TWI589669B - 接合用組成物 - Google Patents
接合用組成物 Download PDFInfo
- Publication number
- TWI589669B TWI589669B TW102136594A TW102136594A TWI589669B TW I589669 B TWI589669 B TW I589669B TW 102136594 A TW102136594 A TW 102136594A TW 102136594 A TW102136594 A TW 102136594A TW I589669 B TWI589669 B TW I589669B
- Authority
- TW
- Taiwan
- Prior art keywords
- inorganic metal
- bonding
- metal particles
- particles
- present
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims description 103
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- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- 229940041616 menthol Drugs 0.000 description 1
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- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 229930003658 monoterpene Natural products 0.000 description 1
- 150000002773 monoterpene derivatives Chemical class 0.000 description 1
- 235000002577 monoterpenes Nutrition 0.000 description 1
- AFFLGGQVNFXPEV-UHFFFAOYSA-N n-decene Natural products CCCCCCCCC=C AFFLGGQVNFXPEV-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
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- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 229940038384 octadecane Drugs 0.000 description 1
- 239000007968 orange flavor Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- MUMZUERVLWJKNR-UHFFFAOYSA-N oxoplatinum Chemical compound [Pt]=O MUMZUERVLWJKNR-UHFFFAOYSA-N 0.000 description 1
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- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
- JQPTYAILLJKUCY-UHFFFAOYSA-N palladium(ii) oxide Chemical compound [O-2].[Pd+2] JQPTYAILLJKUCY-UHFFFAOYSA-N 0.000 description 1
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- 229930006728 pinane Natural products 0.000 description 1
- LCYXQUJDODZYIJ-UHFFFAOYSA-N pinocarveol Chemical compound C1C2C(C)(C)C1CC(O)C2=C LCYXQUJDODZYIJ-UHFFFAOYSA-N 0.000 description 1
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- 239000001739 pinus spp. Substances 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
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- 150000003057 platinum Chemical class 0.000 description 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 1
- 229910003446 platinum oxide Inorganic materials 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
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- 229920001225 polyester resin Polymers 0.000 description 1
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- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
