JP2012523499A - Method for producing metal nanostructure using ionic liquid - Google Patents
Method for producing metal nanostructure using ionic liquid Download PDFInfo
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- JP2012523499A JP2012523499A JP2012504611A JP2012504611A JP2012523499A JP 2012523499 A JP2012523499 A JP 2012523499A JP 2012504611 A JP2012504611 A JP 2012504611A JP 2012504611 A JP2012504611 A JP 2012504611A JP 2012523499 A JP2012523499 A JP 2012523499A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 87
- 239000002184 metal Substances 0.000 title claims abstract description 87
- 239000002608 ionic liquid Substances 0.000 title claims abstract description 59
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 150000003839 salts Chemical class 0.000 claims abstract description 32
- 229920005862 polyol Polymers 0.000 claims abstract description 12
- 150000003077 polyols Chemical class 0.000 claims abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 18
- 150000001450 anions Chemical class 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- 239000002070 nanowire Substances 0.000 claims description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 10
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims description 10
- 150000001449 anionic compounds Chemical class 0.000 claims description 8
- 150000001768 cations Chemical class 0.000 claims description 8
- 125000005842 heteroatom Chemical group 0.000 claims description 8
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 8
- 229910001412 inorganic anion Inorganic materials 0.000 claims description 8
- 150000002891 organic anions Chemical class 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 101710134784 Agnoprotein Proteins 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- -1 alkyl sulphates Chemical class 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- 150000003464 sulfur compounds Chemical class 0.000 claims description 5
- 229910020366 ClO 4 Inorganic materials 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- RAXXELZNTBOGNW-UHFFFAOYSA-O Imidazolium Chemical compound C1=C[NH+]=CN1 RAXXELZNTBOGNW-UHFFFAOYSA-O 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910017464 nitrogen compound Inorganic materials 0.000 claims description 4
- 150000002830 nitrogen compounds Chemical class 0.000 claims description 4
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-O pyridinium Chemical compound C1=CC=[NH+]C=C1 JUJWROOIHBZHMG-UHFFFAOYSA-O 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910016467 AlCl 4 Inorganic materials 0.000 claims description 2
- 229910017008 AsF 6 Inorganic materials 0.000 claims description 2
- 101150003085 Pdcl gene Proteins 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 229910018286 SbF 6 Inorganic materials 0.000 claims description 2
- 229940045714 alkyl sulfonate alkylating agent Drugs 0.000 claims description 2
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 2
- 150000002009 diols Chemical class 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 150000002892 organic cations Chemical class 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- 150000004820 halides Chemical class 0.000 claims 1
- 238000006722 reduction reaction Methods 0.000 abstract description 10
- 239000002243 precursor Substances 0.000 abstract description 6
- 239000002105 nanoparticle Substances 0.000 abstract description 4
- 239000002082 metal nanoparticle Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000002923 metal particle Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- BXSDLSWVIAITRQ-UHFFFAOYSA-M 1-ethyl-3-methylimidazol-3-ium;methyl sulfate Chemical compound COS([O-])(=O)=O.CCN1C=C[N+](C)=C1 BXSDLSWVIAITRQ-UHFFFAOYSA-M 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 239000007810 chemical reaction solvent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 description 2
- XLJSMWDFUFADIA-UHFFFAOYSA-N 1,3-diethylimidazol-1-ium Chemical compound CCN1C=C[N+](CC)=C1 XLJSMWDFUFADIA-UHFFFAOYSA-N 0.000 description 1
- HVVRUQBMAZRKPJ-UHFFFAOYSA-N 1,3-dimethylimidazolium Chemical compound CN1C=C[N+](C)=C1 HVVRUQBMAZRKPJ-UHFFFAOYSA-N 0.000 description 1
- LHGYPGGWEQFVEO-UHFFFAOYSA-N 1-butyl-3,4-dimethylpyridin-1-ium Chemical compound CCCC[N+]1=CC=C(C)C(C)=C1 LHGYPGGWEQFVEO-UHFFFAOYSA-N 0.000 description 1
