JP2017190483A - 銀被覆銅粉およびその製造方法 - Google Patents
銀被覆銅粉およびその製造方法 Download PDFInfo
- Publication number
- JP2017190483A JP2017190483A JP2016079577A JP2016079577A JP2017190483A JP 2017190483 A JP2017190483 A JP 2017190483A JP 2016079577 A JP2016079577 A JP 2016079577A JP 2016079577 A JP2016079577 A JP 2016079577A JP 2017190483 A JP2017190483 A JP 2017190483A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- copper powder
- coated copper
- diameter
- coated
- 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
Links
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 252
- 239000004332 silver Substances 0.000 title claims abstract description 252
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 251
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000010949 copper Substances 0.000 claims abstract description 76
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- 239000002002 slurry Substances 0.000 claims abstract description 33
- 229910052802 copper Inorganic materials 0.000 claims abstract description 30
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- 229910052698 phosphorus Inorganic materials 0.000 claims description 46
- 239000011574 phosphorus Substances 0.000 claims description 46
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- 238000009826 distribution Methods 0.000 claims description 19
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 17
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- 238000006243 chemical reaction Methods 0.000 description 8
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Images
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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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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
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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
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Abstract
【解決手段】銅を加熱して溶解した溶湯を落下させながら高圧水を吹き付けて急冷凝固して得られた銅粉のスラリーを窒素ガスなどの非酸化性ガスの存在下で保持した後、固液分離して得られた銅粉を銀含有層(銀または銀化合物からなる層)で被覆して銀被覆銅粉を得る。
【選択図】なし
Description
無酸素銅15kgを加熱して溶解した1300℃の溶湯中に(15質量%のリンを含む)リン銅合金を(溶湯中の)リン濃度が930ppmになるように添加して撹拌し、混合することにより作製したリン含有銅溶湯をタンディッシュ下部から落下させながら、水アトマイズ装置により大気中において水圧150MPaで高圧水を吹き付けて急冷凝固させ、得られたスラリーをタンク内に収容し、スラリー中に500L/分の流量で窒素ガスを吹き込んで30分間保持した後、固液分離し、固形物を水洗し、110℃で10時間乾燥し、解砕し、風力分級して、少量のリンを含む銅粉を得た。なお、窒素ガスを吹き込んで保持したときのタンク内の雰囲気中の酸素濃度は0.1質量%未満であった。また、高圧水として、高圧ポンプに給水するタンク中の純水に水酸化ナトリウムを添加して得られたpH10.3のアルカリ水溶液を使用した。
EDTA−2Na二水和物143gと炭酸アンモニウム143gを純水1662gに溶解した溶液(溶液1)と、EDTA−2Na二水和物405gと炭酸アンモニウム202gを純水1613gに溶解した溶液に、硝酸銀67gを純水209gに溶解した溶液を加えて得られた溶液(溶液2)を用意した。
溶湯中のリン濃度が950ppmになるようにリン銅合金を添加し、溶湯の温度を1600℃とし、高圧水として、高圧ポンプに給水するタンク中の純水に水酸化ナトリウムを添加して得られたpH10.7のアルカリ水溶液を使用した以外は、実施例1と同様の方法により、少量のリンを含む銅粉を得た。
高圧水の水圧を100MPaとした以外は、実施例1と同様の方法により、少量のリンを含む銅粉を得た。
銅を加熱して溶解した溶湯中にリン銅合金を添加しなかった以外は、実施例4と同様の方法により、銀被覆銅粉末を得た。
銅を加熱して溶解した溶湯中にリン銅合金を添加せず、高圧水としてpH5.8の水を使用し、窒素ガスの吹き込みを行わなかった以外は、実施例1と同様の方法により、銀被覆銅粉末を得た。
銅を加熱して溶解した溶湯中にリン銅合金を添加せず、窒素ガスの吹き込みを行わなかった以外は、実施例1と同様の方法により、銀被覆銅粉末を得た。
Claims (10)
- 銅を加熱して溶解した溶湯を落下させながら高圧水を吹き付けて急冷凝固して得られた銅粉のスラリーを非酸化性ガスの存在下で保持した後、固液分離して得られた銅粉を銀含有層で被覆することを特徴とする、銀被覆銅粉の製造方法。
- 前記スラリー中と前記スラリーを収容する容器内との少なくとも一方に前記非酸化性ガスを吹き込みながら保持することによって、前記スラリーを非酸化性ガスの存在下で保持することを特徴とする、請求項1に記載の銀被覆銅粉の製造方法。
- 前記銅粉のレーザー回折式粒度分布装置により測定した体積基準の累積50%粒子径(D50径)が0.1〜15μmであることを特徴とする、請求項1または2に記載の銀被覆銅粉の製造方法。
- 前記高圧水がアルカリ水溶液であることを特徴とする、請求項1乃至3のいずれかに記載の銀被覆銅粉の製造方法。
- 前記溶湯にリンを添加することを特徴とする、請求項1乃至4のいずれかに記載の銀被覆銅粉の製造方法。
- 銅粉の表面が銀含有層で被覆された銀被覆銅粉であって、Cuの(200)面における結晶子径D(200)に対するCuの(111)面における結晶子径D(111)の比D(111)/D(200)が1.8以上であり且つCuの(220)面における結晶子径D(220)に対するCuの(200)面における結晶子径D(200)の比D(200)/D(220)が1.095以下であることを特徴とする、銀被覆銅粉。
- 前記銀被覆銅粉のCuの(220)面における結晶子径D(220)に対するCuの(111)面における結晶子径D(111)の比D(111)/D(220)が1.90以上であることを特徴とする、請求項6に記載の銀被覆銅粉。
- 前記銀被覆銅粉のレーザー回折式粒度分布装置により測定した体積基準の累積50%粒子径(D50径)が0.1〜15μmであることを特徴とする、請求項6または7に記載の銀被覆銅粉。
- 前記銀被覆銅粉中のリン含有量が10〜1000ppmであることを特徴とする、請求項6乃至8のいずれかに記載の銀被覆銅粉。
- 導電性粉末として請求項6乃至9のいずれかに記載の銀被覆銅粉を含むことを特徴とする、導電性ペースト。
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JP2013258128A (ja) * | 2012-05-18 | 2013-12-26 | Tohoku Univ | 導電性ペースト |
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JP7170464B2 (ja) | 2018-08-30 | 2022-11-14 | Dowaエレクトロニクス株式会社 | 銀被覆金属粉末の洗浄方法、銀被覆金属粉末の製造方法、銀被覆銅粉末、銀被覆銅合金粉末、導電性ペースト及び導電膜の製造方法、電子部品、及び電気装置 |
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