JP2020017340A - 導体形成用組成物、及び導体層を有する物品の製造方法 - Google Patents
導体形成用組成物、及び導体層を有する物品の製造方法 Download PDFInfo
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- JP2020017340A JP2020017340A JP2018137492A JP2018137492A JP2020017340A JP 2020017340 A JP2020017340 A JP 2020017340A JP 2018137492 A JP2018137492 A JP 2018137492A JP 2018137492 A JP2018137492 A JP 2018137492A JP 2020017340 A JP2020017340 A JP 2020017340A
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- Prior art keywords
- conductor
- copper
- forming
- composition
- particles
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- 239000000203 mixture Substances 0.000 title claims abstract description 136
- 238000004519 manufacturing process Methods 0.000 title claims description 9
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- 229910052802 copper Inorganic materials 0.000 claims abstract description 152
- 239000010949 copper Substances 0.000 claims abstract description 152
- 239000002245 particle Substances 0.000 claims abstract description 148
- 239000000758 substrate Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 42
- 238000007639 printing Methods 0.000 claims abstract description 14
- 238000007599 discharging Methods 0.000 claims abstract description 8
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- 238000010438 heat treatment Methods 0.000 claims description 30
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- 239000011247 coating layer Substances 0.000 claims description 14
- 239000007771 core particle Substances 0.000 claims description 13
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
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- 125000003277 amino group Chemical group 0.000 description 3
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- 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 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- 239000012691 Cu precursor Substances 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
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- 238000009835 boiling Methods 0.000 description 2
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Landscapes
