JP2014166939A5 - - Google Patents
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- JP2014166939A5 JP2014166939A5 JP2013225296A JP2013225296A JP2014166939A5 JP 2014166939 A5 JP2014166939 A5 JP 2014166939A5 JP 2013225296 A JP2013225296 A JP 2013225296A JP 2013225296 A JP2013225296 A JP 2013225296A JP 2014166939 A5 JP2014166939 A5 JP 2014166939A5
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- Prior art keywords
- copper
- fine particles
- nitride fine
- copper nitride
- particles according
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- 239000010419 fine particle Substances 0.000 claims description 17
- DOIHHHHNLGDDRE-UHFFFAOYSA-N azanide;copper;copper(1+) Chemical compound [NH2-].[Cu].[Cu].[Cu+] DOIHHHHNLGDDRE-UHFFFAOYSA-N 0.000 claims description 16
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 239000011164 primary particle Substances 0.000 claims description 2
- 239000010949 copper Substances 0.000 description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- -1 ammonium salt compounds Chemical class 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000002904 solvent Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 150000001879 copper Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 239000003223 protective agent Substances 0.000 description 2
- 239000011163 secondary particle Substances 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001540 azides Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- SXBOEBVXYQFVJM-UHFFFAOYSA-L copper;2-azanidylpentanedioate Chemical compound [Cu+2].[O-]C(=O)C([NH-])CCC([O-])=O SXBOEBVXYQFVJM-UHFFFAOYSA-L 0.000 description 1
- 239000002612 dispersion media Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Description
すなわち、本発明は上記の問題を解決するために、以下の発明を提供するものである。
（１）一次粒子の粒径が１〜１００ｎｍであり、かつ分解温度が常圧で３００℃以下である窒化銅微粒子。
（２）二次粒子の粒径が１μｍ以下である上記（１）に記載の窒化銅微粒子。
（３）示差熱天秤分析において７０℃〜３００℃の範囲に重量減少を伴う分解温度を持つ上記（１）または（２）に記載の窒化銅微粒子。
（４）電子顕微鏡観察において、二次粒子が球状である上記（１）〜（３）のいずれかに記載の窒化銅微粒子。
（５）粉末Ｘ線回折において、ＣｕＫα線で２１．５〜２４．５°および３１．０〜３４．０°、３９．０〜４２．０°、４６．０〜４９．０°のいずれかの領域に少なくとも一つ以上の窒化銅由来の回折ピークを持つ上記（１）〜（４）のいずれかに記載の窒化銅微粒子。
（６）銅源および窒素源、または銅源、窒素源および保護剤を、溶媒または分散媒に溶解または分散させ、ついで加熱することにより上記（１）〜（５）のいずれかに記載の窒化銅微粒子を製造することを特徴とする窒化銅微粒子の製造方法。
（７）銅源が、無機銅塩、有機銅塩および銅錯体から選ばれる１種以上を含む上記（６）に記載の窒化銅微粒子の製造方法。
（８）窒素源が、アンモニアガスまたはアンモニウム塩化合物、尿素、尿素誘導体化合物、硝酸塩化合物、アミン化合物、およびアジ化化合物から選ばれる１種以上を含む上記（６）または（７）に記載の窒化銅微粒子の製造方法。
（９）銅源および窒素源が、結合または配位した窒素含有銅錯体である上記（６）〜（８）のいずれかに記載の窒化銅微粒子の製造方法。
（１０）保護剤が、少なくとも１つ以上のカルボキシル基、アミノ基および／またはヒドロキシル基を有する化合物であることを特徴とする上記（６）〜（９）のいずれかに記載の窒化銅微粒子の製造方法。
（１１）溶媒が、沸点１００℃以上の有機溶媒である上記（６）〜（１０）のいずれかに記載の窒化銅微粒子の製造方法。
（１２）加熱温度が１００〜２５０℃である上記（６）〜（１１）のいずれかに記載の窒化銅微粒子の製造方法。
（１３）溶媒に対する銅源の濃度が、Ｃｕ１＋またはＣｕ２＋換算で０．０００１〜１ ｍｏｌ／Ｌの濃度である上記（６）〜（１２）のいずれかに記載の窒化銅微粒子の製造方法。
（１４）上記（１）に記載の窒化銅微粒子を含む配線用インク材料。
（１５）上記（１４）に記載の配線用インク材料を塗布してなる被印刷基材。
（１６）上記（１５）に記載の被印刷基材を加熱することにより、窒化銅微粒子から金属銅膜が形成されてなる被印刷基材。
That is, the present invention provides the following inventions in order to solve the above problems.
(1) Copper nitride fine particles having a primary particle size of 1 to 100 nm and a decomposition temperature of 300 ° C. or less at normal pressure .
(2) The copper nitride fine particles according to (1), wherein the secondary particles have a particle size of 1 μm or less.
(3) The copper nitride fine particles according to the above (1) or (2) having a decomposition temperature accompanied by weight loss in the range of 70 ° C. to 300 ° C. in differential thermal balance analysis.
(4) The copper nitride fine particles according to any one of (1) to (3), wherein the secondary particles are spherical in electron microscope observation.
(5) In powder X-ray diffraction, any of 21.5 to 24.5 °, 31.0 to 34.0 °, 39.0 to 42.0 °, and 46.0 to 49.0 ° with CuKα ray The copper nitride fine particles according to any one of the above (1) to (4), which have a diffraction peak derived from at least one copper nitride in the region.
(6) The nitriding according to any one of (1) to (5) above, wherein a copper source and a nitrogen source, or a copper source, a nitrogen source and a protective agent are dissolved or dispersed in a solvent or a dispersion medium and then heated. A method for producing copper nitride fine particles, comprising producing copper fine particles.
