JP5449154B2 - レーザー照射による電気伝導性銅パターン層の形成方法 - Google Patents
レーザー照射による電気伝導性銅パターン層の形成方法 Download PDFInfo
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- 239000010949 copper Substances 0.000 title claims abstract description 116
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 99
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims description 29
- 239000002245 particle Substances 0.000 claims abstract description 144
- 239000006185 dispersion Substances 0.000 claims abstract description 24
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 230000001678 irradiating effect Effects 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000007639 printing Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims description 14
- 239000004094 surface-active agent Substances 0.000 claims description 13
- 230000015572 biosynthetic process Effects 0.000 claims description 11
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- -1 copper carboxyl compound Chemical class 0.000 claims description 9
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 238000010304 firing Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 7
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 150000001879 copper Chemical class 0.000 claims description 4
- 239000002612 dispersion medium Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 235000011837 pasties Nutrition 0.000 claims 1
- 239000011882 ultra-fine particle Substances 0.000 claims 1
- 238000000059 patterning Methods 0.000 abstract description 10
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 abstract description 7
- 239000005751 Copper oxide Substances 0.000 abstract description 7
- 229910000431 copper oxide Inorganic materials 0.000 abstract description 7
- 239000012298 atmosphere Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract 2
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 62
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 62
- 229940112669 cuprous oxide Drugs 0.000 description 62
- 239000010419 fine particle Substances 0.000 description 13
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 7
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 2
- 229960005070 ascorbic acid Drugs 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229940116411 terpineol Drugs 0.000 description 2
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 1
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 1
- 239000005750 Copper hydroxide Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910001956 copper hydroxide Inorganic materials 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000007261 regionalization Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
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Description
(ステップ1)銅粒子、酸化銅粒子及びこれらの混合物からなる群より選択された銅系粒子の分散液を用意する段階;
(ステップ2)前記銅系粒子の分散液を基材に所定形状で印刷または充填して銅系粒子パターン層を形成する段階;及び