- KYCQOKLOSUBEJK-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;bromide Chemical compound [Br-].CCCCN1C=C[N+](C)=C1 KYCQOKLOSUBEJK-UHFFFAOYSA-M 0.000 description 1
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 1
- MEMNKNZDROKJHP-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;methyl sulfate Chemical compound COS([O-])(=O)=O.CCCCN1C=C[N+](C)=C1 MEMNKNZDROKJHP-UHFFFAOYSA-M 0.000 description 1
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 1
- DADKKHHMGSWSPH-UHFFFAOYSA-N 1-butyl-3-methylpyridin-1-ium Chemical compound CCCC[N+]1=CC=CC(C)=C1 DADKKHHMGSWSPH-UHFFFAOYSA-N 0.000 description 1
- LDVVBLGHGCHZBJ-UHFFFAOYSA-N 1-decyl-3-methylimidazolium Chemical compound CCCCCCCCCCN1C=C[N+](C)=C1 LDVVBLGHGCHZBJ-UHFFFAOYSA-N 0.000 description 1
- WDRZVZVXHZNSFG-UHFFFAOYSA-N 1-ethenylpyridin-1-ium Chemical compound C=C[N+]1=CC=CC=C1 WDRZVZVXHZNSFG-UHFFFAOYSA-N 0.000 description 1
- REITYCXGQIGALX-UHFFFAOYSA-N 1-ethyl-3-methylpyridin-1-ium Chemical compound CC[N+]1=CC=CC(C)=C1 REITYCXGQIGALX-UHFFFAOYSA-N 0.000 description 1
- BSHUCFSTRUDDGO-UHFFFAOYSA-M 1-ethyl-3-methylpyridin-1-ium;methyl sulfate Chemical compound COS([O-])(=O)=O.CC[N+]1=CC=CC(C)=C1 BSHUCFSTRUDDGO-UHFFFAOYSA-M 0.000 description 1
- OIDIRWZVUWCCCO-UHFFFAOYSA-N 1-ethylpyridin-1-ium Chemical compound CC[N+]1=CC=CC=C1 OIDIRWZVUWCCCO-UHFFFAOYSA-N 0.000 description 1
- RVEJOWGVUQQIIZ-UHFFFAOYSA-N 1-hexyl-3-methylimidazolium Chemical compound CCCCCCN1C=C[N+](C)=C1 RVEJOWGVUQQIIZ-UHFFFAOYSA-N 0.000 description 1
- XOYLEVUBUOACOA-UHFFFAOYSA-N 1-hexyl-3-methylpyridin-1-ium Chemical compound CCCCCC[N+]1=CC=CC(C)=C1 XOYLEVUBUOACOA-UHFFFAOYSA-N 0.000 description 1
- BMKLRPQTYXVGNK-UHFFFAOYSA-N 1-methyl-3-tetradecylimidazol-1-ium Chemical compound CCCCCCCCCCCCCCN1C=C[N+](C)=C1 BMKLRPQTYXVGNK-UHFFFAOYSA-N 0.000 description 1
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 1
- WXMVWUBWIHZLMQ-UHFFFAOYSA-N 3-methyl-1-octylimidazolium Chemical compound CCCCCCCCN1C=C[N+](C)=C1 WXMVWUBWIHZLMQ-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- PQBAWAQIRZIWIV-UHFFFAOYSA-N N-methylpyridinium Chemical compound C[N+]1=CC=CC=C1 PQBAWAQIRZIWIV-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920001464 poly(sodium 4-styrenesulfonate) Polymers 0.000 description 1
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229940083575 sodium dodecyl sulfate Drugs 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- IBWGNZVCJVLSHB-UHFFFAOYSA-M tetrabutylphosphanium;chloride Chemical compound [Cl-].CCCC[P+](CCCC)(CCCC)CCCC IBWGNZVCJVLSHB-UHFFFAOYSA-M 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
【課題】本発明は、ナノサイズの金属構造体の製造方法に関する。
【解決手段】本発明は、金属塩を前駆体とするポリオール還元反応において、イオン性液体を用いることにより、ワイヤ状、キュービック状、八面体状など種々の形態の金属ナノ構造体を均一に製造する方法を提供する。
【選択図】図１The present invention relates to a method for producing a nano-sized metal structure.
In the polyol reduction reaction using a metal salt as a precursor, the present invention uniformly produces various forms of metal nanostructures such as wires, cubics, and octahedra by using an ionic liquid. Provide a way to do it.
[Selection] Figure 1
Description
本発明は、ナノサイズの金属ナノ構造体の製造方法に関し、特に、金属塩を前駆体とするポリオール還元反応にイオン性液体を用いることにより、キュービック状又は八面体状の粒子形態、ナノワイヤ形態などの種々の形態の金属ナノ構造体を均一に製造する方法に関する。 The present invention relates to a method for producing a nano-sized metal nanostructure, and in particular, by using an ionic liquid for a polyol reduction reaction using a metal salt as a precursor, a cubic or octahedral particle form, a nanowire form, etc. The present invention relates to a method for uniformly producing metal nanostructures of various forms.
近年、平板ディスプレイ、タッチパネル、太陽光電池などの種々の分野に適用するために金属ナノ粒子の合成に関する研究が多く進められている。これらの金属ナノ粒子は、透明電極又は導電性インクなどの種々の分野に適用でき、これらの金属ナノ粒子の量産化技術の発明が必要である。この際、金属ナノ粒子の形態は、電気伝導度などの特性を左右する重要な要素であるため、金属ナノ粒子の形態を自由に制御できる技術の発明が必要である。 In recent years, much research on the synthesis of metal nanoparticles has been advanced for application to various fields such as flat panel displays, touch panels, and solar cells. These metal nanoparticles can be applied to various fields such as a transparent electrode or a conductive ink, and an invention of a technique for mass production of these metal nanoparticles is required. At this time, since the form of the metal nanoparticles is an important factor that influences characteristics such as electric conductivity, an invention of a technique capable of freely controlling the form of the metal nanoparticles is required.
