JP5256281B2 - 複合銀ナノペースト、その製法及びナノペースト接合方法 - Google Patents
複合銀ナノペースト、その製法及びナノペースト接合方法 Download PDFInfo
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- JP5256281B2 JP5256281B2 JP2010503690A JP2010503690A JP5256281B2 JP 5256281 B2 JP5256281 B2 JP 5256281B2 JP 2010503690 A JP2010503690 A JP 2010503690A JP 2010503690 A JP2010503690 A JP 2010503690A JP 5256281 B2 JP5256281 B2 JP 5256281B2
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- silver
- temperature
- composite
- resin
- paste
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 414
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 397
- 239000004332 silver Substances 0.000 title claims abstract description 396
- 239000002131 composite material Substances 0.000 title claims abstract description 252
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims description 34
- 239000011347 resin Substances 0.000 claims abstract description 155
- 229920005989 resin Polymers 0.000 claims abstract description 155
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 147
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 71
- 238000010438 heat treatment Methods 0.000 claims abstract description 50
- 239000002245 particle Substances 0.000 claims abstract description 41
- 239000002105 nanoparticle Substances 0.000 claims abstract description 26
- 150000003378 silver Chemical group 0.000 claims abstract description 25
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 24
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- 239000011248 coating agent Substances 0.000 claims abstract description 11
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- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 description 18
- 229910001958 silver carbonate Inorganic materials 0.000 description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 14
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- 229910000679 solder Inorganic materials 0.000 description 14
- 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 13
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 239000000853 adhesive Substances 0.000 description 12
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- 230000000694 effects Effects 0.000 description 4
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 4
- 150000002484 inorganic compounds Chemical class 0.000 description 4
- 229910010272 inorganic material Inorganic materials 0.000 description 4