(ステップ3)前記銅系粒子パターン層にレーザーを照射し、前記銅系粒子パターン層に含まれた銅系粒子を焼成しながら相互連結させる段階を含む。
(R1‐COO)2Cu
化学式1において、R1は炭素数が1ないし18のアルキル基である。
R1‐COOH
化学式2において、R1は炭素数が1ないし18のアルキル基である。
ある弱還元剤を投入して、平均粒径が1ないし100nmであって粒径の標準偏差が0ないし10%である複数のCu2O微粒子が相互凝集して形成され、その平均粒径が0.1ないし10μmであって粒径の標準偏差が0ないし40%である球形のCu2O凝集体粒子を形成する。凝集体粒子及び酸化第一銅微粒子の大きさは、溶媒の種類、界面活性剤の添加などの反応条件を変化させて調節することができる。弱還元剤は銅(II)前駆体を溶
媒に溶解させる前に先に投入することもでき、別の溶媒に弱還元剤を溶解させた後、銅(II)前駆体溶液に投入することもできる。弱還元剤としては、酸化第一銅凝集体粒子を均
一に形成するため、標準還元電位が−0.2ないし−0.05Vである弱還元剤を使用する。このような弱還元剤としては、アスコルビン酸、ジオール化合物、クエン酸、フルクトース(fructose)、アミン化合物、α‐ヒドロキシケトン(α‐hydroxy ketone)化合物、コハク酸、マルトース(maltose)などをそれぞれ単独でまたはこれらのうち2種以上を混合して使用することができる。
界面活性剤をさらに添加することができる。界面活性剤の種類及び使用量などによって凝集体粒子の大きさが調節される。添加された界面活性剤は球形の酸化第一銅凝集体粒子の表面に被覆される形態で存在する。界面活性剤としては、1つの分子内に親水性基と親油性基を共に持つ両親媒性物質であって、酸化第一銅粒子の製造に使用される通常の界面活性剤を使用することができる。例えば、−OH、−COOH、−SH、−NHなどの官能基を1つ以上持つ低分子界面活性剤、または、ポリアクリルアミド、ポリビニルピロリドン、ポリビニルアルコールのような高分子界面活性剤を使用でき、これらをそれぞれ単独でまたはこれらのうち2種以上を混合して使用することができる。特に、界面活性剤としてポリアクリルアミドを使用すれば、得られる酸化第一銅凝集体粒子の形状と大きさが一層均一になり、粒径の標準偏差が非常に低くなった球形の酸化第一銅凝集体粒子を得ることができる。
(CH3COO)2Cu・H2O 50mgとポリアクリルアミド200mgを蒸溜水4.5mlに溶解して第1溶液を用意し、アスコルビン酸22mgを蒸溜水0.5mlに溶解して第2溶液を用意した。室温、常圧、及び空気中で、用意した2つの溶液を混合して10分間静置した。次いで、2000rpmで3分間遠心分離した後、上層の上澄み液を捨てて残った沈殿物を水20mlに再分散した後、遠心分離過程をさらに一回行って酸化第一銅粒子を得た。
[実施例1]
前述した方法で製造した酸化第一銅凝集体粒子をテルピネオールに分散させて固形分の含量が50〜85重量比になるように分散液を製造した。次いで、スクリーン印刷法を用いてポリエチレンテレフタレート基板上に厚さが10〜20μmであって幅が2mmである線を印刷した後、40kHz、60%/0.01m/sec/0.2mm mesh/6mm オフセットの条件でレーザーを照射して焼成した。得られた銅線の比抵抗値を測定した結果、4.96E−4Ωmであった。
レーザーの照射条件を40kHz、60%/0.01m/sec/0.02mm mesh/3mm オフセットに変化させたことを除き、実施例1と同様の方法で行った。得られた銅線の比抵抗値を測定した結果、3.96E−5Ωmの比抵抗値が得られた。
Claims (5)
- (ステップ1)下記化学式1で表される銅カルボキシル化合物または下記化学式2で表されるカルボキシル基含有化合物と銅塩とを溶媒に溶解させてCu 2 O前駆体溶液を製造し、
[化学式1]
(R 1 −COO) 2 Cu
化学式1において、R 1 は炭素数が1ないし18のアルキル基である。
[化学式2]
R 1 −COOH
化学式2において、R 1 は炭素数が1ないし18のアルキル基である。
前記Cu 2 O前駆体溶液に標準還元電位が−0.2ないし−0.05Vである弱還元剤を投入して、平均粒径が1ないし100nmであって粒径の標準偏差が0ないし10%である複数のCu 2 O超微粒子が相互凝集して形成され、その平均粒径が0.1ないし10μmであって、前記粒子の縦横比が、1以上2以下である球形のCu 2 O凝集体粒子を形成し、前記球形のCu 2 O凝集体粒子の分散液を用意する段階;
(ステップ2)前記Cu 2 O凝集体粒子の分散液を基材に所定形状で印刷または充填してパターン層を形成する段階;
(ステップ3)空気中で前記パターン層にレーザーを照射し、前記パターン層に含まれたCu 2 O凝集体粒子を焼成しながら相互連結させ電気伝導性銅パターンに変化させる段階を含む電気伝導性銅パターン層の形成方法。 - 前記Cu 2 O凝集体粒子の表面が界面活性剤で被覆されていることを特徴とする請求項1に記載の電気伝導性銅パターン層の形成方法。
- 前記界面活性剤は−OH、−COOH、−SH及び−NHからなる群より選択された少なくとも1つの官能基を持つ低分子、ポリアクリルアミド、ポリビニルピロリドン及びポリビニルアルコールからなる群より選択されたいずれか1つまたはこれらのうち2種以上の混合物であることを特徴とする請求項2に記載の電気伝導性銅パターン層の形成方法。
- 前記界面活性剤はポリアクリルアミドであることを特徴とする請求項3に記載の電気伝導性銅パターン層の形成方法。
- 前記Cu 2 O凝集体粒子の分散液は、前記Cu 2 O凝集体粒子が分散媒に分散された液状の分散液または前記Cu 2 O凝集体粒子がバインダー樹脂溶液に分散されたペースト状の分散液であることを特徴とする請求項1〜4のいずれかに記載の電気伝導性銅パターン層の形成方法。
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KR20200015609A (ko) | 2017-07-18 | 2020-02-12 | 아사히 가세이 가부시키가이샤 | 도전성 패턴 영역을 갖는 구조체 및 그 제조 방법, 적층체 및 그 제조 방법, 그리고 구리 배선 |
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