JP2015082385A - 銀ペースト及びそれを用いた半導体装置、並びに銀ペーストの製造方法 - Google Patents
銀ペースト及びそれを用いた半導体装置、並びに銀ペーストの製造方法 Download PDFInfo
- Publication number
- JP2015082385A JP2015082385A JP2013219283A JP2013219283A JP2015082385A JP 2015082385 A JP2015082385 A JP 2015082385A JP 2013219283 A JP2013219283 A JP 2013219283A JP 2013219283 A JP2013219283 A JP 2013219283A JP 2015082385 A JP2015082385 A JP 2015082385A
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- Prior art keywords
- silver
- paste
- silver paste
- silver particles
- particles
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 304
- 239000004332 silver Substances 0.000 title claims abstract description 304
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 291
- 239000004065 semiconductor Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 106
- 239000002904 solvent Substances 0.000 claims abstract description 38
- 238000009835 boiling Methods 0.000 claims abstract description 37
- 239000003223 protective agent Substances 0.000 claims description 49
- 238000005245 sintering Methods 0.000 claims description 19
- -1 amine compound Chemical class 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 6
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 claims description 6
- DILRJUIACXKSQE-UHFFFAOYSA-N n',n'-dimethylethane-1,2-diamine Chemical compound CN(C)CCN DILRJUIACXKSQE-UHFFFAOYSA-N 0.000 claims description 6
- GVWISOJSERXQBM-UHFFFAOYSA-N n-methylpropan-1-amine Chemical compound CCCNC GVWISOJSERXQBM-UHFFFAOYSA-N 0.000 claims description 6
- JOZZAIIGWFLONA-UHFFFAOYSA-N 3-methylbutan-2-amine Chemical compound CC(C)C(C)N JOZZAIIGWFLONA-UHFFFAOYSA-N 0.000 claims description 4
- QCOGKXLOEWLIDC-UHFFFAOYSA-N N-methylbutylamine Chemical compound CCCCNC QCOGKXLOEWLIDC-UHFFFAOYSA-N 0.000 claims description 4
- KVKFRMCSXWQSNT-UHFFFAOYSA-N n,n'-dimethylethane-1,2-diamine Chemical compound CNCCNC KVKFRMCSXWQSNT-UHFFFAOYSA-N 0.000 claims description 4
- XDIAMRVROCPPBK-UHFFFAOYSA-N 2,2-dimethylpropan-1-amine Chemical compound CC(C)(C)CN XDIAMRVROCPPBK-UHFFFAOYSA-N 0.000 claims description 3
- VJROPLWGFCORRM-UHFFFAOYSA-N 2-methylbutan-1-amine Chemical compound CCC(C)CN VJROPLWGFCORRM-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 3
- BMFVGAAISNGQNM-UHFFFAOYSA-N isopentylamine Chemical compound CC(C)CCN BMFVGAAISNGQNM-UHFFFAOYSA-N 0.000 claims description 3
- KFIGICHILYTCJF-UHFFFAOYSA-N n'-methylethane-1,2-diamine Chemical compound CNCCN KFIGICHILYTCJF-UHFFFAOYSA-N 0.000 claims description 3
- QKYWADPCTHTJHQ-UHFFFAOYSA-N n,2-dimethylpropan-1-amine Chemical compound CNCC(C)C QKYWADPCTHTJHQ-UHFFFAOYSA-N 0.000 claims description 3
