with at least one of a gravity settling chamber, a cyclone, a bag filter, an electrical dust collector, etc., and is capable of collecting the produced silica powder by adjusting the collecting conditions. Examples of such a collecting device are disclosed, for example, in JP-A-11-57451 and JP-A-11-71107.
In the present invention, the Freundlich adsorption constant K of pyridine, of the silica powder, may be increased or reduced by adjusting the sizes of the aluminum source material and/or the boron source material to be fused on the surface of the raw material silica powder, the Al,0, content and the B,0; content in the silica powder, the specific surface area and the average particle size of the silica powder, etc. The Al,0; content and the B,0, content in the silica powder may respectively be increased or reduced by adjusting the ratio of the spray amounts of the raw material silica powder and the aluminum source material and/or the boron source material to the burner flame. The specific surface area, the average particle size, etc. of the silica powder may be adjusted by e.g. the particle size constitution of the raw material silica powder or the flame temperature. Further, the average sphericity and amorphous ratio may be adjusted by e.g. the amount of the raw material silica powder supplied to the flame or the flame temperature. Further, various silica powders different in the specific surface area, the average particle size, the Al,0; content, the B:O; content, eto. may be preliminarily produced, and two or more of them may suitably be mixed to produce a silica powder having the Freundlich adsorption constant K, 41,0: content, RB,0; content, specific surface area, average particle size, etc. further specified.
The resin composition of the present invention is a resin composition containing the silica powder or the inorganic powder of the present invention. The content of the silica powder or the inorganic powder in the resin composition is from 10 tc 95 mass%, more preferably from
30 to 90 mass%.
The resin may, for example, be an epoxy resin, a silicone resin, a phenol resin, a melamine resin, a urea resin, an unsaturated polyester, a £luororesin, a polyamide such as polyimide, polvamideimide or : polyetherimide, a polyester such as polybutylene terephthalate or polyethylene terephthalate, a polyphenylene sulfide, an organic polyester, a polysulfone, a liquid crystal polymer, a polyether sulfone, a polycarbonate, a maleimide-modified resin, an
ABS resin, an AAS (acrylonitrile/acryl rubber /styrene) resin, an AES (acrylonitrile/ethylene/propylene/diene rubber/styrene} resin or the iike. Among them, an epoxy resin, a silicone resin or a phenol resin is, for example, preferred. :
Among them, an epoxy resin having at least two epoxy groups in one molecule is preferred as a sealing agent for semiconductors. For example, a phenol novolac type epoxy resin; an orthocresol novolac type epoxy resin; one 2¢ having a novolac resin of a phenol and an aldehyde epoxidized; a glycidyl ether such as bisphenol Aa, bisphenol F or bisphenol 8; a glycidyl ester acid epoxy resin obtained by a reaction of a polybasic acid such as phthalic acid or dimer acid with epochlorohydrin; a linear aliphatic epoxy resin; an alicyclic epoxy resin; a heterocyclic epoxy resin; an alkyl-modified polyfunctional epoxy resin; a B-naphthol novolac type epoxy resin; a 1,6-dihydroxynaphthalene type epoxy resin; a 2,7-dihydroxynaphthalene type epoxy resin; a bishydroxybiphenyl type epoxy resin; and an epoxy resin having an halogen atom such as bromine introduced to impart flame retardancy, may be mentioned. Among them, from the viewpoint of the moisture resistance or the solder reflow resistance, a orthocresol novolac type epoxy resin, a bishydroxybiphenyl type epoxy resin or a naphthalene-skeleton epoxy resin ig, for example, preferred.
The epoxy resin to be used in the present invention ig one containing a curing agent for an epoxy resin, or a curing agent for an epoxy resin and a curing accelerator for an epoxy resin. The curing agent for an epoxy resgin oo 15 may, for example, be a novolac resin obtainable by reacting one or more selected from the group consisting of phenol, cresol, xylenol, resorcinol, chlorophenol, t- butylphenol, nonylphencl, isopropylphenol and octylphenol with formaldehyde, paraformaldehyde or paraxylene in the presence of an oxidation catalyst; a pelyparahydroxystyrene resin; a bisphenol compound such as bisphenol A or bisphenol §; a tri-functional phenol such as pyrogallol or phloroglucinol; an acid anhydride such as maleic anhydride, phthalic anhydride or pyromellitic anhydride; or an organic amine such as metaphenylenediamine, diaminodiphenylmethane or diaminodiphenylsulfone.