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- UODXCYZDMHPIJE-UHFFFAOYSA-N menthanol Chemical compound CC1CCC(C(C)(C)O)CC1 UODXCYZDMHPIJE-UHFFFAOYSA-N 0.000 description 4
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
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- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- -1 Silver organic compounds Chemical class 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000003125 aqueous solvent Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- WIKQEUJFZPCFNJ-UHFFFAOYSA-N carbonic acid;silver Chemical compound [Ag].[Ag].OC(O)=O WIKQEUJFZPCFNJ-UHFFFAOYSA-N 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
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- KQTXIZHBFFWWFW-UHFFFAOYSA-L silver(I) carbonate Inorganic materials [Ag]OC(=O)O[Ag] KQTXIZHBFFWWFW-UHFFFAOYSA-L 0.000 description 3
- ORYURPRSXLUCSS-UHFFFAOYSA-M silver;octadecanoate Chemical compound [Ag+].CCCCCCCCCCCCCCCCCC([O-])=O ORYURPRSXLUCSS-UHFFFAOYSA-M 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 235000021360 Myristic acid Nutrition 0.000 description 2
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
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Classifications
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- 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
-
- 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
- H01L24/33—Structure, shape, material or disposition of the layer connectors after the connecting process of a plurality of layer connectors
-
- 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
- H01L24/34—Strap connectors, e.g. copper straps for grounding power devices; Manufacturing methods related thereto
- H01L24/36—Structure, shape, material or disposition of the strap connectors prior to the connecting process
- H01L24/37—Structure, shape, material or disposition of the strap connectors prior to the connecting process of an individual strap 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
- H01L24/34—Strap connectors, e.g. copper straps for grounding power devices; Manufacturing methods related thereto
- H01L24/39—Structure, shape, material or disposition of the strap connectors after the connecting process
- H01L24/40—Structure, shape, material or disposition of the strap connectors after the connecting process of an individual strap 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