それで、金属塩前駆体をエチレングリコールなどのポリオール還元剤を使用して金属ナノ構造体を製造する際にして、ポリビニルピロリドンなどの化合物を共に用いてワイヤ状の金属構造体を製造する技術が報告されている（Ｃｈｅｍ． Ｍａｔｅｒ． １４、４７３６−４７４５）。上記の技術は、いわゆるポリオール還元方法と言われるが、この方法は、溶液相の金属ナノ構造体を比較的容易に製造できるという利点がある。しかしながら、上述した方法により製造された金属ナノ構造体は主にワイヤ状を有するものの、ワイヤ状のみでなく他のナノ粒子の形状を有する構造体が混在されている場合が多く、反応条件に応じてナノ構造体の形態を再現性よく製造し難いという欠点がある。 Therefore, when manufacturing metal nanostructures using a polyol reducing agent such as ethylene glycol as a metal salt precursor, a technology for manufacturing wire-like metal structures using a compound such as polyvinylpyrrolidone is reported. (Chem. Mater. 14, 4736-4745). The above technique is called a so-called polyol reduction method, and this method has an advantage that a solution-phase metal nanostructure can be produced relatively easily. However, although the metal nanostructure manufactured by the above-described method mainly has a wire shape, there are many cases where a structure having not only a wire shape but also other nanoparticle shapes is mixed, depending on the reaction conditions. Therefore, it is difficult to produce nanostructures with good reproducibility.
そのため、金属ナノ構造体の製造において、最終の生成物がワイヤ状（ｗｉｒｅ ｓｈａｐｅ）、キュービック状（ｃｕｂｉｃ ｓｈａｐｅ）、又は八面体状（ｏｃｔａｈｅｄｒａｌ）など金属ナノ構造体の形状を均一で、且つ自由に制御できる技術の発明が必要である。 Therefore, in the manufacture of metal nanostructures, the final product is uniform and freely shaped in the shape of metal nanostructures such as wire shape, cubic shape, or octahedral shape. There is a need for an invention that can be controlled.
本発明の目的は、イオン性液体を用いて種々の形状の金属ナノ構造体を自由に選択して均一に製造できるようにする方法を提供することにある。即ち、本発明を用いることにより、金属塩を前駆体とするポリオール還元反応において、ワイヤ状、キュービック状、八面体状など種々の形状の金属ナノ構造体を均一で、且つ自由に製造することができる。 An object of the present invention is to provide a method that allows metal nanostructures of various shapes to be freely selected and uniformly manufactured using an ionic liquid. That is, by using the present invention, in a polyol reduction reaction using a metal salt as a precursor, metal nanostructures of various shapes such as a wire shape, a cubic shape, and an octahedral shape can be uniformly and freely produced. it can.
前記のような本発明の目的を達成するために、本発明は、イオン性液体、金属塩および還元溶媒を混合反応させることにより、種々の形状の金属ナノ構造体を製造する方法を提供する。 In order to achieve the object of the present invention as described above, the present invention provides a method for producing metal nanostructures of various shapes by mixing and reacting an ionic liquid, a metal salt and a reducing solvent.
なお、本発明は、イオン性液体、金属塩および還元溶媒を混合反応させることにより、上記イオン性液体を構成する陽イオンおよび陰イオンの化学的結合構造により金属ナノ構造体の形状が決定されることを特徴とする。 In the present invention, the shape of the metal nanostructure is determined by the chemical bonding structure of the cation and the anion constituting the ionic liquid by mixing and reacting the ionic liquid, the metal salt, and the reducing solvent. It is characterized by that.
なお、本発明は、イオン性液体、金属塩および還元溶媒を混合反応させることにより、金属ナノ構造体の製造方法において、イオン性液体により金属ナノ構造体が一次元、二次元又は三次元形状を含む様々な構造を持つようにすることを特徴とする。 The present invention provides a method for producing a metal nanostructure by mixing and reacting an ionic liquid, a metal salt, and a reducing solvent so that the metal nanostructure has a one-dimensional, two-dimensional or three-dimensional shape by the ionic liquid. It is characterized by having various structures including.
本発明では、金属塩を前駆体のポリオール還元反応のときにイオン性液体を用い、この際、イオン性液体の陰イオン成分を異にして金属ナノ粒子の形状を変化させる方法を用いた。 In the present invention, an ionic liquid is used during the polyol reduction reaction of a metal salt as a precursor, and at this time, a method of changing the shape of the metal nanoparticles by using different anion components of the ionic liquid is used.