In order to accelerate the reaction of the epoxy resin with the curing agent, a curing accelerator such as triphenylphosphine, benzyldimethylamine or 2- methylimidazele, may be used.
To the resin composition of the present invention, the following components may further be incorporated, as the case requires. :
As a stress-lowering agent, a rubber-like substance such as a silicone rubber, a polysulfide rubber, an acrylic rubber, a butadiene rubber, a styrene block copolymer or a saturated elastomer; a thermoplastic resin; a resin-like substance such as a silicone regin; or a resin having a part of or whole of an epoxy resin or phenol resin modified with e.g. an amino silicone, an epoxy silicone or an alkoxy silicone may, for example, be ~ mentioned.
As a silane coupling agent, an epoxysilane such as y-glycidoxypropyltrimethoxysilane or R-(3,4- epoxycyclohexyllethyltrimethoxysilane; an aminosilane such as aminopropyltriethoxysilane, ureidopropyltriethoxysilane or N- . phenylaminopropyltrimethoxysilane; a hydrophobic silane compound such as phenyltrimethoxysilane, methyltrimethoxysilane or octadecyltrimethoxysilane or a mercaptosilane may, for example, be mentioned. hs a surface treating agent, Zr chelate, a titanate coupling agent or an aluminum coupling agent may, for example, be mentioned.
As an auxiliary flame retardant, Sb,0;, Sb:C; or Sh,0s may, for example, be mentioned.
As a flame retardant, a halogenated epoxy resin or a phosphorus compound may, for example, be mentioned.
As a coloring agent, carbon black, iron oxide, a dye or a pigment may, for example, be mentioned. oo
Further, as a mold release agent, a natural wax, a synthetic wax, a metal salt of a linear fatty acid, an acid amide, an ester or a paraffin may, for example, be mentioned.
The composition of the present invention can be produced by blending predetermined amounts of the above respective materials by e.g. a blender or a Henschel + 15 mixer, kneading the blended product by e.g. a hot roll, a kneader, a single screw or twin screw extruder, and cooling and grinding the kneaded product.
The sealing material for semiconductors of the present invention is made of the resin composition containing an epoxy resin, which further contains a curing agent for the epoxy resin and a curing accelerator for the epoxy resin. To seal a semiconductor using the sealing material for semiconductors of the present invention, a conventional molding means such as a transfer molding method or a vacuum printing molding method may be employed.
Now, the present invention will be described in further detail with reference to Examples, but it should ~ be understood that the present invention is by no means restricted to such specific Examples.
EXAMPLES 1 to 9 and COMPARATIVE EXAMPLES 1 to 7
Various raw material silica powders different in the average particle size and in the Al,0, content, aluminum source materials and boron source materials were prepared, and they were subjected to melting, fusing and spheroidizing treatments in the flame to produce various silica powders shown in Table 1 by means of an apparatus disclosed in JP-A-11-57451 i.e. an apparatus wherein a plurality of burners are disposed in a furnace body so that they are adjustable at an angle of from 0 to 15° to the central axis of the furnace body. Further, such powders were suitably blended to produce silica powders and inorganic powders as shown in Table 2.
Here, adjustment of the Freundlich adsorption constant K of pyridine, of the silica powder, was made by changing e.g. the average particle size of the aluminum source material and/or the boron source material to be fused on the surface of the raw material silica powder, the Al;0; content and the B,0. content in the silica 25° powder, or the specific surface area and the average particle size of the silica powder. Adjustment of the
Al,03; content and the B,0; content in the silica powder
‘was carried out by adjusting the ratio of the raw material silica powder and the aluminum source material and/or the boron source material sprayed to the burners.
Adjustment of the specific surface area, the average particle size, etc. of the silica powder was carried out by adjusting e.g. the particle constitution of the raw material silica powder or the flame temperature. Further, adjustment of the average sphericity, amorphous. ratio, etc. of the silica powder was carried out by adjusting the amount of the raw material silica powder supplied to the flame or the flame temperature. Here, the maximum temperature of the flame was within a range of from about 2,000°C to 2,300°C.
The amorphous ratio of the silica powder was at least 99.5% in each case.