- HVOYZOQVDYHUPF-UHFFFAOYSA-N n,n',n'-trimethylethane-1,2-diamine Chemical compound CNCCN(C)C HVOYZOQVDYHUPF-UHFFFAOYSA-N 0.000 claims description 3
- VMOWKUTXPNPTEN-UHFFFAOYSA-N n,n-dimethylpropan-2-amine Chemical compound CC(C)N(C)C VMOWKUTXPNPTEN-UHFFFAOYSA-N 0.000 claims description 3
- GNVRJGIVDSQCOP-UHFFFAOYSA-N n-ethyl-n-methylethanamine Chemical compound CCN(C)CC GNVRJGIVDSQCOP-UHFFFAOYSA-N 0.000 claims description 3
- XCVNDBIXFPGMIW-UHFFFAOYSA-N n-ethylpropan-1-amine Chemical compound CCCNCC XCVNDBIXFPGMIW-UHFFFAOYSA-N 0.000 claims description 3
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical group CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 claims description 3
- IGEIPFLJVCPEKU-UHFFFAOYSA-N pentan-2-amine Chemical compound CCCC(C)N IGEIPFLJVCPEKU-UHFFFAOYSA-N 0.000 claims description 3
- PQPFFKCJENSZKL-UHFFFAOYSA-N pentan-3-amine Chemical compound CCC(N)CC PQPFFKCJENSZKL-UHFFFAOYSA-N 0.000 claims description 3
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 150000001735 carboxylic acids Chemical class 0.000 claims description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 60
- 239000011859 microparticle Substances 0.000 description 38
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- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 19
- 238000010438 heat treatment Methods 0.000 description 19
- 150000003378 silver Chemical class 0.000 description 15
- 239000000654 additive Substances 0.000 description 11
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- 239000010949 copper Substances 0.000 description 8
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- 229920005989 resin Polymers 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
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- 239000004593 Epoxy Substances 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 235000002597 Solanum melongena Nutrition 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- UYXTWWCETRIEDR-UHFFFAOYSA-N Tributyrin Chemical compound CCCC(=O)OCC(OC(=O)CCC)COC(=O)CCC UYXTWWCETRIEDR-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
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- 229940116411 terpineol Drugs 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 description 1
- LAVARTIQQDZFNT-UHFFFAOYSA-N 1-(1-methoxypropan-2-yloxy)propan-2-yl acetate Chemical compound COCC(C)OCC(C)OC(C)=O LAVARTIQQDZFNT-UHFFFAOYSA-N 0.000 description 1
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 description 1
