JPWO2016125355A1 - 導電性の微小粒子 - Google Patents
導電性の微小粒子 Download PDFInfo
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- 239000010419 fine particle Substances 0.000 title claims abstract description 51
- 239000002245 particle Substances 0.000 claims abstract description 127
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 229910052709 silver Inorganic materials 0.000 claims abstract description 16
- 239000004332 silver Substances 0.000 claims abstract description 16
- 230000001186 cumulative effect Effects 0.000 claims description 23
- 239000002904 solvent Substances 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 238000000691 measurement method Methods 0.000 claims description 4
- 239000011859 microparticle Substances 0.000 abstract description 14
- 239000006185 dispersion Substances 0.000 description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 18
- 238000000034 method Methods 0.000 description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 14
- XNGYKPINNDWGGF-UHFFFAOYSA-L silver oxalate Chemical compound [Ag+].[Ag+].[O-]C(=O)C([O-])=O XNGYKPINNDWGGF-UHFFFAOYSA-L 0.000 description 14
- 238000005245 sintering Methods 0.000 description 12
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- -1 oxalate compound Chemical class 0.000 description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 150000002894 organic compounds Chemical class 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 3
- 229940100890 silver compound Drugs 0.000 description 3
- 150000003379 silver compounds Chemical class 0.000 description 3
- 229910001111 Fine metal Inorganic materials 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical class OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
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- 125000003827 glycol group Chemical group 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
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- 239000002060 nanoflake Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- H—ELECTRICITY
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
-
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- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
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- 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
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- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
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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
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- 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
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- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
- H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
- H05K3/321—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by conductive adhesives
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
Description
(1)フレーク状でありその主成分が導電性金属である多数の微小粒子を含む粒子群
及び
(2)溶媒
を含有する。この粒子群の、レーザー回折散乱式粒度分布測定法によって測定された、累積50体積%粒子径D50は0.10μm以上0.50μm以下であり、累積95体積%粒子径D95は1.00μm以下であり、最大粒子径Dmaxは3.00μm以下である。
モード:散乱式、湿式(水)
レーザー光:80−90%
LED光:70−90%
Ag2C2O4 = 2Ag + 2CO2
