JP5431073B2 - 導電性基材を製造する方法 - Google Patents
導電性基材を製造する方法 Download PDFInfo
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- JP5431073B2 JP5431073B2 JP2009200756A JP2009200756A JP5431073B2 JP 5431073 B2 JP5431073 B2 JP 5431073B2 JP 2009200756 A JP2009200756 A JP 2009200756A JP 2009200756 A JP2009200756 A JP 2009200756A JP 5431073 B2 JP5431073 B2 JP 5431073B2
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Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Non-Insulated Conductors (AREA)
Description
基材(又は基板)としては、基材を形成(又は構成)する材質が、有機材料(有機素材)である限り、用途に応じて適宜選択できる。
金属コロイド粒子は、金属ナノ粒子と、この金属ナノ粒子を被覆する保護コロイドで構成された金属コロイド粒子であって、前記保護コロイドは、通常、カルボキシル基を有する有機化合物と、高分子分散剤という特定の組み合わせで構成されている。このような保護コロイドで被覆された金属ナノ粒子を用いることにより、高い密着性で金属膜を形成できる。しかも、樹脂バインダーのような特別な添加剤を必要とせず、金属ナノ粒子の焼結性が高いため、バルク又はそれに近い導電性を有する金属膜を形成できる。また、前記金属コロイド粒子は、前記特定の保護コロイドの組み合わせにより、粗大粒子が少ないにもかかわらず、金属ナノ粒子の割合を大きくでき、金属コロイド粒子(およびその分散液)の保存安定性にも優れている。
金属ナノ粒子を構成する金属(金属原子)としては、例えば、遷移金属(例えば、チタン、ジルコニウムなどの周期表第4A族金属;バナジウム、ニオブなどの周期表第5A族金属;モリブデン、タングステンなどの周期表第6A族金属;マンガンなどの周期表第7A族金属;鉄、ニッケル、コバルト、ルテニウム、ロジウム、パラジウム、レニウム、イリジウム、白金などの周期表第8族金属;銅、銀、金などの周期表第1B族金属など)、周期表第2B族金属(例えば、亜鉛、カドミウムなど)、周期表第3B族金属(例えば、アルミニウム、ガリウム、インジウムなど)、周期表第4B族金属(例えば、ゲルマニウム、スズ、鉛など)、周期表第5B族金属(例えば、アンチモン、ビスマスなど)などが挙げられる。金属は、周期表第8族金属(鉄、ニッケル、ロジウム、パラジウム、白金など)、周期表第1B族金属(銅、銀、金など)、周期表第3B族金属(アルミニウムなど)及び周期表第4B族金属(スズなど)などであってもよい。なお、金属(金属原子)は、保護コロイドに対する配位性の高い金属、例えば、周期表第8族金属、周期表第1B族金属などである場合が多い。
保護コロイドは、カルボキシル基を有する有機化合物と、高分子分散剤とで構成されている。
有機化合物は、カルボキシル基を有している。このようなカルボキシル基の数は、有機化合物1分子あたり、1以上であれば特に限定されず、例えば、1〜10、好ましくは1〜5、さらに好ましくは1〜3程度であってもよい。
高分子分散剤(又は高分子型分散剤)としては、金属ナノ粒子を被覆可能であれば特に限定されないが、両親媒性の高分子分散剤(又はオリゴマー型分散剤)を好適に使用できる。
基材に塗膜(金属膜の前駆体)を形成するための分散液は、前記金属コロイド粒子および溶媒を含んでいる。なお、溶媒は、新たに混合してもよく、少なくとも後述の金属コロイド粒子の製造において使用する溶媒で構成してもよく、これらを組み合わせてもよい。
金属コロイド粒子(又は前記分散液)は、慣用の方法、例えば、前記金属ナノ粒子に対応する金属化合物を、保護コロイド(および必要に応じて前記他の保護コロイド)および還元剤の存在下、溶媒中で還元することにより調製できる。