- WMDZKDKPYCNCDZ-UHFFFAOYSA-N 2-(2-butoxypropoxy)propan-1-ol Chemical compound CCCCOC(C)COC(C)CO WMDZKDKPYCNCDZ-UHFFFAOYSA-N 0.000 description 1
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 1
- BWVZAZPLUTUBKD-UHFFFAOYSA-N 3-(5,6,6-Trimethylbicyclo[2.2.1]hept-1-yl)cyclohexanol Chemical compound CC1(C)C(C)C2CC1CC2C1CCCC(O)C1 BWVZAZPLUTUBKD-UHFFFAOYSA-N 0.000 description 1
- 235000021357 Behenic acid Nutrition 0.000 description 1
- 241000132023 Bellis perennis Species 0.000 description 1
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- 235000005633 Chrysanthemum balsamita Nutrition 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
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- 125000003277 amino group Chemical group 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
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- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- 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
- H01L24/27—Manufacturing methods
-
- 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
-
- 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
- H01L24/31—Structure, shape, material or disposition of the layer connectors after the connecting process
- H01L24/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
-
- 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
- H01L24/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
- H01L24/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—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
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
- H01L2224/29001—Core members of the layer connector
- H01L2224/29099—Material
- H01L2224/29198—Material with a principal constituent of the material being a combination of two or more materials in the form of a matrix with a filler, i.e. being a hybrid material, e.g. segmented structures, foams
- H01L2224/29298—Fillers
- H01L2224/29299—Base material
- H01L2224/293—Base material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
- H01L2224/29338—Base material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
- H01L2224/29339—Silver [Ag] as principal constituent
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—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
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/31—Structure, shape, material or disposition of the layer connectors after the connecting process
- H01L2224/32—Structure, shape, material or disposition of the layer connectors after the connecting process of an individual layer connector
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Abstract
