JP5700864B2 - 銅微粒子分散液、導電膜形成方法及び回路基板 - Google Patents
銅微粒子分散液、導電膜形成方法及び回路基板 Download PDFInfo
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- JP5700864B2 JP5700864B2 JP2013102916A JP2013102916A JP5700864B2 JP 5700864 B2 JP5700864 B2 JP 5700864B2 JP 2013102916 A JP2013102916 A JP 2013102916A JP 2013102916 A JP2013102916 A JP 2013102916A JP 5700864 B2 JP5700864 B2 JP 5700864B2
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- copper fine
- copper
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- 229910052802 copper Inorganic materials 0.000 title claims description 191
- 239000010949 copper Substances 0.000 title claims description 191
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims description 189
- 239000010419 fine particle Substances 0.000 title claims description 153
- 239000006185 dispersion Substances 0.000 title claims description 90
- 238000000034 method Methods 0.000 title claims description 15
- 238000005245 sintering Methods 0.000 claims description 83
- 239000000758 substrate Substances 0.000 claims description 54
- 239000002612 dispersion medium Substances 0.000 claims description 40
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 16
- 239000005751 Copper oxide Substances 0.000 claims description 15
- -1 acetylene glycol Chemical compound 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 15
- 229910000431 copper oxide Inorganic materials 0.000 claims description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 8
- 239000004642 Polyimide Substances 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 7
- 229920001721 polyimide Polymers 0.000 claims description 7
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 5
- 239000002585 base Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 150000003568 thioethers Chemical class 0.000 claims description 5
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 14
- 239000002245 particle Substances 0.000 description 14
- 238000001035 drying Methods 0.000 description 11
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000010452 phosphate Substances 0.000 description 5
- 238000010301 surface-oxidation reaction Methods 0.000 description 5
- 239000004952 Polyamide Substances 0.000 description 4
- 150000001879 copper Chemical class 0.000 description 4
- 229920002647 polyamide Polymers 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000004962 Polyamide-imide Substances 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 3
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 229920002312 polyamide-imide Polymers 0.000 description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 229920003080 Povidone K 25 Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000011889 copper foil Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000000206 photolithography Methods 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 description 1