本発明は、イオン性液体、金属塩および還元溶媒を混合反応させることにより、ポリオール還元反応により金属粒子を製造する際に、イオン性液体の陰イオンの種類を異にしてそれぞれ異なる形状の金属ナノ粒子を製造することを特徴とする。 In the present invention, when metal particles are produced by a polyol reduction reaction by mixing and reacting an ionic liquid, a metal salt, and a reducing solvent, different types of anions of the ionic liquid are used to form metal nanoparticles having different shapes. It is characterized by producing particles.
上記金属塩は、ＡｇＮＯ３、Ａｇ（ＣＨ３ＣＯＯ）２、ＡｇＣｌＯ４、Ａｕ（ＣｌＯ４）３、ＰｄＣｌ２、ＮａＰｄＣｌ４、ＰｔＣｌ２、ＳｎＣｌ４、ＨＡｕＣｌ４、ＦｅＣｌ２、ＦｅＣｌ３、Ｆｅ（ＣＨ３ＣＯＯ）２、ＣｏＣｌ２、Ｋ４Ｆｅ（ＣＮ）６、Ｋ４Ｃｏ（ＣＮ）６、Ｋ４Ｍｎ（ＣＮ）６、Ｋ２ＣＯ３等通常の金属陽イオンおよび有機又は無機陰イオンからなるものであって、これらに特に限定されるのではない。上記金属塩は、還元反応により銀、金、パラジウム、錫、鉄、コバルトなど該当金属ナノ粒子に変換される。 The metal salts are AgNO 3 , Ag (CH 3 COO) 2 , AgClO 4 , Au (ClO 4 ) 3 , PdCl 2 , NaPdCl 4 , PtCl 2 , SnCl 4 , HAuCl 4 , FeCl 2 , FeCl 3 , Fe (CH 3 COO) 2 , CoCl 2 , K 4 Fe (CN) 6 , K 4 Co (CN) 6 , K 4 Mn (CN) 6 , K 2 CO 3, etc. However, it is not particularly limited to these. The metal salt is converted into the corresponding metal nanoparticles such as silver, gold, palladium, tin, iron, and cobalt by a reduction reaction.
上記還元溶媒は、金属塩を溶解させることができる極性溶媒であって、分子内にヒドロキシ基を少なくとも２個以上有するジオール、ポリオール又はグリコールなどの溶媒を言う。こられの具体的な例としては、エチレングリコール、１，２−プロピレングリコール、１，３−プロピレングリコール、グリセリン、グリセロール、ポリエチレングリコール、ポリプロピレングリコールなどがある。上記ポリオール還元溶媒は、金属塩の還元反応を誘導して金属元素を生成させる役割をする。 The reducing solvent is a polar solvent that can dissolve a metal salt, and refers to a solvent such as diol, polyol, or glycol having at least two hydroxy groups in the molecule. Specific examples of these include ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, glycerin, glycerol, polyethylene glycol, and polypropylene glycol. The polyol reducing solvent serves to induce a metal salt reduction reaction to generate a metal element.
上記イオン性液体は、有機陽イオンおよび有機又は無機陰イオンから構成された化合物であって、下記一般式（１ａ）のイミダゾリウム系イオン性液体および／又は下記一般式（１ｂ）のピリジニウム系イオン性液体であることを特徴とする。 The ionic liquid is a compound composed of an organic cation and an organic or inorganic anion, and is an imidazolium-based ionic liquid of the following general formula (1a) and / or a pyridinium-based ion of the following general formula (1b) It is a characteristic liquid.
上記一般式（１ａ）で表されるイミダゾリウムイオン性液体の陽イオンの例を具体的に挙げると、１，３−ジメチルイミダゾリウム、１，３−ジエチルイミダゾリウム、１−エチル−３−メチルイミダゾリウム、１−ブチル−３−メチルイミダゾリウム、１−ヘキシル−３−メチルイミダゾリウム、１−オクチル−３−メチルイミダゾリウム、１−デシル−３−メチルイミダゾリウム、１−ドデシル−３−メチルイミダゾリウム、１−テトラデシル−３−メチルイミダゾリウムなどがあり、上記一般式（１ｂ）で表されるピリジニウム系イオン性液体の陽イオンの例としては、１−メチルピリジニウム、１−エチルピリジニウム、１−ブチルピリジニウム、１−エチル−３−メチルピリジニウム、１−ブチル−３−メチルピリジニウム、１−ヘキシル−３−メチルピリジニウム、１−ブチル−３，４−ジメチルピリジニウムなどがある。 Specific examples of the cation of the imidazolium ionic liquid represented by the general formula (1a) include 1,3-dimethylimidazolium, 1,3-diethylimidazolium, 1-ethyl-3-methyl. Imidazolium, 1-butyl-3-methylimidazolium, 1-hexyl-3-methylimidazolium, 1-octyl-3-methylimidazolium, 1-decyl-3-methylimidazolium, 1-dodecyl-3-methyl Examples of the cation of the pyridinium-based ionic liquid represented by the general formula (1b) include 1-methylpyridinium, 1-ethylpyridinium, 1-tetradecyl-3-methylimidazolium, and the like. -Butylpyridinium, 1-ethyl-3-methylpyridinium, 1-butyl-3-methylpyridinium, 1- Hexyl-3-methylpyridinium, and the like 1-butyl-3,4-dimethyl pyridinium.