- Manufacturing Of Electric Cables (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Conductive Materials (AREA)
Abstract
Description
[1]銅含有粒子と、前記銅含有粒子が分散している分散媒と、を含有する、導体形成用組成物であって、
当該導体形成用組成物の25℃における粘度が0.10〜300Pa・sであり、
当該導体形成用組成物のJIS Z3284に従って測定されるチキソトロピーインデックスが0.50〜0.90である、
導体形成用組成物。
[2]前記銅含有粒子の含有量が、前記銅含有粒子及び前記分散媒の合計量100質量部に対して、40〜80質量部である、[1]に記載の導体形成用組成物。
[3]前記銅含有粒子が、銅を含むコア粒子と、前記コア粒子の表面の少なくとも一部を被覆する有機被覆層とを有する被覆銅粒子である、[1]又は[2]に記載の導体形成用組成物。
[4]前記銅含有粒子の平均粒径が50μm以下である、[1]、[2]又は[3]に記載の導体形成用組成物。
[5]基材上に導体形成用組成物の膜を形成することと、前記導体形成用組成物の膜を焼結して導体層を形成することとを含み、前記導体形成用組成物の膜が、前記基材から離れた位置から液滴状の前記導体形成用組成物を吐出する印刷法により形成される、導体層を有する物品を製造する方法に用いられる、[1]、[2]、[3]又は[4]に記載の導体形成用組成物。
[6]基材上に[1]、[2]、[3]又は[4]に記載の導体形成用組成物の膜を形成することと、前記導体形成用組成物の膜を焼結して導体層を形成することとを含み、前記導体形成用組成物の膜が、前記基材から離れた位置から液滴状の前記導体形成用組成物を吐出する印刷法により形成される、導体層を有する物品を製造する方法。
[7]前記導体形成用組成物の膜を、250℃以下に加熱することにより焼結する、[6]に記載の方法。
[8]液滴状の前記導体形成用組成物が、前記基材から0.1〜20.0mmの距離の位置から吐出される、[6]又は[7]に記載の方法。
一実施形態に係る導体形成用組成物は、銅含有粒子と、銅含有粒子が分散している分散媒とを含有する。本実施形態に係る導体形成用組成物は、任意の基材上に導体層を形成して、導体層を有する物品を製造するために用いることができる。導体層形成用組成物は、導体又は導体層を形成するための導電塗料、導電ペースト、又は導電インクであることができる。
TI値={log(μ2.5/μ10)}/log(20/5)
図2は、導体層を有する物品の一実施形態を示す斜視図である。図2に示される物品1は、基材2と、基材2上に設けられた導体層3とを備える。導体層3は、上述の実施形態に係る導体形成用組成物の焼結体である。焼結体、すなわち導体層3は、導体形成用組成物に含まれていた銅含有粒子が融着した構造を有する。導体層3は、基材2上に、他の層を介さず直接設けられていてもよい。
1−1.ノナン酸銅(II)の合成
まず、セパラブルフラスコ中で水酸化銅(関東化学株式会社製、特級)91.5g(0.94mol)に1−プロパノール(関東化学株式会社製、特級)150mLを加え、これらの混合物を攪拌した。ノナン酸(関東化学株式会社製、90%以上)370.9g(2.34mol)を更に加えてから、フラスコ内の混合物を90℃に加熱しながら30分間攪拌した。得られた溶液を加熱したままろ過して未溶解物を除去した。ろ液を放冷し、生成した粉体を吸引ろ過により回収した。粉体を洗浄液が透明になるまでヘキサンで洗浄した後、50℃の防爆オーブンで3時間加熱することにより乾燥して、ノナン酸銅(II)を得た。収量は340g(収率96質量%)であった。
上記で得られたノナン酸銅(II)15.01g(0.040mol)と酢酸銅(II)無水物(関東化学株式会社製、特級)7.21g(0.040mol)をセパラブルフラスコに入れ、1−プロパノール22mLとヘキシルアミン(東京化成工業株式会社製、純度99%)32.1g(0.32mol)を更に加え、フラスコ内の反応液をオイルバス中80℃に加熱しながら攪拌して固形分を溶解させた。銅(ノナン酸銅及び酢酸銅無水物中の銅の合計量):ヘキシルアミンのモル比は1:4である。フラスコを氷浴に移し、内温が5℃になるまで冷却した後、ヒドラジン一水和物(関東化学株式会社製、特級)7.72mL(0.16mol)を加え、反応液を氷浴中で更に攪拌した。次いで、反応液をオイルバス中で20分間、90℃に加熱しながら攪拌した。その際、発泡を伴う還元反応が進み、セパラブルフラスコの内壁が銅光沢を呈し、溶液が暗赤色に変化した。遠心分離を1000rpm(回転/分)で20秒実施して固体物を回収した。固形物を更にヘキサン15mLで3回繰り返して洗浄することで酸残渣を除去して、銅光沢を有する銅含有粒子(長軸の長さの平均値:0.15μm)を含む銅ケークを得た。
銅ケーク(銅含有粒子)と、分散媒としてのテルピネオール及びイソボルニルシクロヘキサノール(商品名:テルソルブMTPH、日本テルペン化学株式会社製)とを、表1に示す配合比で混合して、実施例及び比較例の導体形成用組成物を調製した。