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- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- KVMLCRQYXDYXDX-UHFFFAOYSA-M potassium;chloride;hydrochloride Chemical compound Cl.[Cl-].[K+] KVMLCRQYXDYXDX-UHFFFAOYSA-M 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- XOJVVFBFDXDTEG-UHFFFAOYSA-N pristane Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(C)C XOJVVFBFDXDTEG-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- KKKDGYXNGYJJRX-UHFFFAOYSA-M silver nitrite Chemical compound [Ag+].[O-]N=O KKKDGYXNGYJJRX-UHFFFAOYSA-M 0.000 description 1
- XNGYKPINNDWGGF-UHFFFAOYSA-L silver oxalate Chemical compound [Ag+].[Ag+].[O-]C(=O)C([O-])=O XNGYKPINNDWGGF-UHFFFAOYSA-L 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 229910000367 silver sulfate Inorganic materials 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- FTNNQMMAOFBTNJ-UHFFFAOYSA-M silver;formate Chemical compound [Ag+].[O-]C=O FTNNQMMAOFBTNJ-UHFFFAOYSA-M 0.000 description 1
- 238000000235 small-angle X-ray scattering Methods 0.000 description 1
- SDKPSXWGRWWLKR-UHFFFAOYSA-M sodium;9,10-dioxoanthracene-1-sulfonate Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)[O-] SDKPSXWGRWWLKR-UHFFFAOYSA-M 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
- 235000015523 tannic acid Nutrition 0.000 description 1
- 229920002258 tannic acid Polymers 0.000 description 1
- 229940033123 tannic acid Drugs 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001029 thermal curing Methods 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- YFCZLXRIKFCQFU-BUHFOSPRSA-N tianshic acid Chemical compound CCCCCCC(O)C(O)\C=C\C(O)CCCCCCC(O)=O YFCZLXRIKFCQFU-BUHFOSPRSA-N 0.000 description 1
- YFCZLXRIKFCQFU-IKGGRYGDSA-N tianshic acid Natural products CCCCCC[C@H](O)[C@@H](O)C=C/[C@H](O)CCCCCCC(=O)O YFCZLXRIKFCQFU-IKGGRYGDSA-N 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
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- AQWHMKSIVLSRNY-UHFFFAOYSA-N trans-Octadec-5-ensaeure Natural products CCCCCCCCCCCCC=CCCCC(O)=O AQWHMKSIVLSRNY-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 description 1
- 229940036248 turpentine Drugs 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3013—Au as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic Table
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- General Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Materials Engineering (AREA)
- Power Engineering (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Conductive Materials (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
本發明係關於一種接合用組成物,包含無機粒子以及附著於無機粒子的至少一部分表面的有機成分。
為了將金屬零件與金屬零件以機械性及/或電性及或熱性地接合,自以往使用焊料、導電性黏著劑、銀糊劑及異向導電性膜等。此等導電性黏著劑、銀糊劑及異向導電性膜等,不僅使用於金屬零件,有時也會使用於將陶瓷零件或樹脂零件等予以接合的情況。例如:將LED等發光元件接合於基板、將半導體晶片接合於基板、及在該等基板更進一步接合散熱構件等。