なお、本発明のイオン性液体の陽イオンは、一般式（１ａ）又は一般式（１ｂ）で表される単分子形態のイオン性液体のみでなく、高分子形態のイオン性液体を含むものであり、例えば、ポリ（１−ビニル−３−アルキルイミダゾリウム）、ポリ（１−ビニル−ピリジニウム）、ポリ（１−ビニル−アルキルピリジニウム）、ポリ（１−アリル−３−アルキルイミダゾリウム）、ポリ（１−（メタ）アクリロイルオキシ−３−アルキルイミダゾリウム）などがあり、これらに限定されない。 In addition, the cation of the ionic liquid of the present invention includes not only a single molecular ionic liquid represented by the general formula (1a) or the general formula (1b) but also a high molecular ionic liquid. Yes, for example, poly (1-vinyl-3-alkylimidazolium), poly (1-vinyl-pyridinium), poly (1-vinyl-alkylpyridinium), poly (1-allyl-3-alkylimidazolium), poly (1- (meth) acryloyloxy-3-alkylimidazolium) and the like are not limited thereto.
上記単分子又は高分子形態のイオン性液体は、有機又は無機陰イオンを有し、例えば、Ｂｒ−、Ｃｌ−、Ｉ−、ＢＦ４−、ＰＦ６−、ＣｌＯ４−、ＮＯ３−、ＡｌＣｌ４−、Ａｌ２Ｃｌ７−、ＡｓＦ６−、ＳｂＦ６−、ＣＨ３ＣＯＯ−、ＣＦ３ＣＯＯ−、ＣＨ３ＳＯ３−、Ｃ２Ｈ５ＳＯ３−、ＣＨ３ＳＯ４−、Ｃ２Ｈ５ＳＯ４−、ＣＦ３ＳＯ３−、（ＣＦ３ＳＯ２）２Ｎ−、（ＣＦ３ＳＯ２）３Ｃ−、（ＣＦ３ＣＦ２ＳＯ２）２Ｎ−、Ｃ４Ｆ９ＳＯ３−、Ｃ３Ｆ７ＣＯＯ−、（ＣＦ３ＳＯ２）（ＣＦ３ＣＯ）Ｎ−などがあり、これらに限定されない。 The monomolecular or polymer form of the ionic liquid has an organic or inorganic anion, for example, Br-, Cl-, I-, BF 4 -, PF 6 -, ClO 4 -, NO 3 -, AlCl 4 -, Al 2 Cl 7 - , AsF 6 -, SbF 6 -, CH 3 COO-, CF 3 COO-, CH 3 SO 3 -, C 2 H 5 SO 3 -, CH 3 SO 4 -, C 2 H 5 SO 4 -, CF 3 SO 3 -, (CF 3 SO 2) 2 N -, (CF 3 SO 2) 3 C -, (CF 3 CF 2 SO 2) 2 N-, C 4 F 9 SO 3 - , C 3 F 7 COO—, (CF 3 SO 2 ) (CF 3 CO) N—, and the like, but are not limited thereto.
上記単分子又は高分子形態のイオン性液体は、陽イオンおよび陰イオンの組合せにより様々な物理的および化学的特性を有する構成が可能であるが、望ましくは金属塩および還元溶媒との相溶性が高いものを選択することが有利である。上記イオン性液体は、金属塩がポリオール還元反応によって金属元素に変換されるときに金属イオン又は金属元素と化学的に相互作用することから、金属元素が一次元、二次元、又は三次元的な成長が可能なように助力する役割をし、最終的に均一な形状を有する金属粒子が作製される。 The ionic liquid in the above monomolecular or polymer form can be configured to have various physical and chemical properties by a combination of a cation and an anion, but preferably has compatibility with a metal salt and a reducing solvent. It is advantageous to choose a higher one. The ionic liquid has a one-dimensional, two-dimensional, or three-dimensional metal element because the metal salt chemically interacts with the metal ion or the metal element when the metal salt is converted into the metal element by a polyol reduction reaction. Metal particles having a uniform shape are finally produced by helping to enable growth.