With respect to these silica powderg, the Freundlich adsorption constant K of pyridine, the 3i0, content, the 21,0, content, the By0; content, the specific surface area, the average particle size, the average sphericity, etc. were measured and shown in Table 2. ol In order to evaluate properties of the obtained silica powders and inorganic powders as a filler for the sealing material for semiconductors, to 86.5 parts (parts by mass, the same applies hereinafter) of each powder, 6.7 parts of a 4,4’'-bis(2,3-epoxypropoxy)-3,3’,5,5 ~ tetramethylbiphenyl type epoxy resin, 5.5 parts of a phenol resin, 0.3 part of triphenylphosphine, 0.6 part of phenylaminosilane, 0.1 part of carbon black and 0.3 part of carnauba wax were added, followed by dry blending by a
Henschel mixer. Then, the blended product was heat- kneaded by a parallel matching twin screw extruder (screw diameter D: 25 mm, kneading disk length: 10 Dmm, number of revolution of paddle: 80 to 120 rpm, discharge amount: 2.5 kg/hr, and temperature of the kneaded product: 100 to 101°C). The kneaded product (discharged product) was pressed by a pressing machine and cooled, and then ground to produce a sealing material for semiconductors, and the flexural strength, the solder cracking resistance and the moldability (spiral flow) were evaluated as follows. The results are shown in Table 2. Do (1} Flexural strength
The flexural strength of the cured product for the sealing material for semiconductors, obtained as described above, was measured as follows. That is, each of the above sealing materials for semiconductors was : molded in a shape of 10 mm in width x 80 mm in length x 4 mm in height by means of a transfer molding machine under molding conditions at 175°C for 120 seconds, followed by pogt-curing at a temperature of 175°C for 6 hours to prepare five test pieces for evaluation in each case.
And, using “Autograph Model AG-5000A”, tradename, manufactured by Shimadzu Corporation, the flexural strength was measured in accordance with JIS K7171. Here, the distance between supporting points was 64 mm, the loading rate was 5 mm/min, and the measuring environment was 25°C under a relative humidity of 50%. The average value of the respective measured values (n=5) was obtained and taken ag the flexural strength. | The larger the numerical value (MPa), the higher the flexural strength. {2) Solder cracking resistance
The solder cracking resistance of the sealing materials fox semiconductors obtained as described above was measured as follows. That is, a simulated semiconductor chip of 9.6 mm x 9.6 mm x 0.4 mm wag bonded by a silver paste to a lead frame made of copper and having a silver plating with a thickness of 150 mm applied. Then, by using each sealing material for semiconductors, sealing was carried out by means of a transfer molding machine under molding conditions of 175°C for 120 seconds, followed by post-curing at a temperature of 175°C for 6 hours to obtain 60 pin QFP (Quad Flat Package) samples of 15 mm x 19 mm x 1.8 mm for evaluation of solder cracking resistance. Then, in each case, ten such samples for evaluation were treated for 72 hours under environmental conditions at 85°C under a relative humidity of 85% and then heated in a solder reflow apparatus at a temperature of 250°C. Then, each sample for evaluation was cut into a half, and the cut surface was polished, whereupon the size of a formed crack was observed by a microscope. A case where the size of the crack is 70 um or more was regarded as “no good”, and the number of “no good” among ten samples was obtained. The results are shown in Table 2. ~~ (3) Spiral flow 8 Using a transfer molding machine having a mold for measuring spiral flow attached thereto in accordance with
EMMI-I-66 (Epoxy Molding Material Institute; Society of
Plastic Industry), the spiral flow value of the sealing material for semiconductors was measured, The transfer molding conditions were such that the mold temperature was 175°C, the molding pressure was 7.4 MPa and the holding time was 120 seconds. The larger the spiral flow : value, the better the fluidity.
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As is apparent from the comparison between Examples and Comparative Examples, according to the silica powder of the present invention, it is possible to prepare a resin composition, particularly a sealing material for semiconductors, which is excellent in flexural strength and solder cracking resistance, as compared with
Comparative Examples.
