JP6659712B2 - 導電材用粉末、導電材用インク及び導電性ペースト並びに導電材用粉末の製造方法 - Google Patents
導電材用粉末、導電材用インク及び導電性ペースト並びに導電材用粉末の製造方法 Download PDFInfo
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- JP6659712B2 JP6659712B2 JP2017543420A JP2017543420A JP6659712B2 JP 6659712 B2 JP6659712 B2 JP 6659712B2 JP 2017543420 A JP2017543420 A JP 2017543420A JP 2017543420 A JP2017543420 A JP 2017543420A JP 6659712 B2 JP6659712 B2 JP 6659712B2
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- 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
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Description
S2 遠心分離工程
上記公報に開示される導電性ペースト用の銅粉末は、アトマイズ法により製造されるものであるため、比較的粒子径が大きくなる。従って、上記公報に開示される導電性ペーストは、均一な厚さで薄く塗布することが難しく、例えばメッキ下地とされる導電性薄膜を形成する場合には使用に適さない。また、上記公報に開示される導電性ペーストは、銅粉末の粒子径に起因して、得られる導電層の表面の平滑性を向上することが容易ではないという不都合もある。
本発明の一態様に係る導電材用粉末及び本発明の別の態様に係る導電材用粉末の製造方法によって得られる導電材用粉末は、比較的厚さが小さくかつ表面が平滑な導電層を形成できる。
本発明の一態様に係る導電材用粉末は、銅を主成分とする多数の粒子から構成され、平均一次粒子径が1nm以上200nm以下の導電材用粉末であって、上記粒子の表面又は内部にチタンを含み、このチタンの含有率が0.003atomic%以上0.5atomic%以下である。
以下、本発明の各実施形態について、適宜図面を参照しつつ詳説する。
本発明の一実施形態に係る導電材用粉末は、銅を主成分とする多数の粒子から構成され、導電性を有する層を形成するために用いられる。
続いて、当該導電材用粉末の製造方法について詳説する。
ステップS1の投入工程では、還元剤水溶液を撹拌しながら、この還元剤水溶液に原料水溶液を投入する。
還元剤水溶液としては、三価のチタンイオンを生じる水溶性チタン化合物を水に溶解したものや、水溶液中の四価のチタンイオンを電解還元して三価のチタンイオンに転換したものを用いることができる。上記三価のチタンイオンを生じる化合物としては、例えば三塩化チタン等が挙げられる。また、市販の高濃度三塩化チタン水溶液を使用してもよい。
原料水溶液としては、水溶性銅化合物を水に溶解して電離させることにより銅イオンを生じたものを用いることができる。銅イオンを生じる水溶性銅化合物としては、例えば硝酸銅(II)〔Cu(NO3)2〕、硫酸銅(II)五水和物〔CuSO4・5H2O〕、塩化銅(II)〔CuCl2〕等が挙げられる。
ステップS2の遠心分離工程では、上記投入工程後の水溶液、つまり還元剤水溶液に原料水溶液を投入した合成液の遠心分離により、合成液から析出した粒子を分離する。
続いて、本発明の別の実施形態に係る導電材用インクについて詳説する。
当該導電材用インクの水性分散媒としては、水又は水に高極性溶媒を混合したものが使用され、中でも水及び水と相溶する高極性溶媒を混合したものが好適に利用される。このような水性分散媒としては、導電材用粉末析出後の還元剤水溶液を調整したものを使用することができる。つまり、予め導電材用粉末を含む還元剤水溶液を限外ろ過、遠心分離、電気透析等の処理に供して不純物を除去したものに高極性溶媒を加えることで、予め一定量の導電材用粉末を含む水性分散媒が得られる。
続いて、本発明の別の実施形態に係る導電性ペーストについて詳説する。
今回開示された実施の形態は全ての点で例示であって制限的なものではないと考えられるべきである。本発明の範囲は、上記実施形態の構成に限定されるものではなく、特許請求の範囲によって示され、特許請求の範囲と均等の意味及び範囲内での全ての変更が含まれることが意図される。