(7) The manufacturing method of the copper nitride fine particle as described in said (6) in which a copper source contains 1 or more types chosen from inorganic copper salt, organic copper salt, and a copper complex.
(8) The nitriding as described in (6) or (7) above, wherein the nitrogen source contains one or more selected from ammonia gas or ammonium salt compounds, urea, urea derivative compounds, nitrate compounds, amine compounds, and azide compounds A method for producing copper fine particles.
(9) The method for producing copper nitride fine particles according to any one of (6) to (8), wherein the copper source and the nitrogen source are bonded or coordinated nitrogen-containing copper complexes.
(10) The copper nitride fine particles according to any one of (6) to (9) above, wherein the protective agent is a compound having at least one carboxyl group, amino group and / or hydroxyl group. Production method.
(11) The method for producing copper nitride fine particles according to any one of (6) to (10), wherein the solvent is an organic solvent having a boiling point of 100 ° C. or higher.
(12) The method for producing copper nitride fine particles according to any one of (6) to (11), wherein the heating temperature is 100 to 250 ° C.
(13) The method for producing copper nitride fine particles according to any one of (6) to (12), wherein the concentration of the copper source with respect to the solvent is a concentration of 0.0001 to 1 mol / L in terms of Cu 1+ or Cu 2+. .
(14) A wiring ink material containing the copper nitride fine particles according to (1).
(15) A substrate to be printed formed by applying the wiring ink material according to (14).
(16) A substrate to be printed, in which a metal copper film is formed from copper nitride fine particles by heating the substrate to be printed according to (15).
Claims (1)
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2013225296A JP6057379B2 (en) | 2013-01-31 | 2013-10-30 | Copper nitride fine particles and method for producing the same |
| CN201480006826.7A CN104981427A (en) | 2013-01-31 | 2014-01-31 | Fine copper nitride particles and production method therefor |
| KR1020157020804A KR20150112984A (en) | 2013-01-31 | 2014-01-31 | Fine copper nitride particles and production method therefor |
| PCT/JP2014/052321 WO2014119748A1 (en) | 2013-01-31 | 2014-01-31 | Fine copper nitride particles and production method therefor |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2013017510 | 2013-01-31 | ||
| JP2013017510 | 2013-01-31 | ||
| JP2013225296A JP6057379B2 (en) | 2013-01-31 | 2013-10-30 | Copper nitride fine particles and method for producing the same |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| JP2014166939A JP2014166939A (en) | 2014-09-11 |
| JP2014166939A5 true JP2014166939A5 (en) | 2016-06-23 |
| JP6057379B2 JP6057379B2 (en) | 2017-01-11 |
Family
ID=51262445
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2013225296A Expired - Fee Related JP6057379B2 (en) | 2013-01-31 | 2013-10-30 | Copper nitride fine particles and method for producing the same |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP6057379B2 (en) |
| KR (1) | KR20150112984A (en) |
| CN (1) | CN104981427A (en) |
| WO (1) | WO2014119748A1 (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015147561A1 (en) * | 2014-03-26 | 2015-10-01 | 전자부품연구원 | Composite material with which conductor pattern can easily be formed, method for manufacturing the composite material, copper nitride seed material of the composite material and method for synthesising the copper nitride |
| JP6574553B2 (en) * | 2014-06-26 | 2019-09-11 | 昭和電工株式会社 | Conductive pattern forming composition and conductive pattern forming method |
| RU2647055C1 (en) * | 2017-07-11 | 2018-03-13 | Юлия Алексеевна Щепочкина | Steel |
| RU2647056C1 (en) * | 2017-07-11 | 2018-03-13 | Юлия Алексеевна Щепочкина | Steel |
| KR102303767B1 (en) * | 2017-11-01 | 2021-09-23 | 한국전자기술연구원 | Method for manufacturing copper nitride powder for conductor pattern |
| CN110642304B (en) * | 2019-10-09 | 2021-12-31 | 上海师范大学 | Trimetal nitride material for super capacitor and preparation method thereof |
| CN111450867A (en) * | 2020-05-09 | 2020-07-28 | 青岛科技大学 | Cu for electrocatalytic carbon dioxide reduction3Preparation method of N nano catalyst |
| CN115057417B (en) * | 2022-06-08 | 2023-09-12 | 安徽大学 | Preparation of copper nitride nano-sheet and application of copper nitride nano-sheet in formate electrosynthesis |
| CN116516280A (en) * | 2023-04-27 | 2023-08-01 | 常州大学 | Efficient and energy-saving workpiece nitriding method |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005122230A1 (en) * | 2004-06-07 | 2005-12-22 | Kyushu Institute Of Technology | Method for processing copper surface, method for forming copper pattern wiring and semiconductor device manufactured using such method |
| JP3870273B2 (en) * | 2004-12-28 | 2007-01-17 | 国立大学法人九州工業大学 | Copper pattern wiring formation method, semiconductor device created using the method, and nano copper metal particles |
| JP5778382B2 (en) * | 2008-10-22 | 2015-09-16 | 東ソー株式会社 | Composition for producing metal film, method for producing metal film, and method for producing metal powder |
| JP5243510B2 (en) * | 2010-10-01 | 2013-07-24 | 富士フイルム株式会社 | Wiring material, wiring manufacturing method, and nanoparticle dispersion |
-
2013
- 2013-10-30 JP JP2013225296A patent/JP6057379B2/en not_active Expired - Fee Related
-
2014
- 2014-01-31 KR KR1020157020804A patent/KR20150112984A/en not_active Application Discontinuation
- 2014-01-31 CN CN201480006826.7A patent/CN104981427A/en active Pending
- 2014-01-31 WO PCT/JP2014/052321 patent/WO2014119748A1/en active Application Filing
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