- CYSGHNMQYZDMIA-UHFFFAOYSA-N 1,3-Dimethyl-2-imidazolidinon Chemical compound CN1CCN(C)C1=O CYSGHNMQYZDMIA-UHFFFAOYSA-N 0.000 description 1
- CRWNQZTZTZWPOF-UHFFFAOYSA-N 2-methyl-4-phenylpyridine Chemical compound C1=NC(C)=CC(C=2C=CC=CC=2)=C1 CRWNQZTZTZWPOF-UHFFFAOYSA-N 0.000 description 1
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920003082 Povidone K 90 Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 150000003009 phosphonic acids Chemical class 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- YODZTKMDCQEPHD-UHFFFAOYSA-N thiodiglycol Chemical compound OCCSCCO YODZTKMDCQEPHD-UHFFFAOYSA-N 0.000 description 1
- 229950006389 thiodiglycol Drugs 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Description
焼結進行剤を含有する。焼結進行剤は、常温より高い温度で銅から銅酸化物を除去する化合物である。銅酸化物は、酸化銅(I)及び酸化銅(II)である。常温より高いこのような温度は、銅微粒子を光焼結するための光の照射によってもたらされる。
実施例1と同じ銅微粒子分散液と基板を用いた。この基板上に膜厚1μmの皮膜を形成した。皮膜の色は黒色であった。皮膜を乾燥した後、皮膜に光を照射した。光の照射前に皮膜を乾燥したので、分散媒は焼結進行剤として機能しない。光照射のエネルギーは、実施例1と同じとした。
分散媒としてジエチレングリコールジブチルエーテルを用い、平均粒子径が70nmの銅微粒子を用いて、銅微粒子分散液を作った。分散剤も焼結進行剤も分散媒に添加しなかった。銅微粒子の濃度は、40質量%とした。この銅微粒子分散液は、銅微粒子の安定分散性が低く、銅微粒子は、かき混ぜた後しばらくの間は分散したが、1時間程度で沈殿した。基板として、実施例3と同じガラス基板を用いた。この基板上に銅微粒子分散液から成る皮膜を形成した。皮膜を乾燥した後、皮膜に光を照射した。光照射のエネルギーは、11J/cm2とした。光の照射によって、凝集した銅微粒子が多くの塊として基板上に残った状態となった。このような状態は、「吹き飛び(blow-off)」と呼ばれる。銅微粒子の焼結はある程度進行したが、導電膜は形成されなかった。
分散媒としてn−ヘキサンを用いた。分散剤としてリン酸エステル(商品名「DISPERBYK(登録商標)−102」)を用いた。分散剤の濃度は、銅微粒子分散液に対して2質量%とした。それ以外の条件を比較例2と同じにした。基板上に銅微粒子分散液から成る皮膜を形成した。皮膜を乾燥した後、皮膜に光を照射した。光の照射後、基板上の皮膜は、黒色であり、そのシート抵抗は、1Ω/sqという高い値であった。光照射エネルギーを11J/cm2より高くすると、皮膜の色が青色に変化し、皮膜の表面酸化が起こった。
分散媒として1,3−ジメチル−2−イミダゾリジノンを用いた。それ以外の条件を比較例3と同じにした。光の照射後、基板上の皮膜は、黒色であり、そのシート抵抗は、1Ω/sqであった。光照射エネルギーを11J/cm2より高くすると、皮膜の色が青色に変化し、皮膜の表面酸化が起こった。
分散媒としてN−メチルピロリドンを用いた。それ以外の条件を比較例4と同じにした。光の照射後、基板上の皮膜は、黒色であり、そのシート抵抗は、1Ω/sqであった。光照射エネルギーを11J/cm2より高くすると、皮膜の色が青色に変化し、皮膜の表面酸化が起こった。
分散媒として炭酸プロピレンを用いた。それ以外の条件を比較例5と同じにした。光の照射後、基板上の皮膜は、黒色であり、そのシート抵抗は、1Ω/sqであった。光照射エネルギーを11J/cm2より高くすると、皮膜の色が青色に変化し、皮膜の表面酸化が起こった。
分散媒として水を用いた。分散剤として、酸基を有する共重合物のアルキロールアンモニウム塩(商品名「DISPERBYK(登録商標)−180」)を用いた。それ以外の条件を比較例6と同じにした。作った銅微粒子分散液は、銅微粒子の水への溶解が進行するため、1日後には青色の液体になった。このため、銅微粒子分散液を作成後速やかに使用した。光の照射後、基板上の皮膜は、黒色であり、そのシート抵抗は、1Ω/sqであった。光照射エネルギーを11J/cm2より高くすると、皮膜の色が青色に変化し、皮膜の表面酸化が起こった。
11 銅微粒子
2 皮膜
3 基材
4 導電膜
Claims (4)
- 分散媒と、前記分散媒中に分散された銅微粒子とを有する銅微粒子分散液であって、
焼結進行剤を含有し、
前記焼結進行剤は、常温より高い温度で銅から銅酸化物を除去する化合物であり、常温より高い温度で銅と錯生成する化合物であり、
常温より高い前記温度は、前記銅微粒子を光焼結するための光の照射によってもたらされ、
前記化合物は、ポリアミドイミド、ポリイミド、ホスホン酸、β−ジケトン、アセチレングリコール、チオエーテル、及び硫酸エステルよりなる群から選ばれることを特徴とする銅微粒子分散液。 - 分散媒と、前記分散媒中に分散された銅微粒子とを有する銅微粒子分散液であって、
焼結進行剤を含有し、
前記焼結進行剤は、常温より高い温度で銅から銅酸化物を除去する化合物であり、常温より高い温度で銅酸化物を溶解するアルカリであり、
常温より高い前記温度は、前記銅微粒子を光焼結するための光の照射によってもたらされ、
前記アルカリは、水酸化カリウムであることを特徴とする銅微粒子分散液。 - 請求項1又は請求項2に記載の銅微粒子分散液から成る皮膜を基材上に形成する工程と、
前記皮膜に光を照射することによって、その皮膜中の銅微粒子を光焼結して導電膜を形成する工程とを有することを特徴とする導電膜形成方法。 - 請求項3に記載の導電膜形成方法によって形成された導電膜を有する回路を前記基材から成る基板上に備えることを特徴とする回路基板。
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