其中,焊料與包含由金屬構成之導電填料的黏著劑、糊劑及膜,使用在須要電連接的部分的接合。再者,金屬一般而言熱傳導性高,所以有時此等焊料及包含導電填料之黏著劑、糊劑及膜,也會用於提高散熱性。
另一方面,例如當使用LED等發光元件製作高亮度之照明裝置或發光裝置時,或使用稱為功率裝置之在高溫以高效率動作之半導體元件製作半導體裝置時等,會有發熱量提高的傾向。已有人嘗試提高裝置或元件的效率而減少發熱,但現狀為尚未有充足的成果,實情為裝置或元件的使用溫度會上升。
又,從防止在接合時造成裝置損傷之觀點,尋求能於低接合溫度(例如300℃以下)確保充分接合強度的接合材。因此對於為了將裝置或元件等接合之接合材要求能降低接合溫度且同時耐受接合後裝置動作所致之使用溫度上昇的足夠接合強度的耐熱性,但自以往的接合材常無法充分地應付。例如:焊料經過將金屬加熱到熔點以上的步驟(回焊(reflow)步驟)而將構件彼此接合,但一般而言熔點係其組成固有,所以若欲提高耐熱溫度,加熱(接合)溫度也會升高。
而且,當使用焊料重疊數層元件或基板進行接合時,須要經過相應於重疊層之數目的加熱步驟,為了防止已接合部分熔融,須要降低其次接合使用之焊料之熔點(接合溫度),而且須要有相應於重疊層數目的焊料組成種類,操作變得煩雜。
另一方面,導電性黏著劑、銀糊劑及異向導電性膜係利用含有之環氧樹脂等的熱硬化而將構件彼此接合,但是若獲得之裝置或元件之使用溫度上升,樹脂成分會有分解、劣化的情況。例如:專利文獻1(日本特開2008-63688號公報)提出將微粒作為接合材之主材,使被接合構件彼此接合時獲得更高接合強度,但是仍未解決使用溫度上昇時樹脂成分分解、劣化的問題。
又,於高使用溫度使用之高溫焊料,自以往係使用含鉛的焊料。鉛有毒性,所以焊料往無鉛化的趨勢顯著。高溫焊料不存在其他良好的代替材料,所以仍舊是使用鉛焊料,但從環境問題之觀點,迫切需要不使用鉛的接合材。
近年來,已開發出使用銀、金等貴金屬為中心之金屬奈米粒子的接合材作為高溫焊料的代替材料(例如日本特開2012-046779)。但是為了使用金屬奈米粒子達成接合,須於300~350℃之鈍性氣體環境下實施加壓接合,會有要克服接合溫度下降及無加壓化的課題。
【先前技術文獻】
【專利文獻】
【專利文獻1】日本特開2008-63688號公報
【專利文獻2】日本特開2012-046779號公報
有鑑於如以上的狀況,本發明之目的在於提供一種接合用組成物,尤其含金屬粒子之接合用組成物,能於較低溫且於無加壓之接合獲得高接合強度,而且具備不易發生使用溫度上昇時之樹脂成分分解、劣化等所致之接合強度下降的耐熱性。
本案發明人為了達成上述目的,針對接合用組成物的組成努力研究,結果發現含有無機金屬粒子與附著於無機金屬粒子之至少部分表面的有機成分且將該有機成分予以最適化,在達成上述目的方面極為有效,乃完成本發明。
亦即本發明提供一種接合用組成物,含有:無機金屬粒子、與含不飽和烴及碳數為4~7之胺之有機成分。
構成本發明之接合用組成物的無機金屬粒子的粒徑,宜為可產生熔點下降的奈米尺寸,理想為1~200nm,但視需要也可添加微米尺寸之粒子。於此情形,藉由奈米尺寸之粒子在微米尺寸之粒子的周圍發生熔點下降,可達成接合。
為了將顯示熔點下降能力之奈米尺寸之無機金屬粒子安定地保存,必須在無機金屬粒子的表面有某程度量的有機成分,本發明的有機成分包括不飽和烴及碳數4~7之胺。
亦即,本發明之接合用組成物中係將碳數4~7之胺當作所謂的分散劑。藉由碳鏈數相對較少之低沸點胺,可獲得低溫煅燒型之無機金屬粒子。惟,本發明之接合用組成物也可含有碳數4~7之胺以外的其他的胺。無機金屬粒子合成時之組成莫耳比,於令金屬之鹽為1時,可於碳數4~7之胺為0.001~30之範圍內任意選擇,較佳為0.005~20,又更佳為0.01~10。
有機成分中的不飽和烴具有雙鍵,利用該立體結構能夠提高無機金屬粒子對於有機溶劑的分散性,有抑制無機金屬粒子彼此凝聚之效果。又,上述胺其官能基以適度的強度吸附在無機金屬粒子的表面,妨礙無機金屬粒子彼此相互接觸,故有助於無機金屬粒子在保存狀態的安定性。又,據認為:由於在接合溫度,從無機金屬粒子的表面移動及或揮發,會促進無機金屬粒子彼此融接或無機金屬粒子與基材間的接合。
前述不飽和烴宜有羥基較佳。羥基或羧基容易配位在無機金屬粒子表面,可提高該無機金屬粒子彼此之凝聚抑制效果。又,藉由使疏水基與親水基共存,亦有使接合用組成物與接合基材間的透濕性大舉提高的效果存在。又,官能基不限於羥基,也可為羧基等。
前述不飽和烴宜為蓖麻油酸(ricinoleic acid)較佳。蓖麻油酸具有羧基與羥基,據認為有吸附在無機金屬粒子表面而使該無機金屬粒子均勻分散的效果,及促進無機金屬粒子融接的效果。有機物揮發須要熱與氧,在無機金屬粒子表面的有機物亦同。蓖麻油酸之無機金屬粒子燒結促進效果,據認為係羧基及羥基之氧促進附著於無機金屬粒子表面之有機物之揮發.分解的原故。
又,蓖麻油酸在200℃附近開始分解,所以含蓖麻油酸之有機成分之熱重量減少與粒子之燒結收縮會於良好的時點進行且達成無加壓接合。其結果,可獲得殘留有機成分少的緻密接合層,能於200℃的大氣中以無加壓形成有充足強度的接合部。
蓖麻油酸,可於無機金屬粒子合成時添加作為被覆該無機金屬粒子表面用的分散劑,也可以於無機金屬粒子精製後加入作為添加劑。作為無機金屬粒子合成時之組成莫耳比,令金屬之鹽為1時,不飽和烴可於0.001~10之範圍內任意選擇,較佳為0.005~5,更佳為0.01~3。無機金屬粒子精製後添加時之重量比,可於無機金屬粒子(包括被覆表面之有機物)/不飽和烴=99/1~50/50的範圍內任意選擇,較佳為98/2~70/30,更佳為97/3~75/25。
在此,例如假定將本發明之接合用組成物塗佈於例如在表面施有鍍金之氧化鋁性陶瓷基板,從上方載置相同基板,並將獲得的疊層體於300℃加熱的情況。因加熱使得接合用組成物的溫度逐漸上升時,在到達200℃為止,較易揮發的有機成分會揮發。於此階段仍有相當量的有機成分殘存,無機金屬粒子彼此尚未積極地融接,已塗佈之狀態之接合用組成物仍舊有可撓性。所以,即便有機成分變成氣體揮發後,該氣體通過的路徑出現如空洞之部分(通道),周圍的接合用組成物仍會移動並填埋該部分。並且已融接的無機金屬粒子連結成為一體,可獲得充足的接合強度,是以導電性或熱傳導性也提高。