- H01L24/84—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 strap connector
-
- 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
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
- H05K1/097—Inks comprising nanoparticles and specially adapted for being sintered at low temperature
-
- 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
- H01L2224/291—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
- H01L2224/29101—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 less than 400°C
-
- 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
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- 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
- H01L2224/321—Disposition
- H01L2224/32151—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
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Description
本発明では、樹脂の機能に最大の特徴がある。前記樹脂は30℃以下で非流動状態にあって前記複合銀ナノ粒子と前記銀微粒子を分散状態に保持し、加熱により流動化する性質を有する。前記非流動状態とは、固体状態又は高粘度状態を意味し、前記複合銀ナノ粒子と前記銀微粒子を分散状態に固定的に保持する性質を云う。30℃以下とは、通常室温領域であり、室温で保管する場合には、ペーストは非流動状態にあり、内部に分散した複合銀ナノ粒子や銀微粒子は樹脂によりペースト内で固定され、相互に凝集することはできない。即ち、30℃以下の室温で本発明のペーストを長期保存した場合、樹脂が非流動状態にあるから、樹脂中で銀微粒子と複合銀ナノ粒子が固定状態に保持され、それら粒子が相互に凝集することができず、ペースト保存中に粒子相互が凝集して団子化することが完全に防止される。この非流動性ペーストを非凝集性ペーストと称することができる。しかし、例えば40℃以上に加熱すると、樹脂が液化したり急激に粘性が低下して流動状態になり、ペーストとして対象物に塗着可能になる。従って、本発明のペーストを製造した後は30℃以下で保存して非凝集化(非流動化)しておく。ペーストを対象物に塗着する直前に加熱して流動化させて流動性ペーストにし、この流動性ペーストを対象物に塗着すれば、金属分(銀分)が凝集していないから極めて緻密な銀膜を形成することが可能になる。余った流動性ペーストは直ちに30℃以下に冷却すれば、非凝集性ペーストとして長期保存することが出来る。加熱により高粘度から低粘度に変化する樹脂として、例えばイソボルニルシクロヘキサノール(松脂状と称する)やグリセリン(シロップ状と称する)がある。30℃以下で固体であり、加熱すると液体化する樹脂として、例えばミリスチルアルコール(C14)、パルミチルアルコール(C16)、ステアリルアルコール(C18)、ベヘニルアルコール(C22)といったアルコール類、その他の物質が利用できる。これらの樹脂は、焼成したときに全ての成分が気散するか、又は炭化物などの残留物が極めて少ない性質を有することが必要であり、この性質により焼成により形成される銀膜の電気伝導性や熱伝導性を格段に向上できる。
加熱温度は樹脂が流動化する温度であり、しかも有機物が蒸発しない温度以下で調整される。まず、銀微粒子と樹脂を均一に混練し、その次に複合銀ナノ粒子を添加して均一に混練する。ヒーターにより加熱しなくても、混練する際の摩擦熱によりペースト温度が上昇し、例えば40℃位まで上昇すると自然にペーストが流動化し均一混練が可能になるから、強制加熱でなくても摩擦加熱(自然加熱)でも流動化を発現できる。また、先に銀微粒子と樹脂の二者を混練すると、ミクロンサイズの銀微粒子が樹脂中に均一に分散し易い。この後に、ナノサイズの複合銀ナノ粒子を添加して混練すると、複合銀ナノ粒子が樹脂中に均一分散し、樹脂と銀微粒子と複合銀ナノ粒子の三者が独立的に均一に分散したペーストを作り易い。混練方法には公知の混連装置が利用でき、自転遠心器だけでなく、自転公転遠心器なども利用できることは云うまでもない。