本発明の導電性基材(又は金属複合膜)は、前記基材と、この基材上に形成された金属膜とで構成されており、この金属膜は、前記金属コロイド粒子を含む分散液の塗膜を焼結した膜(焼結膜、焼結パターン)である。
(I)銀コロイド粒子の作製
硝酸銀66.8g、カルボキシル基を有する有機化合物(B1)として酢酸(和光純薬工業(株)製、沸点118℃、炭素数2)10g、および高分子分散剤(B2)としてポリアクリル酸(和光純薬工業(株)製、重合度5000、酸価780mgKOH/g)3.0gを、イオン交換水1000gに投入し、激しく撹拌した。これに2−ジメチルアミノエタノール(和光純薬工業(株)製)100gを加えたのち、70℃で2時間加熱撹拌。この反応物を高速遠心分離器((株)コクサン(Kokusan)製、H−200 SERIES)を用い、7000rpm、1時間遠心分離し、銀ナノ粒子が保護コロイドにより保護された銀コロイド粒子(一次粒子径1〜100nm、個数平均粒子径20nm)が凝集した沈殿物を回収した。なお、銀ナノ粒子の粒径は、透過型電子顕微鏡(TEM)により測定した。
銀コロイド粒子に含まれる保護コロイド(分散剤)(B)の量をTG−DTAで測定(一分間に10℃の速さで30℃から550℃まで昇温した時の質量減少から算出)したところ5.3質量%であり、(B1)/(B2)(質量比)は25/75であった。なお、(B1)/(B2)の比は、まず(B1)量を30℃から200℃までの質量減少から算出し、(B2)を(B)−(B1)から算出し、これらの値から求めた。
合成例1で得た銀コロイド粒子に、エチレングリコール(極性パラメータ6.9)を加えて作製した銀濃度80%のペーストを、ポリエチレンテレフタレート(PET)フィルム(東洋紡績(株)製、品番A−4300、ポリエステル易接着層が表面に形成されたフィルム)の易接着層が形成された面上に、アプリケータを用いて塗布し、120℃で30分間焼成した。形成された銀膜の厚みは15μmであった。比抵抗を測定したところ30μΩ・cmであった。銀膜を碁盤目に、1mm間隔で10個×10個の計100個のマスでクロスカットし、テープ剥離試験を行ったところ、100/100で剥がれず(すなわち、どのマスも剥がれず)強固に密着していた。また鉛筆硬度(膜の表面を硬度の異なる鉛筆の芯で5回引っかき、その膜に「破れ」、「基板からの剥がれ」が生じる直前の芯の硬度)は3H以上であった。
有機化合物(B1)としてプロピオン酸(和光純薬工業(株)製、沸点141℃、炭素数3)を用い、高分子分散剤(B2)として7.2gのディスパービック190(ビックケミー社製、親水性ユニットであるポリエチレンオキサイド鎖と疎水性ユニットであるアルキル基とを有する両親媒性分散剤、酸価10mgKOH/g、水60%含有)を用いる以外は、実施例1と同様に行った。保護コロイド(B)の量は5.5質量%であり、(B1)/(B2)(質量比)は18/82であった。焼成後形成された銀膜の厚みは15μmであった。比抵抗を測定したところ18μΩ・cmであった。銀膜を碁盤目に、1mm間隔で10個×10個の計100個のマスでクロスカットし、テープ剥離試験を行ったところ、100/100で剥がれず(すなわち、どのマスも剥がれず)強固に密着していた。また鉛筆硬度は3H以上であった。
有機化合物(B1)としてギ酸(和光純薬工業(株)製、沸点100.7℃、炭素数1)を用いる以外は、実施例2と同様に行った。なお、保護コロイド(B)の量は4.3質量%であり、(B1)/(B2)(質量比)は15/85であった。焼成後形成された銀膜の厚みは15μmであった。比抵抗を測定したところ12μΩ・cmであった。銀膜を碁盤目に、1mm間隔で10個×10個の計100個のマスでクロスカットし、テープ剥離試験を行ったところ、100/100で剥がれず(すなわち、どのマスも剥がれず)強固に密着していた。また鉛筆硬度は3H以上であった。
有機化合物(B1)としてコール酸(和光純薬工業(株)製、分解温度198℃)を用いる以外は、実施例2と同様に行った。なお、保護コロイド(B)の量は7.3質量%であり、(B1)/(B2)(質量比)は28/72であった。焼成後形成された銀膜の厚みは15μmであった。銀膜を碁盤目に、1mm間隔で10個×10個の計100個のマスでクロスカットし、テープ剥離試験を行ったところ、100/100で剥がれず(すなわち、どのマスも剥がれず)強固に密着していた。また鉛筆硬度は3H以上であった。