3−1.粘度
E型粘度計(東機産業株式会社製、製品名:VISCOMETER−TV33)を用いて、導体形成用組成物の25℃における粘度を測定した。測定用冶具として、コーンプレートを用い、回転数を2.5rpmとした。
TI値を、JIS Z3284に従って測定した。より具体的には、E型粘度計(東機産業株式会社製、製品名:VISCOMETER−TV33)を用いて、25℃で回転数2.5rpm及び回転数10rpmの条件で粘度を測定した。回転数2.5rpmの粘度μ2.5、及び回転数10rpmの粘度μ10から、下記式によりTI値を算出した。
TI値={log(μ2.5/μ10)}/log(20/5)
長さ1cmで深さ5mmの凹部を形成している表面を有する液晶ポリマー(LCP)立体基材を準備した。このLCP立体基材の凹部に、各導体形成用組成物を、ジェットディスペンサ(HOTMELT SUPER JET MJET−S−HM、武蔵エンジニアリング株式会社製)を用いて、幅0.4mmの線状に塗布し、濡れ広がり性及び飛び散りの状態を以下の方法で評価した。ジェットディスペンサのノズルとLCP立体基材の表面との距離は、6.0mmであった。その後、塗膜を加熱して、導体形成用組成物の焼結体である導体層を形成した。塗膜は、5%ギ酸雰囲気中、昇温速度40℃/分で180℃まで昇温し、180℃で60分間保持する条件で加熱した。
導体形成用組成物を塗布した直後と、塗布から5分後における塗膜の最大幅及び最小幅を測定し、以下の基準で濡れ広がり性を判定した。塗膜の幅の増加率は、平均的な幅の部分に関して、塗布直後の幅と5分後の幅との差の、塗布直後の幅に対する割合である。実施例2〜6の場合、塗膜の幅の最大値と最小値の差(塗膜の幅むら)が、最大値と最小値の平均値に対して5%以内であり、塗膜の幅の均一性の点でも良好であった。実施例7では、塗膜の幅むらが5%以上とやや大きかった。
A:塗膜の幅の増加率が5%以内
B:塗膜の幅の増加率が5%を超えて10%以内
C:塗膜の幅の増加率が10%を超える
導体形成用組成物の塗膜の周辺を観察し、飛び散って基材に付着した導体形成用組成物の数(飛び散りの数)に基づいた以下の基準で飛び散りの状態を評価した。一般に、飛び散りの数が2個以下であれば、塗布性が良好であるとみなすことができる。
A:飛び散りが認められない
B:飛び散りの数が1〜2個
C:飛び散りの数が3個以上
形成された導体層の体積抵抗率を、4端針面抵抗測定器で測定した面抵抗値と、非接触表面・層断面形状計測システム(VertScan、三菱ケミカルシステム株式会社製)で測定した膜厚とから計算した。体積低効率の値に基づく以下の基準により、導体層の導電性を判定した。一般に、体積抵抗率が100μΩ・cm未満であれば、導電性に優れるといえる。
A:10μΩ・cm未満
B:10μΩ・cm以上30μΩ・cm未満
C:30μΩ・cm以上100μΩ・cm未満
D:100μΩ・cm以上
Claims (8)
- 銅含有粒子と、前記銅含有粒子が分散している分散媒と、を含有する、導体形成用組成物であって、
当該導体形成用組成物の25℃における粘度が0.10〜300Pa・sであり、
当該導体形成用組成物のJIS Z3284に従って測定されるチキソトロピーインデックスが0.50〜0.90である、
導体形成用組成物。 - 前記銅含有粒子の含有量が、前記銅含有粒子及び前記分散媒の合計量100質量部に対して、40〜80質量部である、請求項1に記載の導体形成用組成物。
- 前記銅含有粒子が、銅を含むコア粒子と、前記コア粒子の表面の少なくとも一部を被覆する有機被覆層とを有する被覆銅粒子である、請求項1又は2に記載の導体形成用組成物。
- 前記銅含有粒子の平均粒径が50μm以下である、請求項1〜3のいずれか一項に記載の導体形成用組成物。
- 基材上に導体形成用組成物の膜を形成することと、前記導体形成用組成物の膜を焼結して導体層を形成することとを含み、前記導体形成用組成物の膜が、前記基材から離れた位置から液滴状の前記導体形成用組成物を吐出する印刷法により形成される、導体層を有する物品を製造する方法に用いられる、請求項1〜4のいずれか一項に記載の導体形成用組成物。
- 基材上に請求項1〜4のいずれか一項に記載の導体形成用組成物の膜を形成することと、前記導体形成用組成物の膜を焼結して導体層を形成することとを含み、前記導体形成用組成物の膜が、前記基材から離れた位置から液滴状の前記導体形成用組成物を吐出する印刷法により形成される、導体層を有する物品を製造する方法。
- 前記導体形成用組成物の膜を、250℃以下に加熱することにより焼結する、請求項6に記載の方法。
- 液滴状の前記導体形成用組成物が、前記基材から0.1〜20.0mmの距離の位置から吐出される、請求項6又は7に記載の方法。
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