此外,本發明之接合用組成物中,碳數4~7之胺其一分子內中的胺基具有較高極性且易發生因氫鍵所致之相互作用,但此等官能基以外的部分具有較低極性。再者,胺基各自易顯現鹼性性質。因此碳數4~7之胺,在本發明之接合用組成物中若局部存在(附著於)無機金屬粒子的至少部分表面(亦即,被覆無機金屬粒子的至少部分表面),能使有機成分與無機金屬粒子充分地親和,防止無機金屬粒子彼此凝聚。
又,於視需要添加分散媒的情形,由於有機成分有分散劑之作用,故分散媒中之無機金屬粒子之分散狀態顯著提升。亦即依本發明之接合用組成物,由於含有特定組合的有機物,故無機金屬粒子不容易凝聚,塗膜中之無機金屬粒子之分散性良好,可均勻融接而獲得強接合強度。
在此,本發明之接合用組成物換言之係以無機金屬粒子與有機成分構成之膠體粒子作為主成分之組成物,但也可為更含有分散媒之膠體分散液。「分散媒」係使上述膠體粒子分散於分散液中者,上述膠體粒子之一部分構成成分也可溶於「分散媒」。又,「主成分」,係指構成成分當中含量最多的成分。
又,本發明之接合用組成物中,前述無機金屬粒子宜為金、銀、銅、鎳、鉍、錫或鉑族元素中至少1種金屬之粒子較佳。若使用如此構成之接合用組成物,可獲得優良的接合強度或耐熱性。又,上述本發明之接合用組成物宜用在金屬彼此接合較佳。
依照本發明能夠提供一種接合用組成物,其含有無機金屬粒子與附著於無機金屬粒子之至少部分表面的有機成分,且藉由將該有機成分最適化,於低接合溫度即使無加壓也能獲得高接合強度。
以下針對本發明之接合用組成物之一理想實施形態詳細說明。又,以下說明只不過是提示本發明之一實施形態,本發明並非限定於此等實施形態,又,有時將重複說明省略。
(1)接合用組成物
本實施形態之接合用組成物,特徵為含有:無機金屬粒子、及含有不飽和烴及碳數4~7之胺之有機成分。以下針對此等各成分說明。
(1-1)針對無機金屬粒子
本實施形態之接合用組成物之無機金屬粒子不特別限定,為了使得使用本實施形態之接合用組成物獲得之黏著層之導電性能為良好,宜使用比鋅的游離化傾向小的(貴)金屬為較佳。
該金屬,例如金、銀、銅、鎳、鉍、錫、鐵及鉑族元素(釕、銠、鈀、鋨、銥及鉑)中之至少1種。上述金屬,宜為選自於由金、銀、銅、鎳、鉍、錫或鉑族元素構成之群組中之至少1種金屬之粒子較佳,更佳為銅或比銅的游離傾向更小的(貴)金屬亦即金、鉑、銀及銅中至少1種較佳。該等金屬可以單獨使用也可併用2種以上,併用方法,有使用含多數金屬之合金粒子的情形、或使用具有核-殼結構或多層結構之金屬粒子的情形。
例如:使用銀粒子作為上述接合用組成物之無機金屬粒子時,使用本實施形態之接合用組成物所形成之黏著層的導電率良好,但考慮遷移(migration)的問題,藉由使用由銀與其他金屬構成之接合用組成物,能使遷移不易發生。該「其他金屬」,宜為上述游離化順位比氫更貴的金屬,亦即金、銅、鉑、鈀為較佳。
本實施形態之接合用組成物中,無機金屬粒子(或無機金屬膠體粒子)之平均粒徑,只要是不損及本發明效果之範圍內即無特別限制,宜為具有發生熔點下降之平均粒徑者較理想,例如:1~200nm。再者,2~100nm較佳。無機金屬粒子之平均粒徑若為1nm以上,可獲得能形成良好黏著層之接合用組成物,無機金屬粒子製造成本不會提高,係實用的。又,若為200nm以下,無機金屬粒子之分散性不易隨時間變化,較理想。
又,視需要也可添加併用微米尺寸之無機金屬粒子。於如此的情形,藉由使奈米尺寸之無機金屬粒子於微米尺寸之無機金屬粒子周圍發生熔點下降,能夠接合。
又,本實施形態之接合用組成物中,無機金屬粒子之粒徑不限於固定。又,接合用組成物有時會含有後述分散媒、樹脂成分、有機溶劑、增黏劑
或表面張力調整劑等作為任意成分、含有平均粒徑超過200nm之無機金屬膠體粒子成分,但只要是不發生凝聚、不顯著損害本發明效果的成分,可含有平均粒徑超過200nm之粒子成分。
在此,本實施形態之接合用組成物(金屬膠體分散液)中,無機金屬粒子之粒徑可利用動態光散射法、小角X射線散射法、廣角X射線繞射法測定。為了顯現奈米尺寸之金屬粒子之熔點下降,以廣角X射線繞射法求得之結晶直徑為適當。例如廣角X射線繞射法中,更具體而言,可使用理學電機(股)製RINT-UltimaIII,以繞射法於2θ為30~80°之範圍測定。於此情形,將試樣薄薄地擴開在中央部有約深0.1~1mm之凹洞的玻璃板使得表面成為平坦後測定即可。又,使用理學電機(股)製JADE,將獲得之繞射光譜之半值寬代入下列Scherrer式,將算出的結晶直徑(D)作為粒徑即可。
D=Kλ/Bcosθ
在此,K:Scherrer常數(0.9)、λ:X射線之波長、B:繞射線之半值寬、θ:布拉格角(Bragg angle)。
(1-2)附著於無機金屬粒子之至少部分表面的有機成分
本實施形態之接合用組成物中,附著於無機金屬粒子之至少部分表面的有機成分,亦即無機金屬膠體粒子中之「有機成分」,係作為所謂分散劑,與上述無機金屬粒子一同構成實質上的無機金屬膠體粒子。該有機成分,概念上不包括在金屬中起先含有作為雜質的微量有機物、於後述製造過程混入而附著於金屬成分之微量有機物、於洗滌過程未完全除去的殘留還原劑、殘留分散劑等般於無機金屬粒子微量附著的有機物等。又,上述「微量」,具體而言,係指在金屬膠體粒子中少於1質量%。
上述有機成分,係被覆無機金屬粒子並防止該無機金屬粒子凝聚且同時能形成無機金屬膠體粒子之有機物,針對被覆形態無特別規定,但本實施形態中,從分散性及導電性等觀點,包括不飽和烴及碳數4~7之胺。又,該等有機成分,據認為於與無機金屬粒子係化學性或物理性結合時會變化為陰離子或陽離子,本實施形態中,來自該等有機成分之離子或錯合物等
也包括於上述有機成分。
作為碳數4~7之胺,只要是碳數4~7即可,可為直鏈狀也可為分支鏈狀,又,也可有側鏈。例如:丁胺、戊胺、己胺、己胺等烷胺(直鏈狀烷胺,也可有側鏈)、環戊胺、環己胺等環烷胺、苯胺等烯丙胺等一級胺、二丙胺、二丁胺、哌啶、六亞甲基亞胺等二級胺、三丙胺、二甲基丙烷二胺、環己基二甲胺、吡啶、喹啉等三級胺等。