高分子分散剤(B2)として0.12gのディスパービック190を用いる以外は、実施例1と同様に行った。なお、保護コロイド(B)の量は1.5質量%であり、(B1)/(B2)(質量比)は86/14であった。焼成後形成された銀膜の厚みは15μmであった。比抵抗を測定したところ7.0μΩ・cmであった。銀膜を碁盤目に、1mm間隔で10個×10個の計100個のマスでクロスカットし、テープ剥離試験を行ったところ、100/100で剥がれず(すなわち、どのマスも剥がれず)強固に密着していた。また鉛筆硬度は3H以上であった。
高分子分散剤(B2)として0.72gのディスパービック190を用いる以外は、実施例1と同様に行った。なお、保護コロイド(B)の量は1.9質量%であり、(B1)/(B2)(質量比)は53/47であった。焼成後形成された銀膜の厚みは15μmであった。比抵抗を測定したところ8μΩ・cmであった。銀膜を碁盤目に、1mm間隔で10個×10個の計100個のマスでクロスカットし、テープ剥離試験を行ったところ、100/100で剥がれず(すなわち、どのマスも剥がれず)強固に密着していた。また鉛筆硬度は3H以上であった。
高分子分散剤(B2)として2.12gのディスパービック190を用いる以外は、実施例1と同様に行った。なお、保護コロイド(B)の量は2.4質量%であり、(B1)/(B2)(質量比)は35/65であった。焼成後形成された銀膜の厚みは15μmであった。比抵抗を測定したところ10μΩ・cmであった。銀膜を碁盤目に、1mm間隔で10個×10個の計100個のマスでクロスカットし、テープ剥離試験を行ったところ、100/100で剥がれず(すなわち、どのマスも剥がれず)強固に密着していた。また鉛筆硬度は3H以上であった。
高分子分散剤(B2)として5.04gのディスパービック190を用いる以外は、実施例1と同様に行った。なお、保護コロイド(B)の量は3.9質量%であり、(B1)/(B2)(質量比)は20/80であった。焼成後形成された銀膜の厚みは15μmであった。比抵抗を測定したところ11μΩ・cmであった。銀膜を碁盤目に、1mm間隔で10個×10個の計100個のマスでクロスカットし、テープ剥離試験を行ったところ、100/100で剥がれず(すなわち、どのマスも剥がれず)強固に密着していた。また鉛筆硬度は3H以上であった。
高分子分散剤(B2)として7.2gのディスパービック190を用いる以外は、実施例1と同様に行った。なお、保護コロイド(B)の量は5.0質量%であり、(B1)/(B2)(質量比)は23/77であった。焼成後形成された銀膜の厚みは15μmであった。比抵抗を測定したところ14μΩ・cmであった。銀膜を碁盤目に、1mm間隔で10個×10個の計100個のマスでクロスカットし、テープ剥離試験を行ったところ、100/100で剥がれず(すなわち、どのマスも剥がれず)強固に密着していた。また鉛筆硬度は3H以上であった。
Claims (3)
- 有機素材で形成された基材に、金属ナノ粒子と、この金属ナノ粒子を被覆する保護コロイドとで構成された金属コロイド粒子を含む分散液であって、前記保護コロイドの割合が、前記金属ナノ粒子100質量部に対して1.0〜60質量部であり、前記保護コロイドが、酢酸と、高分子分散剤とで構成され、かつ酢酸と高分子分散剤との割合が、前者/後者(質量比)=99/1〜5/95である分散液をコーティングした後、得られた前駆体を150℃以下で熱処理して金属膜を形成させ、導電性基材を製造する方法。
- 金属ナノ粒子を構成する金属が、少なくとも貴金属を含む金属である請求項1記載の方法。
- 高分子分散剤が、カルボキシル基又はアミノ基を有する請求項1又は2記載の方法。
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JP5697964B2 (ja) * | 2010-12-17 | 2015-04-08 | 丸善石油化学株式会社 | 光硬化性組成物並びにこれを用いた金属ナノ粒子分散膜及び導電性薄膜の製造方法 |
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