【解決手段】銀粒子及び溶剤を含有する銀ペーストであって、銀粒子は、粒子径が1μm〜20μmである銀粒子と、大気圧下における沸点が130℃未満である保護剤で被覆された、粒子径が1nm〜300nmである銀粒子とを含む、銀ペースト。
【選択図】なし
Description
緻密度[%]=銀焼結体の密度[g/cm3]×100/銀の理論密度[10.49g/cm3]
約100mgの銀ナノ粒子をXRD測定用のガラスセルに乗せ、これを粉末X線回折装置(Rigaku CN4036)の試料ホルダーにセットした。加速電圧40kV、電流20mAでCuKα線を発生させ、グラファイトモノクロメータにより単色光化し、測定線源とした。2θ=5°〜85°の範囲で銀粒子の回折パターンを測定した。
銀粒子あるいは銀ペーストをTG−DTA測定用のAlサンプルパンに10mg乗せ、これをTG−DTA測定装置(エスアイアイ・ナノテクノロジー EXSTAR6000 TG/DTA6300)の試料ホルダーにセットした。ドライエアを流量約400mL/分で流しながら、昇温速度10℃/分で室温から約500℃までサンプルを加熱し、その際の重量変化と熱挙動を測定した。重量変化の停止点を有機物脱離の完了温度とした。
銀ペーストをホットプレート(井内盛栄堂 SHAMAL HOTPLATE HHP−401)により110℃で10分間予熱し、さらに200℃で1時間加熱することで銀焼結体(約10mm×10mm×1mm)を得た。作製した銀焼結体を紙やすり(800番)で研磨し、研磨後の銀焼結体の体積及び質量を測定した。これらの値から銀焼結体の密度を算出し、さらに下記の式に従い緻密度を算出した。
緻密度[%]=銀焼結体の密度[g/cm3]×100/銀の理論密度[10.49g/cm3]
銀ペーストをAgめっきCuリードフレーム(ランド部:10×5mm)上に0.1mg塗布し、その上に1mm×1mmのAuめっきSiチップ(Auめっき厚:0.1μm、チップ厚:400μm)を接着した。これをホットプレート(井内盛栄堂 SHAMAL HOTPLATE HHP−401)で、200℃で1時間加熱した。得られた銀焼結体の接着強度を、ダイシェア強度[MPa]により評価した。万能型ボンドテスタ(デイジ社製 4000シリーズ)を用い、測定スピード500μm/s、測定高さ100μmでAuめっきSiチップを水平方向に押し、銀焼結体のダイシェア強度[MPa]を測定した。
銀ペーストをホットプレート(井内盛栄堂 SHAMAL HOTPLATE HHP−401)により110℃で10分間予熱し、さらに200℃で1時間加熱することで銀焼結体(約10mm×10mm×1mm)を得た。この銀焼結体の熱拡散率をレーザーフラッシュ法(ネッチ社製 LFA 447、25℃)で測定し、さらにこの熱拡散率と、示差走査熱量測定装置(パーキンエルマー社製 Pyris1)で得られた比熱容量と焼結密度の積より、25℃における銀焼結体の熱伝導率[W/m・K]を算出した。
銀ペーストをガラス板上に塗布し、ホットプレート(井内盛栄堂 SHAMAL HOTPLATE HHP−401)により110℃で10分間予熱し、さらに200℃で1時間加熱することで、ガラス板上に1mm×50mm×0.03mmの銀焼結体を得た。この銀焼結体を4端子法(アドバンテスト(株)製 R687E DIGTAL MULTIMETER)にて体積抵抗率[μΩ・cm]を測定した。
銀ペーストをAgめっきCuリードフレーム(ランド部:10×5mm、Agめっき厚:約4μm)上に0.1mgを塗布し、この上に1mm×1mmのAuめっきSiチップ(Auめっき厚:0.1μm、チップ厚:400μm)を接着した。これをホットプレート(井内盛栄堂 SHAMAL HOTPLATE HHP−401)を用い200℃で1時間加熱した。接続したサンプルをエポキシ樹脂中に埋め込み、AuめっきSiチップ/銀焼結体/AgめっきCuリードフレームの断面が確認できるまで研磨した。研磨後のサンプルにイオンスパッター装置(日立ハイテクノロジーズ株式会社 E1045)で白金を蒸着し、これを卓上走査電子顕微鏡(日本電子株式会社 NeoScope JCM−5000)により、電子加速電圧10kV、倍率5000倍で観察し、SEM写真を撮影した。
銀ナノ粒子を次の手順で合成した。銀源としてAg2O(和光純薬株式会社)、還元剤としてジエチレングリコール(和光純薬株式会社、沸点244℃)、銀ナノ粒子の保護剤としてN,N−ジメチルエチレンジアミン(東京化成株式会社、沸点107℃)を使用した。これらの試薬を表1に示す配合割合でナスフラスコに加えた。反応溶液をマグネチックスターラーで約700rpmで攪拌しながら、110℃で3時間、加熱還流した。反応後の溶液にアセトンを約300mL加え、上澄み液を取り除き、沈殿した銀ナノ粒子を回収した。この銀ナノ粒子を40℃で3時間加熱し、乾燥させた。この銀ナノ粒子のXRD測定を行ったところ、図6に示すXRDパターンが得られ、金属銀であることを確認した。また、銀ナノ粒子は球状であり、銀ナノ粒子の粒子径は50〜200nmであることを確認した(図7)。この銀ナノ粒子のTG−DTA測定を行い、図1のチャートを得た。これより、銀ナノ粒子表面を被覆しているN,N−ジメチルエチレンジアミンが約225℃で脱離することが分かる。
銀ナノ粒子の保護剤としてN−メチルブチルアミン(東京化成株式会社、沸点91℃)を使用した以外は、実施例1と同様の手順で銀ナノ粒子を合成した。この銀ナノ粒子を使用して、実施例1と同様の手順で銀ペーストを作製した。銀ペーストの配合は表2のとおりである。この銀ペーストの特性を表3に示す。また、銀ナノ粒子は球状であり、銀ナノ粒子の粒子径は50〜200nmであることを確認した。
銀ナノ粒子の保護剤として1,2−ジメチルプロピルアミン(東京化成株式会社、沸点86℃)を使用した以外は、実施例1と同様の手順で銀ナノ粒子を合成した。この銀ナノ粒子を使用して、実施例1と同様の手順で銀ペーストを作製した。銀ペーストの配合は表2のとおりである。この銀ペーストの特性を表3に示す。また、銀ナノ粒子は球状であり、銀ナノ粒子の粒子径は200〜250nmであることを確認した。