上述碳數4~7之胺,可為包括例如:羥基、羧基、烷氧基、羰基、酯基、巰基等胺以外之官能基的化合物。於此情形,官能基中之碳數不包括在「碳數4~7之胺」之碳數。又,來自胺之氮原子之數目,宜為胺以外之官能基之數目以上較佳。又,上述胺可以分別單獨使用,也可併用2種以上。此外,於常溫之沸點宜為300℃以下,更佳為250℃以下。
本實施形態之接合用組成物,只要是不損及本發明效果之範圍內,除了上述碳數4~7之胺,也可含羧酸。於羧酸一分子內之羧基,具有較高極性且容易發生因氫鍵所致之相互作用,但此等官能基以外之部分具有較低極性。又,羧基容易顯現酸性性質。又,羧酸在本實施形態之接合用組成物中若局部存在(附著於)無機金屬粒子之至少部分表面(亦即,被覆無機金屬粒子之至少部分表面),能使有機成分與無機金屬粒子充分地親和,防止無機金屬粒子彼此凝聚(使分散性提高)。
羧酸可泛稱具有至少1個羧基的化合物,例如:甲酸、草酸、乙酸、己酸、丙烯酸、辛酸、油酸等。羧酸的部分羧基也可與金屬離子形成鹽。又,針對該金屬離子,可含有2種以上的金屬離子。
上述羧酸,可為含有例如胺基、羥基、烷氧基、羰基、酯基、巰基等羧基以外之官能基之化合物。於此情形,羧基之數目宜為羧基以外之官能基之數目以上較佳。又,上述羧酸可分別單獨使用也可併用2種以上。此外,於常溫的沸點為300℃以下,更佳為250℃以下。又,胺與羧酸會形成醯胺。
該醯胺基也會適度地吸附在銀粒子表面,所以有機成分中也可含有醯胺基。
本實施形態之接合用組成物中,金屬膠體中之有機成分之含量宜為0.5~50質量%較佳。有機成分含量若為0.5質量%以上,獲得之接合用組成物之貯藏安定性有變得良好的傾向,若為50質量%以下,接合用組成物之導電性有良好的傾向。有機成分的更理想含量為1~30質量%,更理想含量為2~15質量%。
併用胺與羧酸時之組成比(質量),可於1/99~99/1之範圍任意選擇,較佳為20/80~98/2,又更佳為30/70~97/3。又,胺或羧酸可分別使用多種胺或羧酸。
本實施形態之接合用組成物所含之不飽和烴,例如:乙烯、乙炔、苯、丙酮、1-己烯、1-辛烯、4-乙烯基環己烯、環己酮、萜烯系醇、烯丙醇、油醇、2-棕櫚油酸(2-Palmitoleic acid)、岩芹酸(petroselinic acid)、油酸、反油酸(elaidic acid)、天師酸(Tianshic acid)、蓖麻油酸、亞油酸(Linoleic acid)、反亞油酸(Linoelaidic Acid)、亞麻酸(Linolenic acid)、花生四烯酸、丙烯酸、甲基丙烯酸、没食子酸及水楊酸等。
該等之中,具有羥基之不飽和烴為較佳。羥基易配位在無機金屬粒子表面,能抑制該無機金屬粒子凝聚。具有羥基之不飽和烴,例如:萜烯系醇、烯丙醇、油醇、天師酸、蓖麻油酸、没食子酸及水楊酸等。較佳為具有羥基之不飽和脂肪酸,例如:天師酸、蓖麻油酸、没食子酸及水楊酸等。
前述不飽和烴為蓖麻油酸較佳。蓖麻油酸具有羧基與羥基,能吸附於無機金屬粒子表面而使該無機金屬粒子均勻分散,且同時促進無機金屬粒子融接。
本實施形態之接合用組成物中,除了上述成分,在無損本發明效果之範圍,為了因應使用目的賦予適度黏性、密合性、乾燥性或印刷性等機能,
也可添加分散媒、或作為例如黏結劑之作用的寡聚物成分、樹脂成分、有機溶劑(可溶解或分散一部分固體成分)、界面活性劑、增黏劑或表面張力調整劑等任意成分。該任意成分不特別限定。
作為任意成分中之分散媒,在不損及本發明效果之範圍可使用各種分散媒,例如烴及醇等。
烴可列舉脂肪族烴、環狀烴及脂環族烴等,可分別單獨使用也可併用2種以上。
作為脂肪族烴,例如:十四烷、十八烷、七甲基壬烷、四甲基十五烷、己烷、庚烷、辛烷、壬烷、癸烷、十三烷、甲基戊烷、正鏈烷烴(normal paraffin)、異鏈烷烴(isoparaffin)等飽和或不飽和脂肪族烴。
環狀烴,例如:甲苯、二甲苯等。
又,作為脂環族烴,例如:檸檬烯(limonene)、雙戊烯(dipentene)、松油烯(terpinene)、松油烯(亦稱為terpinene)、松油烯(nesol)、松油烯(cinene)、橙香料(orange flavor)、品油烯(terpinolene)、品油烯(亦稱為terpinolene)、水芹烯(phellandrene)、薄荷二烯(menthadiene)、芸香烯(terebene)、二氫-異丙基甲苯(dihydro-cymene)、海茴香烯(moslene)、異松油烯(iso-terpinene)、異松油烯(亦稱為iso-terpinene)、海茴香烯(crithmene)、檸檬烯(kautschin)、檸檬烯(cajeputene)、檸檬烯(eulimen)、蒎烯(pinene)、松節油(turpentine)、薄荷烷(menthane)、蒎烷(pinane)、萜烯(terpene)、環己烷(cyclohexane)等。
另,醇類係於分子結構中含1個以上OH基之化合物,可列舉出脂肪族醇類、環狀醇類及脂環式醇類,係可各別單獨使用,亦可合併2種以上使用。另,部分OH基在不影響本發明效果範圍內亦可將其衍生成乙醯氧基等。
脂肪族醇類可列舉出庚醇(heptanol)、辛醇(octanol)(1-辛醇、2-辛醇、3-
辛醇等)、癸醇(decanol)(1-癸醇等)、月桂醇(lauryl alcohol)、十四醇(tetradecyl alcohol)、鯨蠟醇(cetyl alcohol)、2-乙基-1-己醇(2-ethyl-1-hexanol)、十八醇(octadecyl alcohol)、十六烯醇、油醇(oleyl alcohol)等飽和或不飽和C6-30脂肪族醇類。
作為環狀醇類可列舉出甲酚、丁香油酚等。
再者,脂環族醇類可列舉出環己醇等環烷醇(cycloalkanol)、松油醇(terpineol)(包含α、β、γ同分異構體或該等之任意之混合物)、二氫松油醇(dihydroterpineol)等萜品醇(terpene alcohol)(單萜醇(monoterpene alcohol)等)、二氫松油醇、桃金娘烯醇(myrtenol)、索布瑞醇(sobrerol)、薄荷醇(menthol)、香芹醇(carveol)、紫蘇子醇(perillyl alcohol)、松香芹醇(pinocarveol)、索布瑞醇(sobrerol)、馬鞭草烯醇(verbenol)等。