特に、上記イオン性液体の陰イオン成分が最終的に製造された金属ナノ粒子の形状を左右するが、例えば、アルキル硫酸塩（ＲＳＯ４−）やスルホン酸アルキル（ＲＳＯ３−）のような硫黄化合物の陰イオンを有するイオン性液体を用いると、主に一次元的な成長をしてナノワイヤ状の金属構造体が製造され、ハロゲン化物（Ｈａｌｉｄｅ）系陰イオンを有するイオン性液体を用いると、主に三次元的な成長をして塩素陰イオン（Ｃｌ−）の場合はキュービック状、ブロム陰イオン（Ｂｒ−）の場合は八面体状の粒子を有する金属構造体が製造される。イオン性液体の陰イオン成分によりそれぞれ異なる形状の金属ナノ粒子を選択的に製造することができる。最終のナノ構造体の形状は、反応初期段階で金属ナノ粒子とイオン性液体間の相互作用により金属ナノ粒子の成長方向が変わるので、この段階で、特に、イオン性液体の陰イオンが重要な役割をすることになる。即ち、反応初期に先に金属塩が還元溶媒によって先に金属ナノ粒子が形成され、金属ナノ粒子とイオン性液体の陰イオン（Ｃｌ−、Ｂｒ−、ＣＨ３ＳＯ４−）と相互作用しながら、一定方向の成長をするように助力し、種々の形状の金属ナノ構造体を製造できることになる。 In particular, anionic component of the ionic liquid affects the shape of the finally produced metal nanoparticles, for example, alkyl sulfates sulfur such as (RSO 4 - -) and alkyl sulfonates (RSO 3) When an ionic liquid having a compound anion is used, a nanowire-like metal structure is produced mainly by one-dimensional growth, and when an ionic liquid having a halide anion is used, It grows mainly three-dimensionally to produce a metal structure having cubic particles in the case of chlorine anions (Cl-) and octahedral particles in the case of bromo anions (Br-). Depending on the anionic component of the ionic liquid, metal nanoparticles having different shapes can be selectively produced. Since the final nanostructure shape changes the growth direction of the metal nanoparticles due to the interaction between the metal nanoparticles and the ionic liquid at the initial stage of the reaction, the anion of the ionic liquid is particularly important at this stage. Will play a role. That is, the metal salt is first formed by the reducing solvent in the early stage of the reaction, and the metal nanoparticle is interacted with the anion (Cl−, Br−, CH 3 SO 4 −) of the ionic liquid. The metal nanostructures of various shapes can be manufactured by assisting the growth in a certain direction.
本発明の代表的な例として、ナノワイヤ状を有する金属ナノ構造体を製造するための具体的な方法は次の通りである。先ず、上記の金属塩、還元溶媒および硫化物の陰イオンからなるイオン性液体を適正比率で混合した後、常温で一定時間撹はんする。均一に混合した後上記混合物の反応温度を１５０〜２００℃に上げて反応を持続することにより、金属ナノワイヤを製造する。これにより製造された金属ナノワイヤは、ナノ粒子の形状は殆どなく、平均直径が０．０１〜０．１ミクロン、平均長さが５〜１００ミクロンのナノワイヤ状を有する。前記の過程でナノワイヤの形状を有するためには、各成分の混合比率を適宜調節することが必要であるが、これは、還元溶媒に対して金属塩０．０１〜１モル濃度およびイオン性液体（高分子形態のイオン性液体の場合には繰り返し単位を基準として）０．００１〜１モル濃度に維持することが望ましい。上記濃度において、金属塩の濃度が０．０１およびイオン性液体の濃度が０．００１以下であると、濃度が低すぎて生成される金属ワイヤの含有量が非常に低くなり、或いはイオン性液体の含有量が非常に低くなって、金属ナノワイヤの生成が良くなく不利である。その反面、金属塩の濃度が１モル以上であると、金属塩の含有量が高すぎて生成された金属粒子がくっつき合ったり、粒子の大きさが大きくなるという欠点があって不利であり、又はイオン性液体の含有量が１モル以上であると、全体溶液の粘度が高くなりすぎ、金属ナノワイヤの合成が難しくなってむしろ不利である。 As a typical example of the present invention, a specific method for manufacturing a metal nanostructure having a nanowire shape is as follows. First, an ionic liquid composed of the above metal salt, reducing solvent and sulfide anion is mixed in an appropriate ratio, and then stirred at room temperature for a predetermined time. After uniformly mixing, the reaction temperature of the mixture is raised to 150 to 200 ° C. to maintain the reaction, thereby producing metal nanowires. The metal nanowires thus produced have almost no nanoparticle shape, and have a nanowire shape with an average diameter of 0.01 to 0.1 microns and an average length of 5 to 100 microns. In order to have a nanowire shape in the above-described process, it is necessary to appropriately adjust the mixing ratio of each component, which is 0.01 to 1 molar concentration of metal salt and ionic liquid with respect to the reducing solvent. It is desirable to maintain the concentration at 0.001 to 1 molar (based on repeating units in the case of ionic liquids in polymer form). In the above concentration, when the concentration of the metal salt is 0.01 and the concentration of the ionic liquid is 0.001 or less, the content of the metal wire generated due to the concentration being too low, or the ionic liquid As a result, the production of metal nanowires is not good and disadvantageous. On the other hand, if the concentration of the metal salt is 1 mol or more, the metal salt content is too high and the produced metal particles stick together, and the particle size is disadvantageous. Alternatively, if the content of the ionic liquid is 1 mol or more, the viscosity of the whole solution becomes too high, which makes it difficult to synthesize metal nanowires, which is rather disadvantageous.