ビーカーに還元剤として三塩化チタン溶液80g(約0.1mol)、pH調整剤として炭酸ナトリウム50g、錯化剤としてのクエン酸ナトリウム90g、及び分散剤としてのポリビニルピロリドン(分子量30000)1gを純水に溶解して還元剤水溶液が0.8Lとなるよう調製した。
硝酸銅三水和物10g(約0.04mol)を純水に溶解して原料水溶液が0.2Lとなるよう調製した。
上記還元剤水溶液及び原料水溶液の温度を35℃に保持し、還元剤水溶液を撹拌しながらこの還元剤水溶液に原料水溶液を2秒かけて投入して、銅を主成分とする金属粒子を析出させた。つまり、原料水溶液の投入速度を、合成液の単位量に対する銅イオン量に換算して0.02mol・L−1・s−1とした。
原料水溶液の投入時間を1秒(合成液を基準とする銅イオンの投入速度に換算して0.04mol・L−1・s−1)とした以外は上記試作品No.1と同じ条件で、導電材用粉末の試作品No.2を得た。
遠心分離の遠心加速度を30,000Gに設定した以外は上記試作品No.1と同じ条件で、導電材用粉末の試作品No.3を得た。
還元剤水溶液及び原料水溶液の温度を50℃にした以外は上記試作品No.1と同じ条件で、導電材用粉末の試作品No.4を得た。
原料水溶液の投入時間を5秒(合成液を基準とする銅イオンの投入速度に換算して0.008mol・L−1・s−1)とした以外は上記試作品No.1と同じ条件で、導電材用粉末の試作品No.5を得た。
遠心分離の遠心加速度を15,000Gに設定した以外は上記試作品No.1と同じ条件で、導電材用粉末の試作品No.6を得た。
上記導電材用粉末の試作品No.1〜6の表面を100k〜300k倍の倍率で走査型電子顕微鏡(SEM)にて観察し、任意に抽出した金属微粒子100個を測長して粒子径の小さい順に体積を積算した際の累積体積が50%となる粒子径[nm]を算出して平均一次粒子径とした。
上記導電材用粉末の試作品No.1〜6における、チタン及び塩素の含有率をそれぞれ測定した。なお、チタンの含有率は、サーモフィッシャーサイエンティフィック社のICP分析(高周波誘導結合プラズマ発光分光分析)装置「iCAP6300DUO」により測定した。また、塩素の含有率は、サーモフィッシャーサイエンティフィック社のイオンクロマトグラフィ「ICS−2100」により測定した。
上記導電材用粉末の試作品No.1〜6にそれぞれ純水を加えて導電材用粉末の含有率が30質量%の導電材用インクを調製した。そして、親水化処理され、一辺10cmの正方形状に切り出されたポリイミドフィルムの表面に各導電材用インクを滴下してバーコートを行った。さらに、これら塗膜を自然乾燥した後、窒素雰囲気中において、300℃で30分間焼成することで、ポリイミドフィルム上に導電層を形成した。
上記焼成の前後において、各塗膜(導電層)の平滑性の指標として、ISO25178に準拠して表面粗さ(算術平均高さSa)をそれぞれ測定し、各塗膜(導電層)の焼成前後での表面粗さの変化率として、焼成後の表面粗さの焼成前の表面粗さに対する比をそれぞれ算出した。
Claims (6)
- 銅を主成分とする多数の粒子から構成され、平均一次粒子径が1nm以上200nm以下の導電材用粉末であって、
上記粒子の表面又は内部にチタンを含み、
このチタンの含有率が0.003atomic%以上0.5atomic%以下であり、
上記粒子の表面又は内部に塩素を含み、
この塩素の含有率が0.05atomic%以上5atomic%以下である導電材用粉末。 - 上記チタンが上記粒子の内部に含まれる請求項1に記載の導電材用粉末。
- 水性分散媒と、
この水性分散媒中に分散される請求項1に記載の導電材用粉末と
を備える導電材用インク。 - ポリマー組成物と、
このポリマー組成物中に含まれる請求項1に記載の導電材用粉末と
を備える導電性ペースト。 - 銅を主成分とする多数の粒子から構成され、平均一次粒子径が1nm以上200nm以下の導電材用粉末の液相還元法による製造方法であって、
三価のチタンイオンを含む還元剤水溶液に銅イオンを含む原料水溶液を投入する工程を備え、
上記原料水溶液の投入速度が、還元剤水溶液に原料水溶液を投入して得られる合成液の単位量に対する銅イオン量に換算して0.01mol・L−1・s−1以上であり、
上記還元剤水溶液の三価のチタンイオンの濃度が0.01mol/L以上2mol/L以下であり、
上記原料水溶液の銅イオンの濃度が0.05mol/L以上10mol/L以下であり、
上記粒子の表面又は内部に塩素を含み、
この塩素の含有率が0.05atomic%以上5atomic%以下である導電材用粉末の製造方法。 - 上記合成液を遠心分離する工程をさらに備え、
上記遠心分離の遠心加速度が20,000G以上である請求項5に記載の導電材用粉末の製造方法。
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