本實施形態之接合用組成物中含有分散媒時之含量,可依黏度等所望特性調整即可,接合用組成物中之分散媒之含量宜為1~30質量%較佳。分散媒之含量若為1~30質量%,能獲得在容易使用接合性組成物之範圍調整黏度調整之效果。分散媒之更理想含量為1~20質量%,又更理想含量為1~15質量%。
樹脂成分,例如:聚酯系樹脂、封端化異氰酸酯等聚胺甲酸酯系樹脂、聚丙烯酸酯系樹脂、聚丙烯醯胺系樹脂、聚醚系樹脂、三聚氰胺系樹脂或萜烯系樹脂等,此等可以單獨使用也可併用2種以上。
有機溶劑除了上述就分散媒列舉者以外,例如:甲醇、乙醇、正丙醇、2-丙醇、1,3-丙二醇、1,2-丙二醇、1,4-丁二醇、1,2,6-己三醇、1-乙氧基-2-丙醇、2-丁氧基乙醇、乙二醇、二乙二醇、三乙二醇、重量平均分子量為200以上1,000以下之範圍內的聚乙二醇、丙二醇、二丙二醇、三丙二醇、重量平均分子量為300以上1,000以下之範圍內的聚丙二醇、N,N-二甲基甲醯胺、二甲基亞碸、N-甲基-2-吡咯烷酮、N,N-二甲基乙醯胺、甘油或丙酮,此等
可以單獨使用也可併用2種以上。
增黏劑可列舉出黏土(clay)、膨土(bentonite)或鋰皂土(hectorite)等黏土礦物;聚酯類乳化樹脂、丙烯酸系乳化樹脂、聚胺基甲酸酯類乳化樹脂或封端異氰酸酯等乳劑;甲基纖維素(methyl cellulose)、羧甲基纖維素(carboxymethylcellulose)、羥乙基纖維素(hydroxyethyl cellulose)、羥丙纖維素(hydroxypropyl cellulose)、羥丙基甲基纖維素(hydroxypropyl methyl cellulose)等纖維素衍生物;黃原膠(xanthan gum)或瓜爾膠(guar gum)等多醣類等;該些係可各別單獨使用,亦可合併2種以上使用。
亦可添加與該有機物不同之界面活性劑。多成分溶媒類金屬膠體分散液係因乾燥時揮發速度之差異導致易產生塗膜表面粗糙及固體成分不均勻而集中。於本實施形態接合用組成物添加界面活性劑可藉此抑制該些缺失,並可取得能形成均勻導電被膜之接合用組成物。
本實施形態所使用之界面活性劑並無特別之限制,係可使用陰離子界面活性劑、陽離子界面活性劑、非離子界面活性劑之任一種,可列舉出烷基苯磺酸鹽(alkyl benzene sulfonate)、四級銨鹽(quaternary ammonium)等。氟類界面活性劑以少量之添加量便可發揮效果因此較佳。
又,將有機成分量調整為既定範圍之方法將於後述,進行加熱以調整係簡便。又,也可藉由調整在製作無機金屬粒子時添加的有機成分的量以進行,也可改變製備無機金屬粒子後之洗滌條件或次數。加熱可以用烘箱或蒸發器等進行,也可於減壓下進行。於常壓下進行時,可於大氣中也可於鈍性氣體環境中進行。再者,為了進行有機成分量的微調整,上述胺(及羧酸)也可於之後添加。
本實施形態之接合用組成物中,含有後述無機金屬粒子膠體化而得之無機金屬膠體粒子作為主成分,關於該無機金屬膠體粒子之形態可列舉例如:在無機金屬粒子的部分表面附著有機成分而構成之無機金屬膠體粒子、
將上述無機金屬粒子作為核並將其表面以有機成分被覆而構成之無機金屬膠體粒子、此等混雜而構成之無機金屬膠體粒子等,不特別限定。其中,宜為將無機金屬粒子作為核並於其表面被覆有機成分而構成之無機金屬膠體粒子較佳。該技術領域中具有通常知識者可使用該領域中之公知技術適當製備具有上述形態之無機金屬膠體粒子。
本實施形態之接合用組成物,係將無機金屬粒子及由有機成分構成之膠體粒子作為主成分之流動體,除了無機金屬粒子、構成無機金屬膠體粒子之有機成分以外,也可含有未構成無機金屬膠體粒子之有機成分、分散媒或殘留還原劑等。
本實施形態之接合用組成物之黏度、固體成分之濃度可在不損及本發明效果之範圍內適當調整,例如可為0.01~5000Pa.S之黏度範圍,0.1~1000Pa.S之黏度範圍更佳,1~100Pa.S之黏度範圍尤佳。藉由定為該黏度範圍,可以廣泛使用各種方法作為在基材上塗佈接合用組成物的方法。
於基材上塗佈接合用組成物之方法,舉例而言,可從浸泡(dipping)、網印(screen printing)、噴霧式(spray)、棒狀塗佈(bar coating)、旋轉塗佈(spin coating)、噴墨式(inkjet)、分配器(dispenser)、針轉移法(pintransfer)、刷毛等塗佈方式、流動式(flow casting)、柔板印刷式(flexo)、凹版印刷式(gravure)、平板印刷式(offset)、轉印法(transfer)、親/疏水性圖樣法(hydrophilic/hydrophobic pattern)或注射式(syringe)等之中適當挑選。
黏度調整可透過調整無機金屬粒子粒徑、調整有機物含量、調整分散媒或其他成分添加量、調整各成分摻合比或添加增黏劑等加以進行。接合用組成物之黏度係可以用平底錐形黏度計(cone plate viscometer)(如:ANTON-PAAR公司製之RHEOMETER MCR301)進行測量。
(2)接合用組成物之製造
其次,為了製備本實施形態之含有無機金屬膠體而成之接合用組成
物,製備作為主成分之以有機成分被覆之無機金屬粒子(無機金屬膠體粒子)。
又,有機成分量及重量減少率之調整不特別限定,以進行加熱來調整係為簡便。又,也可藉由調整在製作無機金屬粒子時添加的有機成分的量以進行,也可改變製備無機金屬粒子後之洗滌條件或次數。加熱可以用烘箱或蒸發器等進行。加熱溫度於約50~300℃之範圍進行即可,加熱時間可為數分鐘~數小時。加熱也可於減壓下進行。藉由於減壓下加熱,能以更低溫度進行有機物量之調整。於常壓下進行時,可於大氣中也可於鈍性氣體環境中進行。再者,為了進行有機成分量的微調整,胺或羧酸也可於之後添加。
作為製備本實施形態之被覆了有機成分的無機金屬粒子的方法,不特別限定,例如製備含有無機金屬粒子之分散液,然後實施此分散液之洗滌的方法等。在作為製備含無機金屬粒子之分散液之步驟,例如可如下述,使溶於溶劑中之金屬鹽(或金屬離子)還原,還原程序採用基於化學還原法之程序即可。