The silica powder of the present invention is useful for a sealing material for semiconductors to be used for e.g. automobiles, portable electronic equipments, personal computers, household electric products, etc., : for a laminated plate for mounting semiconductors, and as a filler for e.g. patty, sealing materials, various . rubbers, various engineering plastics, etc. Further, the resin composition of the present invention is useful for, in addition to a sealing material for semiconductors, prepregs for printed boards obtained by impregnating and curing it in glass woven fabric, glass nonwoven fabric or other organic material, or various engineering plastics.
The entire disclosure of Japanese Patent Application
No. 2008-018973 filed on January 30, 2008 including specification, claims and summary is incorporated herein by reference in its entirety.
Claims (11)
1. A silica powder characterized in that it has a ~ Freundlich adsorption constant K of pyridine of from 1.3 to 5.0. )
2. The silica powder according to Claim 1, wherein the total of contents (as calculated as oxides) of Si0;, Al.0, and B;0; is at least 99.5 mass%, and the total of contents of Al.0; and B,0; ig from 0.1 to 20 massed.
3. The silica powder accoxding to Claim 1 or 2, which 1c has a specific surface area of from 0.5 to 5m /g and an average particle size of from 1 to 60 pm.
4. An inorganic powder characterized in that it contains the silica powder as defined in any one of Claims 1 to 3.
5. The inorganic powder according to Claim 4, wherein the inorganic powder is a silica powder and/or an alumina powder.
6. A process for producing the silica powder as defined in any one of Claims 1 to 3, characterized in that at least two burners are disposed in a furnace body with an angle of from 2 to 10° to the central axis of the furnace body, and from one burner, a raw material =ilica powder is sprayed and from at least one burner, an aluminum source material and/or a boron source material is sprayed, into a flame,
7. The process for producing the silica powder according to Claim 6, wherein the aluminum scurce material is an aluminum oxide powder, and the raw material silica powder has an Al,0; content of at most 1 mass%. :
8. The process for producing the silica powder Co 5 according to Claim 7, wherein the aluminum oxide powder has an average particle size of from 0.01 to 10 um.
9. A resin composition characterized in that it contains the silica powder as defined in any one of : Claims 1 to 3 or the inorganic powder as defined in Claim 4 or 5.
1¢. The resin composition according to Claim 9, wherein the resin in the resin composition is an epoxy resin.
11. A sealing material for semiconductors, employing the resin composition as defined in Claim 9 or 10.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008018973 | 2008-01-30 |
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| JP (1) | JP5606740B2 (en) |
| KR (1) | KR101442034B1 (en) |
| CN (1) | CN101925534B (en) |
| MY (1) | MY158423A (en) |
| SG (1) | SG188093A1 (en) |
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| JP5968137B2 (en) * | 2012-07-20 | 2016-08-10 | ナミックス株式会社 | Liquid encapsulant and electronic parts using it |
| JP7112179B2 (en) * | 2016-10-19 | 2022-08-03 | 日鉄ケミカル＆マテリアル株式会社 | Spherical siliceous powder for semiconductor encapsulant and method for producing the same |
| CN110040735A (en) * | 2019-04-01 | 2019-07-23 | 成亚资源科技股份有限公司 | The silica regeneration method of discarded package material |
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| JP3501631B2 (en) * | 1997-08-25 | 2004-03-02 | 電気化学工業株式会社 | Method and apparatus for producing inorganic spherical particles |
| JP3608968B2 (en) * | 1999-02-08 | 2005-01-12 | 電気化学工業株式会社 | Method for producing spherical inorganic particles |
| JP4428490B2 (en) * | 2000-01-11 | 2010-03-10 | 電気化学工業株式会社 | Method for producing spherical alumina powder |
| JP4815209B2 (en) * | 2005-03-17 | 2011-11-16 | 株式会社アドマテックス | Curing agent and resin composition |
| TWI412506B (en) * | 2006-05-12 | 2013-10-21 | Denki Kagaku Kogyo Kk | Ceramic powder and uses thereof |
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- 2009-01-23 JP JP2009551501A patent/JP5606740B2/en active Active
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| JPWO2009096343A1 (en) | 2011-05-26 |
| WO2009096343A1 (en) | 2009-08-06 |
| TWI457281B (en) | 2014-10-21 |
| TW200936500A (en) | 2009-09-01 |
| KR101442034B1 (en) | 2014-09-18 |
| JP5606740B2 (en) | 2014-10-15 |
| MY158423A (en) | 2016-10-14 |
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