接着剤の役割を果たす前記複合銀ナノ粒子の重量が5(wt%)以下では銀微粒子相互の接着強度が小さくなり、30(wt%)以上ではペーストが高価格になると同時に、有機物量が多くなってボイドの発生量がやや増大する。また、複合銀ナノ粒子は、C10又はC12であるから、上述したように銀含有率が比較的高い。また、最大重量を占める銀微粒子は純銀であるから、ペースト全体における銀含有率を一層に高くでき、電気伝導度の増大化を実現できる。銀微粒子の重量が60(wt%)以下になると、相対的に銀含有率が低下し、90(wt%)以上では、接着剤となる複合銀ナノ粒子が少なくなり、銀粒子間の接着強度が低下する傾向がある。そして、有機分である樹脂は15(wt%)以下と少ないから、有機物含量が少なく、ペースト膜を焼成したときに、発生するガスは少なく、後に残るボイド(気泡空洞)が少なくなる。銀含有率が大きくなるほど、発生ガスは少なく、ボイドが少なくなるのは当然である。ボイドが少ない分だけ、銀膜と基体との接合面積割合は大きくなり、電気伝導性が高く、接合強度の高い銀膜を形成することができる。
更に、全体として銀含有率が80(wt%)以上の複合銀ナノペーストの製法を提供できる。銀含有率が80(wt%)未満になると、有機物含有率が20(wt%)以上になり、焼成時の発生ガス量が増大して、ボイド量が増加し、有効な接合強度と電気伝導度が得られなくなる。銀含有率は、85(wt%)以上が好ましく、90(wt%)以上であれば最も好ましく、半導体接合やパターン形成等の分野でも画期的なペーストを提供できる。
窒素雰囲気下で焼成すると、ペースト内の有機物は酸化されず、加熱により有機物は蒸発して気散されることが本発明者等の研究により明らかになった。複合銀ナノ粒子の場合、窒素雰囲気下では、銀核の周囲に結合したアルコラート基がアルコラート基単体で銀核から蒸発し、殆んど分解しないことが分かった。また、窒素雰囲気下では、樹脂成分も加熱により分解しないで蒸発して気散される。分解されないから、発生ガス量は少なく、ボイド発生量も必然的に少なくなる。その結果、銀膜と基体との接合面積割合は増大し、同時に接合強度と電気伝導度が増大する効果が得られる。また、有機物の蒸発温度は、空気による酸化温度よりも低いから、空気下焼成よりも焼成温度を低下でき、低温焼成を可能にする利点がある。更に、空気下焼成では、有機物が酸化されるため、有機物は分解されてCO2やH2Oとなって気散する結果、1モルの有機物が2モル、3モルと増加し、大量のガス発生によりボイド発生量が窒素雰囲気下とは比較できないほど増大する弱点がある。これに対し、上述したように、窒素雰囲気下ではガスの発生量を抑制でき、ボイドが少なく、接合面積割合が増大し、接合強度と電気伝導度の増大を実現することができる。
また、前記接合は荷重をかけながら行うこともできるが、無荷重下でも十分な接合を行えることを確認した。即ち、無荷重下でも接合面積割合や接合強度や電気伝導度を規定範囲内で実現できることが分かった。更に、焼成温度の範囲は250〜500℃であり、250℃という低温焼成でも、500℃という高温焼成でも本発明のぺーストを使用すれば、十分な接合を実現できることが確認された。そのことはその間の温度、即ち中間温度接合でも実用に耐える接合を実現できることを意味しており、実験的に確認されたものである。
2・・・・リードフレーム
4・・・・リードフレーム
6・・・・複合銀ナノペート層
6a・・・銀導体層
8・・・・ダイオードチップ
10・・・複合銀ナノペート層
10a・・銀導体層
12・・・複合銀ナノペート層
12a・・銀導体層
14・・・接続端子
16・・・電気炉
18・・・ダイオード樹脂モールド体
20・・・樹脂モールド
22・・・アノード
24・・・カソード
26・・・直流電源
28・・・電流計
VF・・・順方向電圧
ΔVF・・順方向電圧差
また、他の変形例として、まず所定重量%の銀微粒子Ag粉体と所定重量%の樹脂を加熱しながら混合してペースト中間体を製造する。このペースト中間体に所定重量%の複合銀ナノ粒子CnAgAL粉体を加熱しながら均一混合して複合銀ナノペーストを製造し、急速冷却して固形化する。摩擦熱を利用する場合には、強制加熱は不要である。この変形製造法では、まず樹脂中に銀微粒子を均一分散させ、その次に複合銀ナノ粒子を均一分散させるから、複合銀ナノ粒子と銀微粒子が独立に分散され、両者の相互作用を無くすため均一分散性が一層に増大する。
図19と図20を対比すると、金属化温度は、窒素中焼成では173℃、空気中焼成では249℃となり、窒素中温度がかなり低くなることが分かった。つまり、窒素中では焼成温度を低く設定できるから、コスト低減に効果がある。また、窒素中の焼成温度を空気中焼成温度と同じくらいに高く設定すれば、生成される銀膜の緻密化は一層改善され、高電気伝導と高熱伝導を保証できる。
図21と図22を対比すると、金属化温度は、窒素中焼成では177℃、空気中焼成では277℃となり、窒素中温度がかなり低くなることが分かった。つまり、窒素中では焼成温度を低く設定できるから、コスト低減に効果がある。また、窒素中の焼成温度を空気中焼成温度と同じくらいに高く設定すれば、生成される銀膜の緻密化は一層改善され、高電気伝導と高熱伝導を保証できることが実証された。
図23と図24を対比すると、金属化温度は、窒素中焼成では177℃、空気中焼成では277℃となり、窒素中温度がかなり低くなることが分かった。つまり、窒素中では焼成温度を低く設定できる。また、窒素中の焼成温度を空気中焼成温度と同じくらいに高く設定すれば、生成される銀膜の緻密化は一層改善され、高電気伝導と高熱伝導を保証できることが実証された。
図25と図26を対比すると、金属化温度は、窒素中焼成では170℃、空気中焼成では267℃となり、窒素中温度がかなり低くなることが分かった。つまり、窒素中では焼成温度を低く設定できるから、コスト低減に効果がある。また、窒素中の焼成温度を空気中焼成温度と同じくらいに高く設定すれば、生成される銀膜の緻密化は一層改善され、高電気伝導と高熱伝導を保証できることが実証された。