亦即,如上述被覆了有機成分的無機金屬粒子,可藉由將包含構成無機金屬粒子之金屬之金屬鹽、作為分散劑之有機物、與溶劑(基本上為甲苯等有機系,但也可含水)之原料液(一部分成分也可未溶解而是分散)予以還原以製備。
藉由此還原,可獲得作為分散劑之有機成分附著於無機金屬粒子之至少部分表面的無機金屬膠體粒子。此無機金屬膠體粒子可單獨地供作本實施形態之接合用組成物,但是視需要,也可將其於後述步驟添加到分散媒,而獲得由無機金屬膠體分散液構成的接合用組成物。
作為用以獲得被覆了有機物之無機金屬粒子用的起始材料,可使用各種公知之金屬鹽或其水合物,例如:硝酸銀、硫酸銀、氯化銀、氧化銀、乙
酸銀、草酸銀、甲酸銀、亞硝酸銀、氯酸銀、硫化銀等銀鹽;例如:氯化金酸、氯化金鉀、氯化金鈉等金鹽;例如:氯化鉑酸、氯化鉑、氧化鉑、氯化鉑酸鉀等鉑鹽;例如:硝酸鈀、乙酸鈀、氯化鈀、氧化鈀、硫酸鈀等鈀鹽等,但是只要能溶於適當的分散媒中且能還原者即可,不特別限定。又,此等可以單獨使用也可併用多種。
又,將上述原料液中之該等金屬鹽予以還原的方法不特別限定,例如:使用還原劑之方法、照射紫外線等光、電子束、超音波或熱能量的方法等。其中,從容易操作之觀點,使用還原劑之方法為較佳。
作為上述還原劑,例如:二甲胺基乙醇、甲基二乙醇胺、三乙醇胺、1-苯-3-吡唑啉酮(Phenidone)、聯胺等胺化合物;例如:氫化硼鈉、碘化氫、氫氣等氫化合物;例如:一氧化碳、亞硫酸等氧化物;例如:硫酸鐵(II)、氧化鐵、富馬酸鐵、乳酸鐵、草酸鐵、硫化鐵、乙酸錫、氯化錫、二磷酸錫、草酸錫、氧化錫、硫酸錫等低原子價金屬鹽;例如:乙二醇、甘油、甲醛、氫醌、五倍子酚、單寧、單寧酸、水楊酸、D-葡萄糖等糖等,但只要能溶於分散媒並且將上述金屬鹽還原者即可,不特別限定。使用上述還原劑時,也可照光及/或加熱以促進還原反應。
使用上述金屬鹽、有機成分、溶劑及還原劑製備被覆了有機物之金屬粒子的具體方法,例如:將上述金屬鹽溶於有機溶劑(例如甲苯等)以製備金屬鹽溶液,於該金屬鹽溶液添加作為分散劑之有機物,然後於其中緩慢滴加溶有還原劑之溶液的方法等。
在以上述方式獲得之包含被覆了作為分散劑之有機成分的無機金屬粒子的分散液中,除了無機金屬粒子以外,尚存在金屬鹽之相對離子、還原劑之殘留物或分散劑,液體全體之電解質濃度傾向為高。如此狀態之液體,電導度高,所以會引起無機金屬粒子之凝析且易沉澱。或者即使未沉澱,若金屬鹽之相離子、還原劑之殘留物、或對於分散為必要之量以上之過量分散劑殘留,會有使導電性惡化之虞。而,藉由洗滌上述包含無機金屬粒
子之溶液以去除掉多餘的殘留物,能確實地獲得被覆了有機物的無機金屬粒子。
上述洗滌方法,可列舉例如:將包含被覆了有機成分之無機金屬粒子的分散液靜置一段時間,去除生成的上清液後,加入醇(甲醇等)再度攪拌,並再靜置一段期間,去除生成的上清液,將此等步驟重複多次;將上述靜置替換為離心分離;利用超過濾裝置或離子交換裝置等進行脫鹽的方法等。藉由利用如此的洗滌以去除有機溶劑,能獲得本實施形態之被覆了有機成分之無機金屬粒子。
本實施形態之中,無機金屬膠體分散液,可藉由混合上述獲得之被覆了有機成分之無機金屬粒子及上述本實施形態說明之分散媒以獲得。該被覆了有機成分之無機金屬粒子與分散媒之混合方法不特別限定,可使用攪拌機或攪拌器(stirrer)等依以往公知之方法實施。也可用如刮勺之類的物件攪拌,或適用適當輸出的超音波均質機。
獲得含有多數金屬之無機金屬膠體分散液時,其製造方法不特別限定,例如製造由銀與其他金屬構成之無機金屬膠體分散液的情形,在製備上述被覆了有機物之無機金屬粒子時,可以分別地製造包含無機金屬粒子之分散液與包含其他無機金屬粒子之分散液且之後混合,也可以混合銀離子溶液與其他金屬離子溶液且之後予以還原。
(3)接合方法
若使用本實施形態之接合用組成物,可於伴隨加熱之構件彼此之接合獲得高接合強度。亦即,可藉由如下的步驟,將第1被接合構件與第2被接合構件接合,該等步驟係:接合用組成物塗佈步驟,將上述接合用組成物塗佈於第1被接合構件與第2被接合構件之間;接合步驟,將已塗佈於第1被接合構件與第2被接合構件之間的接合用組成物,於理想的溫度(例如300℃以下,較佳為150~200℃)煅燒並接合。此時也可加壓,尤其即使不加壓仍能獲得足夠接合強度也是本發明之優點之一。又,進行煅燒時,可以分段地將
溫度上升或下降。又,也可在預先在被接合構件表面塗佈界面活性劑或表面活化劑等。
本案發明人努力探討,結果發現若使用上述本實施形態之接合用組成物作為在前述接合用組成物塗佈步驟之接合用組成物,能夠將第1被接合構件與第2被接合構件以高接合強度確實地接合(可獲得接合體)。
在此,本實施形態之接合用組成物之「塗佈」,概念上包括將接合用組成物塗佈為面狀的情況,也包括塗佈為線狀(描繪)的情況。由塗佈後利用加熱煅燒前之狀態之接合用組成物構成之塗膜的形狀,可成為理想形狀。因此利用加熱進行煅燒後之本實施形態之接合體中,接合用組成物在概念上包括面狀之接合層及線狀之接合層中任一者,此等面狀之接合層及線狀之接合層可以連續也可不連續,也可包括連續部分及不連續的部分。
作為在本實施形態可使用的第1被接合構件及第2被接合構件,只要是能塗佈接合用組成物並利用加熱煅燒而接合者即可,不特別限制,宜為具備不會因接合時之溫度而受損之程度之耐熱性的構件較佳。
構成如此之被接合構件之材料,例如:聚醯胺(PA)、聚醯亞胺(PI)、聚醯胺醯亞胺(PAI)、聚對苯二甲酸乙二醇酯(PET)、對苯二甲酸丁二醇酯(PBT)、聚萘二甲酸乙二醇酯(PEN)等聚酯、聚碳酸酯(PC)、聚醚碸(PES)、乙烯基樹脂、氟樹脂、液晶聚合物、陶瓷、玻璃或金屬等,其中金屬製之被接合構件為較佳。金屬製之被接合構件為較佳的原因為:耐熱性優異,而且無機粒子與金屬本發明之接合用組成物間的親和性優異。
又,被接合構件,可為例如板狀或條狀等各種形狀,可為剛性也可為撓性。基材厚度也可適當選擇。為了黏著性或密合性提高或其他目的,可使用形成了表面層的構件或施行了親水化處理等表面處理的構件。
於被接合構件上塗佈接合用組成物之步驟,可使用各種方法,如上述,