銀ナノ粒子の保護剤としてトリエチルアミン(東京化成株式会社、沸点89.7℃)を使用した以外は、実施例1と同様の手順で銀ナノ粒子を合成した。この銀ナノ粒子を使用して、実施例1と同様の手順で銀ペーストを作製した。銀ペーストの配合は表2のとおりである。この銀ペーストの特性を表3に示す。また、銀ナノ粒子は球状であり、銀ナノ粒子の粒子径は35〜100nmであることを確認した。
銀ナノ粒子の保護剤として酢酸(東京化成株式会社、沸点118℃)を使用した以外は、実施例1と同様の手順で銀ナノ粒子を合成した。この銀ナノ粒子を使用して、実施例1と同様の手順で銀ペーストを作製した。銀ペーストの配合は表2のとおりである。この銀ペーストの特性を表3に示す。また、銀ナノ粒子は球状であり、銀ナノ粒子の粒子径は100〜280nmであることを確認した。
銀ナノ粒子の保護剤としてジエタノールアミン(和光純薬株式会社、沸点217℃)を使用した以外は、実施例1と同様の手順で銀ナノ粒子を合成した。銀ナノ粒子のTG−DTA測定を行い、図9のチャートを得た。これより、銀ナノ粒子表面からジエタノールアミンが約335℃で脱離することが分かる。この銀ナノ粒子を使用して、実施例1と同様の手順で銀ペーストを作製した。銀ペーストの配合は表2のとおりである。この銀ペーストの特性を表3に示す。また、銀ナノ粒子は球状であり、銀ナノ粒子の粒子径は100〜280nmであることを確認した。また、上記(7)に従って作製したAuめっきSiチップ/銀焼結体/AgめっきCuリードフレームにおけるAuめっきSiチップと銀焼結体との接続部の断面を撮影したSEM写真を図10に示す。比較例1の銀焼結体は、銀ナノ粒子の保護剤の脱離温度が高いために200℃では十分焼結が進まず、銀焼結体の緻密度、ダイシェア強度、体積抵抗率、及び熱伝導率の点で実施例1の銀焼結体よりも劣っていた。
実施例1と同様の手順で銀ナノ粒子を合成した。この銀ナノ粒子を使用して、銀マイクロ粒子を添加せずに、実施例1と同様の手順で銀ペーストを作製した。銀ペーストの配合は表2のとおりである。この銀ペーストの特性を表3に示す。また、上記(7)に従って作製したAuめっきSiチップ/銀焼結体/AgめっきCuリードフレームにおけるAuめっきSiチップと銀焼結体との接続部の断面を撮影したSEM写真を図11に示す。銀ナノ粒子の焼結時の体積収縮が大きく、AuめっきSiから焼結体が剥離した箇所が観察された。
銀ナノ粒子を添加せずに、銀マイクロ粒子だけを用いて、実施例1と同様の手順で銀ペーストを作製した。銀ペーストの配合は表2のとおりである。この銀ペーストの特性を表3に示す。また、上記(7)に従って作製したAuめっきSiチップ/銀焼結体/AgめっきCuリードフレームにおけるAuめっきSiチップと銀焼結体との接続部の断面を撮影したSEM写真を図12に示す。比較例3の銀焼結体の各特性は、実施例1の銀焼結体の各特性よりも劣っていた。
Claims (8)
- 銀粒子及び溶剤を含有する銀ペーストであって、
前記銀粒子は、粒子径が1μm〜20μmである銀粒子と、大気圧下における沸点が130℃未満である保護剤で被覆された、粒子径が1nm〜300nmである銀粒子とを含む、銀ペースト。 - 大気圧下における沸点が400℃以下であり、かつ常温で固体であるカルボン酸を更に含有する、請求項1に記載の銀ペースト。
- 前記保護剤が、アミン化合物、カルボン酸化合物、アミノ酸化合物、アミノアルコール化合物、及びアミド化合物からなる群より選ばれる少なくとも1種である、請求項1又は2に記載の銀ペースト。
- 前記保護剤が、1−アミノペンタン、2−アミノペンタン、3−アミノペンタン、2−メチルブチルアミン、3−メチルブチルアミン、1,2−ジメチルプロピルアミン、2,2−ジメチルプロピルアミン、N−メチルブチルアミン、N−メチルイソブチルアミン、エチルプロピルアミン、ピペリジン、メチルプロピルアミン、ジエチルアミン、モルホリン、トリエチルアミン、N,N−ジエチルメチルアミン、N,N−ジメチルイソプロピルアミン、N,N,N’−トリメチルエチレンジアミン、N,N−ジメチルエチレンジアミン、1,2−ビス(メチルアミノ)エタン、1,2−ジアミノプロパン、N−メチルエチレンジアミン、1,2−ジアミノエタン、及び酢酸からなる群より選ばれる少なくとも1種である、請求項1〜3のいずれか一項に記載の銀ペースト。
- 前記粒子径が1μm〜20μmである銀粒子の表面が、炭素数2〜20の脂肪族モノカルボン酸で被覆されている、請求項1〜4のいずれか一項に記載の銀ペースト。
- 前記粒子径が1μm〜20μmである銀粒子が、板状の銀粒子、又は板状の銀粒子と球状の銀粒子との混合物である、請求項1〜5のいずれか一項に記載の銀ペースト。
- 請求項1〜6のいずれか一項に記載の銀ペーストを焼結してなる焼結体を介して、半導体素子と半導体素子搭載用支持部材とが互いに接着した構造を有する半導体装置。
- 銀粒子及び溶剤を混合して銀ペーストを得る、銀ペーストの製造方法であって、
前記銀粒子として、粒子径が1μm〜20μmである銀粒子と、大気圧下における沸点が130℃未満である保護剤で被覆された、粒子径が1nm〜300nmである銀粒子とを用いる、銀ペーストの製造方法。
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JPWO2017043540A1 (ja) * | 2015-09-07 | 2018-08-09 | 日立化成株式会社 | 接合体及び半導体装置 |
JPWO2018131095A1 (ja) * | 2017-01-11 | 2019-11-07 | 日立化成株式会社 | 無加圧接合用銅ペースト、接合体、及び半導体装置 |
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