前述したような方法を用いながら陰イオンが互いに異なるイオン性液体を用いるとキュービック状の金属ナノ粒子又は八面体状の金属ナノ粒子を均一で、且つ安定的に合成することができる。 When ionic liquids having different anions are used while using the method described above, cubic metal nanoparticles or octahedral metal nanoparticles can be synthesized uniformly and stably.
本発明のイオン性液体、金属塩および還元溶媒を混合反応することにより、種々の形状の金属ナノ構造体の製造方法において、金属ナノ構造体の形状および大きさをより一層効果的に制御するために、下記一般式（２ａ）の窒素化合物又は一般式（２ｂ）の硫黄化合物を添加剤として追加することが可能であり、この際、上記化合物の含有量の範囲は金属塩１００重量部を基準として０．１〜１００重量部にすることが望ましい。これらの化合物の濃度が０．１重量部以下であると形状および大きさの制御効果が僅かであり、１００重量部以上であるとナノ構造体の形状が変化してしまう副作用が生じむしろ不利である。 In order to more effectively control the shape and size of a metal nanostructure in a method for producing metal nanostructures of various shapes by mixing and reacting the ionic liquid, metal salt and reducing solvent of the present invention. It is possible to add a nitrogen compound of the following general formula (2a) or a sulfur compound of the general formula (2b) as an additive, and the content range of the above compound is based on 100 parts by weight of a metal salt. Is preferably 0.1 to 100 parts by weight. If the concentration of these compounds is 0.1 parts by weight or less, the effect of controlling the shape and size is slight, and if it is 100 parts by weight or more, there is a side effect of changing the shape of the nanostructure, which is rather disadvantageous. is there.
上記一般式（２ａ）で表される窒素化合物の例としては、塩化テトラブチルアンモニウム、臭化セチルトリメチルアンモニウム、塩化テトラブチルホスホニウムなどを含み、上記一般式（２ｂ）で表される硫黄化合物の例としては、ドデシル硫酸ナトリウム、ドデシルベンゼンスルホン酸、ポリスチレンスルホン酸、ポリ（４−スチレンスルホン酸ナトリウム）等がある。 Examples of the nitrogen compound represented by the general formula (2a) include tetrabutylammonium chloride, cetyltrimethylammonium bromide, tetrabutylphosphonium chloride, and the like, and examples of the sulfur compound represented by the general formula (2b). As sodium dodecyl sulfate, dodecyl benzene sulfonic acid, polystyrene sulfonic acid, poly (sodium 4-styrene sulfonate), and the like.
本発明は、イオン性液体、金属塩および還元溶媒を混合反応させることにより、種々の形状の金属ナノ構造体を製造することができる。 In the present invention, metal nanostructures of various shapes can be produced by mixing and reacting an ionic liquid, a metal salt, and a reducing solvent.
なお、金属塩を前駆体とするポリオール還元反応において、陰イオンの種類が異なるイオン性液体を選択的に用いることにより、種々の形状の金属ナノ粒子を選択的に再現性よく製造できて効果的である。 In addition, in the polyol reduction reaction using a metal salt as a precursor, by selectively using ionic liquids having different types of anions, metal nanoparticles of various shapes can be selectively produced with good reproducibility and effective. It is.
以下、本発明を次の実施例により具体的に説明するが、本発明はこれらの実施例により限定されるものではない。 Hereinafter, the present invention will be specifically described with reference to the following examples, but the present invention is not limited to these examples.
（実施例１）
丸底フラスコにＡｇＮＯ３をエチレングリコールに０．１モル濃度で溶かした溶液５０ミリリットルと、１−ブチル−３−メチルイミダゾリウムメチルサルフェイトをエチレングリコールに０．１５モル濃度で溶かした溶液５０ミリリットルとを混合した。上記混合溶液は、１６０℃で６０分間撹はんしながら反応させた後、温度を再度常温に冷却させた。上記溶液を１ミクロンの気孔を有したフィルタでろ過した後、走査電子顕微鏡で観察した結果、図１に示すように、直径が約２２０ナノメートル、長さが約７ミクロンのナノワイヤが形成されたことを確認した。
Example 1
50 ml of a solution obtained by dissolving AgNO 3 in ethylene glycol at a 0.1 molar concentration in a round bottom flask and 50 ml of a solution obtained by dissolving 1-butyl-3-methylimidazolium methyl sulfate in ethylene glycol at a 0.15 molar concentration. And mixed. The mixed solution was reacted at 160 ° C. with stirring for 60 minutes, and then the temperature was again cooled to room temperature. The solution was filtered through a filter having 1 micron pores and then observed with a scanning electron microscope. As a result, as shown in FIG. 1, nanowires having a diameter of about 220 nanometers and a length of about 7 microns were formed. It was confirmed.