舉例而言,可從浸泡(dipping)、網印(screen printing)、噴霧式(spray)、棒狀塗佈(bar coating)、旋轉塗佈(spin coating)、噴墨式(inkjet)、分配器(dispenser)、針轉移法(pintransfer)、刷毛等塗佈方式、流動式(flow casting)、柔板印刷式(flexo)、凹版印刷式(gravure)、或注射式(syringe)等之中適當挑選。
將如上述方式塗佈後之塗膜於不損傷被接合構件的範圍,例如於300℃以下的溫度加熱以煅燒,可獲得本實施形態之接合體。本實施形態中,如前述,係使用本實施形態之接合用組成物,所以可獲得對被接合構件有優良密合性的接合層,能更確實地獲得強接合強度。
本實施形態中,接合用組成物含有黏結劑成分的情形,從提高接合層之強度及提高與被接合構件間之接合強度等觀點,係連黏結劑成分也燒結,但是視情況,也可為了適用於各種印刷法,而將調整接合用組成物之黏度作為黏結劑成分的主要目的,控制煅燒條件以去除全部黏結劑成分。
進行上述煅燒之方法不特別限定,例如可使用以往公知之烘箱等,進行煅燒使得塗佈或描繪在被接合構件上的上述接合用組成物的溫度成為例如300℃以下以進行接合。上述煅燒之溫度下限不一定受限,宜為被接合構件彼此能接合之溫度且不損及本發明效果之範圍之溫度較佳。在此,上述煅燒後接合用組成物中,於儘可能獲得高接合強度的觀點,有機物之殘存量較少為佳,但在無損本發明效果之範圍內,有一部分有機物殘存亦無妨。
又,本發明之接合用組成物中含有有機物,其與以往例如環氧樹脂等利用熱硬化者不同,並非是利用有機物作用而獲得煅燒後之接合強度,而是如前述,利用已融接之無機金屬粒子之融接而獲得充分接合強度者。如此,於接合後即使放在比接合溫度更高溫之使用環境,而發生殘存有機物劣化或分解.消失的情形仍無接合強度下降之虞,因此耐熱性優異。
依本實施形態之接合用組成物,即使在例如約150~200℃之低溫加熱進
行煅燒,也能達成具有展現高導電性之接合層的接合,所以能將較不耐熱的被接合構件彼此接合。又,煅燒時間無特別限定,只要是因應煅燒溫度能接合之煅燒時間即可。
本實施形態中,為了更提高上述被接合構件與接合層間的密合性,也可進行上述被接合構件之表面處理。上述表面處理方法,例如:實施電暈處理、電漿處理、UV處理、電子束處理等乾處理之方法、在基材上預先設置底塗層或導電性糊劑容納層之方法等。
以上已針對本發明之代表實施形態說明,但本發明不僅限定於該等實施形態。例如:上述實施形態中,係針對採用金屬粒子作為無機粒子之無機金屬膠體分散液說明,但也可使用例如:導電性、熱傳導性、介電性、離子傳導性等優異之錫摻雜氧化銦、氧化鋁、鈦酸鋇、鐵磷酸鋰等無機粒子。
以下對於實施例中之本發明之接合用組成物更進一步說明,但本發明不限定於該等實施例。
【實施例】
≪實施例1≫
於甲苯(和光純藥工業(股)製特級)300mL中加入己胺(東京化成工業(股)製EP級)50g,以磁性攪拌器充分攪拌。邊攪拌邊加入硝酸銀(和光純藥工業(股)製特級)10g,於硝酸銀已溶解的時點依序添加油酸(和光純藥工業(股)製一級)10g及己酸(和光純藥工業(股)製特級)5g,製成硝酸銀之甲苯溶液。
充分攪拌並散熱後,於此硝酸銀之甲苯溶液中滴加在離子交換水100mL中添加硼氫化鈉(和光純藥工業(股)製化學用)2g所製成的0.02g/mL的硼氫化鈉水溶液,繼續攪拌1小時,使銀粒子生成。之後,加入甲醇(和光純藥工業(股)製特級)500mL使銀粒子沈降。再以離心分離使銀粒子完全沈降之後,去除上清所含之反應殘渣或溶劑等。
將已去除上清後殘留的含銀粒子的沈降物(未處理銀粒子組成物)使用隔膜泵浦進行數分鐘減壓,使少量殘存的甲醇充分蒸發後,於大氣氣體環境下放入200℃之烘箱20分鐘以進行加熱處理,獲得適量減少了包括己胺、油酸及己酸之有機物之量的銀粒子組成物1。
[接合強度測定]
於5g上述銀粒子組成物1中添加蓖麻油酸(和光純藥工業(股)製化學用)1g,充分攪拌混合以獲得接合用組成物1。將少量該接合用組成物使用黏晶機(die bonder)(HISOL公司製)承載於表面施有鍍金的氧化鋁板(50mm四方),並於其上疊層市售的藍色LED晶片(GENELITE公司製、底面積600μm×600μm)。此時,未施加外力予以加壓。
然後將獲得之疊層體放入調整為200℃的熱風循環族烘箱,於大氣氣體環境下利用120分鐘之加熱實施煅燒處理。取出疊層體並將其冷卻後,於常溫使用接合測試機(bond tester)(RHESCA公司製PTR-1101)進行接合強度試驗(剪切高度:距基板10μm、剪切工具(shear tool)速度:0.01mm/sec)。剝離時之接合強度以晶片之底面積進行換算。評價結果中之數值以MPa表示記載。
≪實施例2≫
未添加蓖麻油酸,除此以外與實施例1同樣地製備接合用組成物2,並進行接合強度測定。結果如表1。
≪實施例3≫
將油酸替換為使用蓖麻油酸,除此以外與實施例1同樣進行,製備接合用組成物3,並實施接合強度測定。結果如表1。
≪實施例4≫
使用蓖麻油酸替代油酸且於獲得之銀粒子組成物未進一步添加蓖麻油酸,除此以外與實施例1同樣地實施,製備接合用組成物4,進行接合強度
測定。結果如表1。
≪比較例1≫
未添加油酸與蓖麻油酸,除此以外與實施例1同樣實施,製備比較接合用組成物1,進行接合強度測定。結果如表1。
≪比較例2≫
將己胺替換為使用十二胺,且之後不添加蓖麻油酸,除此以外與實施例1同樣地進行,製備比較接合用組成物2,並測定接合強度。結果如表1。
≪比較例3≫
將己胺替換為使用油胺且之後不使用蓖麻油酸,除此以外與實施例1同樣地進行,製備比較接合用組成物3,並測定接合強度。結果如表1。
由表1所示結果可得知:本發明之實施例中,接合溫度為200℃之低溫,且僅為利用無加壓實施接合仍顯現約20MPa的高接合強度。另一方面,使用不具備本發明之構成的接合用組成物時,於同樣的接合條件成為極低的接合強度。
Claims (3)
- 一種接合用組成物,含有:無機金屬粒子、及含不飽和烴及沸點300℃以下且碳數4~7之胺之有機成分。
- 如申請專利範圍第1項之接合用組成物,其中,該不飽和烴具有羥基。
- 如申請專利範圍第2項之接合用組成物,其中,該不飽和烴為蓖麻油酸。
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