Pb−5Snの測定値と比較して、他のペーストの測定値が小さければ、従来の高温ハンダより本発明ペーストが優れている(○)と判定され、同程度なら可(△)、大きければ不可(×)と判定される。初期試験では、P23だけが(△)で、残り3種は(×)であった。リフロー耐熱試験後では、全てのペーストが(×)である。
Claims (14)
- 銀原子の集合体からなる銀核の周囲に、炭素数10又は12いずれかのアルコール分子残基、アルコール分子誘導体(ここで、アルコール分子誘導体とは、カルボン酸及び/又はアルデヒドに限定される)及び/又はアルコール分子の一種以上からなる有機被覆層を形成した複合銀ナノ粒子と、銀微粒子と、樹脂を混合して構成され、前記樹脂は30℃以下で非流動状態にあって前記複合銀ナノ粒子と前記銀微粒子を均一分散状態に保持し、加熱により流動化して塗着可能になることを特徴とする複合銀ナノペースト。
- 前記銀核の平均粒径は1〜20nmであり、前記銀微粒子の平均粒径は0.1〜3.0μmである請求項1に記載の複合銀ナノペースト。
- 前記複合銀ナノ粒子の重量は5〜30(wt%)、前記銀微粒子の重量は60〜90(wt%)であり、前記樹脂の重量は15(wt%)以下である請求項1又は2に記載の複合銀ナノペースト。
- 全体として銀含有率が80(wt%)以上である請求項3に記載の複合銀ナノペースト。
- 所望量の溶剤を添加して、30℃以下でも流動状態化させて塗着可能にする請求項1〜4のいずれかに記載の複合銀ナノペースト。
- 基体に塗着し、窒素雰囲気下で250〜500℃の温度で焼成して有機物を気散させて銀膜を形成したときに、前記銀膜と基体との接合面積割合が70%以上であり、前記銀膜の比抵抗が10(μΩcm)以下である請求項1〜5のいずれかに記載の複合銀ナノペースト。
- 銀原子の集合体からなる銀核の周囲に、炭素数10又は12いずれかのアルコール分子残基、アルコール分子誘導体(ここで、アルコール分子誘導体とは、カルボン酸及び/又はアルデヒドに限定される)及び/又はアルコール分子の一種以上からなる有機被覆層を形成した所定量の複合銀ナノ粒子を、30℃以下で非流動状態にあり加熱により流動化する所定量の樹脂に添加し、前記樹脂が流動状態になる温度で均一分散するまで混練してペースト中間体を形成し、このペースト中間体に所定量の銀微粒子を添加して前記温度で均一分散するまで混練し、混練後に前記樹脂が非流動状態になる温度まで冷却して、前記複合銀ナノ粒子と前記銀微粒子を前記樹脂中に均一分散状態に保持することを特徴とする複合銀ナノペーストの製法。
- 所定量の銀微粒子を、30℃以下で非流動状態にあり加熱により流動化する所定量の樹脂に添加し、前記樹脂が流動状態になる温度で均一分散するまで混練してペースト中間体を形成し、このペースト中間体に、銀原子の集合体からなる銀核の周囲に、炭素数10又は12いずれかのアルコール分子残基、アルコール分子誘導体(ここで、アルコール分子誘導体とは、カルボン酸及び/又はアルデヒドに限定される)及び/又はアルコール分子の一種以上からなる有機被覆層を形成した所定量の複合銀ナノ粒子を添加して前記温度で均一分散するまで混練し、混練後に前記樹脂が非流動状態になる温度まで冷却して、前記複合銀ナノ粒子と前記銀微粒子を前記樹脂中に均一分散状態に保持することを特徴とする複合銀ナノペーストの製法。
- 銀原子の集合体からなる銀核の周囲に、炭素数10又は12のアルコール分子残基、アルコール分子誘導体(ここで、アルコール分子誘導体とは、カルボン酸及び/又はアルデヒドに限定される)又はアルコール分子の一種以上からなる有機被覆層を形成した所定量の複合銀ナノ粒子と、所定量の銀微粒子を、30℃以下で非流動状態にあり加熱により流動化する所定量の樹脂に添加し、前記樹脂が流動状態になる温度で均一分散するまで混練し、混練後に前記樹脂が非流動状態になる温度まで冷却して、前記複合銀ナノ粒子と前記銀微粒子を前記樹脂中に均一分散状態に保持することを特徴とする複合銀ナノペーストの製法。
- 前記銀核の平均粒径は1〜20nm、前記銀微粒子の平均粒径は0.1〜3.0μmである請求項7、8又は9に記載の複合銀ナノペーストの製法。
- 前記複合銀ナノ粒子の前記所定量は5〜30(wt%)、前記銀微粒子の前記所定量は60〜90(wt%)、前記樹脂の前記所定量は15(wt%)以下であり、全体として銀含有率が80(wt%)以上である請求項7〜10のいずれかに記載の複合銀ナノペーストの製法。
- 所望量の溶剤を添加して、30℃以下でも流動状態化させて塗着可能なペーストにする請求項7〜11のいずれかに記載の複合銀ナノペーストの製法。
- 請求項1〜6のいずれかに記載の流動状態にある複合銀ナノペーストを用意し、前記複合銀ナノペーストを下部基体上に塗着して接合用ペースト層を形成し、及び/又は前記接合用ペースト層の上に上部基体を載置して接合体を形成し、前記接合体を窒素雰囲気下及び/又は無荷重下で250〜500℃の温度で焼成することを特徴とするナノペースト接合方法。
- 前記上部基体は半導体素子である請求項13に記載のナノペースト接合方法。
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JP5824201B2 (ja) * | 2009-09-11 | 2015-11-25 | Dowaエレクトロニクス株式会社 | 接合材およびそれを用いた接合方法 |
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