この分散液の中に、銀が粒子として析出する。この銀粒子の表面に、シュウ酸銀、キャリヤー又は分散剤に由来する有機化合物が付着する。この有機化合物は、銀粒子と化学的に結合している。換言すれば、微小粒子2は、銀と、有機化合物とを含む。微小粒子2の主成分は、銀である。微小粒子2の質量に占める銀の質量は、99.0%以上が好ましく、99.5%以上が特に好ましい。微小粒子2が、有機化合物を含まなくてもよい。
(1)分散液におけるシュウ酸銀の濃度を所定の範囲に設定する
(2)特定の分散剤を用いる
(3)加熱時の圧力を所定の範囲に設定する
(4)撹拌速度を所定の範囲に設定する
(5)分散液のPHを適正にする
等が挙げられる。
1Lの蒸留水に50gの硝酸銀を溶解させて、第一の溶液を得た。一方、1Lの蒸留水に22.2gのシュウ酸を溶解させて、第二の溶液を得た。第一の溶液と第二の溶液とを混合し、シュウ酸銀を含む混合液を得た。この混合液から、不純物を除去した。1Lの混合液に3gのポリエチレングリコール(分散剤)を添加し、超音波を加えつつ、30分間撹拌した。これにより、シュウ酸銀を分散させた。この分散液に適量の酢酸を添加し、PHを3に調整した。この分散液を、オートクレーブに投入した。この分散液を、0.5MPaの圧力で加圧した。この分散液を300rpmの速度で撹拌しつつ、130℃まで加熱した。この温度下で30分間の撹拌を行い、銀を主成分とする微小粒子を含む液体を得た。
酢酸に代えて蟻酸を分散液に添加してPHを4とし、分散液の温度を150℃とし、攪拌速度を350rpmとした他は実施例1と同様にして、微小粒子を含む液体を得た。
酢酸に代えてプロピオン酸を分散液に添加してPHを5とし、反応前の加圧を行わず、反応時の温度を150℃とした他は実施例1と同様にして、微小粒子を含む液体を得た。
酢酸を添加しないことでPHを7とし、反応前の加圧を行わず、反応時の温度を120℃とし、反応時の撹拌速度を150rpmとした他は実施例1と同様にして、微小粒子を含む液体を得た。
銀からなり球状である微小粒子を、ボールミルにてフレーク状に加工した。
多数の微小粒子、バインダー及び分散剤を混合して、導電性ペーストを得た。この導電性ペーストを用い、線幅が3μm、10μm及び60μmである配線を印刷した。印刷状況を顕微鏡で確認した。良好な配線が印刷された場合を「Good」とし、良好な配線が印刷されなかった場合を「Bad」とした。この結果が、下記の表1に示されている。
線幅が60μmである配線を、下記の条件で加熱した。加熱後の配線の電気比抵抗を測定した。この結果が、下記の表1に示されている。電気比抵抗が大きすぎて測定できなかった場合を、表1において、Over Rangeと表している。
Claims (7)
- フレーク状でありその主成分が導電性金属である多数の微小粒子を含んでおり、
レーザー回折散乱式粒度分布測定法によって測定された、累積50体積%粒子径D50が0.10μm以上0.50μm以下であり、累積95体積%粒子径D95が1.00μm以下であり、最大粒子径Dmaxが3.00μm以下である導電性の粒子群。 - 上記主成分が銀又は銅である請求項1に記載の粒子群。
- レーザー回折散乱式粒度分布測定法によって測定された累積10体積%粒子径D10が0.05μm以上である請求項1又は2に記載の粒子群。
- BET比表面積が2.0m2/g以上である請求項1から3のいずれかに記載の粒子群。
- タップ密度TDが2.0g/cm3以上である請求項1から4のいずれかに記載の粒子群。
- 上記微小粒子の厚みの平均値Taveが0.05μm以下である請求項1から5のいずれかに記載の粒子群。
- (1)フレーク状でありその主成分が導電性金属である多数の微小粒子を含む粒子群
及び
(2)溶媒
を含有しており、
上記粒子群の、レーザー回折散乱式粒度分布測定法によって測定された、累積50体積%粒子径D50が0.10μm以上0.50μm以下であり、累積95体積%粒子径D95が1.00μm以下であり、最大粒子径Dmaxが3.00μm以下である導電性ペースト。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2015022333 | 2015-02-06 | ||
JP2015022333 | 2015-02-06 | ||
PCT/JP2015/081105 WO2016125355A1 (ja) | 2015-02-06 | 2015-11-05 | 導電性の微小粒子 |
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Publication Number | Publication Date |
---|---|
JPWO2016125355A1 true JPWO2016125355A1 (ja) | 2017-07-27 |
JP6446069B2 JP6446069B2 (ja) | 2018-12-26 |
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Country | Link |
---|---|
US (1) | US20170326639A1 (ja) |
EP (1) | EP3248713B1 (ja) |
JP (1) | JP6446069B2 (ja) |
KR (1) | KR20170110613A (ja) |
CN (1) | CN107206485B (ja) |
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JP6870436B2 (ja) * | 2017-03-31 | 2021-05-12 | 三菱マテリアル株式会社 | 金属粒子凝集体とその製造方法、ペースト状金属粒子組成物および接合体の製造方法 |
JP6467542B1 (ja) * | 2018-03-29 | 2019-02-13 | トクセン工業株式会社 | インク用又は塗料用の銀粉 |
JP7080950B2 (ja) | 2020-10-15 | 2022-06-06 | トクセン工業株式会社 | 金属粉 |
CN115007875A (zh) * | 2022-06-14 | 2022-09-06 | 江苏连银新材料有限公司 | 一种银粉及其制备方法 |
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Also Published As
Publication number | Publication date |
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WO2016125355A1 (ja) | 2016-08-11 |
JP6446069B2 (ja) | 2018-12-26 |
CN107206485A (zh) | 2017-09-26 |
US20170326639A1 (en) | 2017-11-16 |
EP3248713B1 (en) | 2020-03-25 |
CN107206485B (zh) | 2020-06-02 |
EP3248713A1 (en) | 2017-11-29 |
EP3248713A4 (en) | 2018-09-19 |
KR20170110613A (ko) | 2017-10-11 |
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