（実施例２）
丸底フラスコにＡｇＮＯ３を１，３−プロピレングリコールに０．２モル濃度で溶かした溶液１０ミリリットルと、１−エチル−３−メチルイミダゾリウムメチルサルフェイトを１，３−プロピレングリコールに０．３モル濃度で溶かした溶液１０ミリリットルとを混合した。上記混合溶液は、１００℃の温度で約３０分間撹はんして反応させた後、温度を常温に冷却させた。上記溶液を１ミクロンの気孔を有したフィルタでろ過した後、走査電子顕微鏡で観察した結果、直径が約１８０ナノメートル、長さが約１０ミクロンのナノワイヤが形成されたことを確認した。
(Example 2)
In a round bottom flask, 10 ml of a solution prepared by dissolving AgNO 3 in 1,3-propylene glycol at a 0.2 molar concentration, and 1-ethyl-3-methylimidazolium methyl sulfate in 1,3-propylene glycol were mixed in 0.3. 10 ml of the solution dissolved in molarity was mixed. The mixed solution was stirred and reacted at a temperature of 100 ° C. for about 30 minutes, and then the temperature was cooled to room temperature. The solution was filtered through a filter having 1 micron pores and then observed with a scanning electron microscope. As a result, it was confirmed that nanowires having a diameter of about 180 nanometers and a length of about 10 microns were formed.
（実施例３）
丸底フラスコにＡｇＮＯ３を１，２−プロピレングリコールに０．２モル濃度で溶かした溶液１０ミリリットルと、１−エチル−３−メチルイミダゾリウムメチルサルフェイトを１，３−プロピレングリコールに０．３モル濃度で溶かした溶液１０ミリリットルとを混合した後、添加したＡｇＮＯ３の重量に対して１％重量のドデシル硫酸ナトリウムを添加した。上記混合溶液は、１００℃の温度で約３０分間撹はんして反応させた後、温度を常温に冷却させた。上記溶液を１ミクロンの気孔を有したフィルタでろ過した後、走査電子顕微鏡で観察した結果、直径が約８０ナノメートル、長さが約１０ミクロンのナノワイヤが形成されたことを確認した。
(Example 3)
10 mL of a solution obtained by dissolving AgNO 3 in 1,2-propylene glycol at a 0.2 molar concentration in a round bottom flask, and 1-ethyl-3-methylimidazolium methyl sulfate in 1,3-propylene glycol in 0.3 After mixing with 10 ml of the solution dissolved at a molar concentration, 1% by weight of sodium dodecyl sulfate was added with respect to the weight of AgNO 3 added. The mixed solution was stirred and reacted at a temperature of 100 ° C. for about 30 minutes, and then the temperature was cooled to room temperature. The solution was filtered through a filter having 1 micron pores and then observed with a scanning electron microscope. As a result, it was confirmed that nanowires having a diameter of about 80 nanometers and a length of about 10 microns were formed.
（実施例４）
イオン性液体として１−エチル−３−メチルピリジニウムメチルサルフェイトを使用したことを除いては、実施例１と同一の方法で金属ナノ構造体を製造した。上記溶液を１ミクロンの気孔を有したフィルタでろ過した後、走査電子顕微鏡で観察した結果、直径が約３２０ナノメートル、長さが約５ミクロンのナノワイヤが形成されたことを確認した。
Example 4
A metal nanostructure was produced in the same manner as in Example 1 except that 1-ethyl-3-methylpyridinium methylsulfate was used as the ionic liquid. The solution was filtered through a filter having 1 micron pores and then observed with a scanning electron microscope. As a result, it was confirmed that nanowires having a diameter of about 320 nanometers and a length of about 5 microns were formed.
（実施例５）
イオン性液体として１−ブチル−３−メチルイミダゾリウムクロライドを使用したことを除いては、実施例１と同一の方法で金属ナノ構造体を製造した。最終的に生成された反応溶媒を０．２ミクロン大きさのテフロンフィルタでろ過した後、走査電子顕微鏡で観察した結果、図２に示すように、約４００ナノメートルのキュービック状を有する銀ナノ粒子が形成されたことを確認した。
(Example 5)
A metal nanostructure was produced in the same manner as in Example 1 except that 1-butyl-3-methylimidazolium chloride was used as the ionic liquid. After the reaction solvent finally produced was filtered with a 0.2 micron size Teflon filter and observed with a scanning electron microscope, as shown in FIG. 2, silver nanoparticles having a cubic shape of about 400 nanometers. It was confirmed that was formed.
（実施例６）
イオン性液体として１−ブチル−３−メチルイミダゾリウムブロマイドを使用したことを除いては、実施例１と同一の方法で金属構造体を製造した。最終的に生成された反応溶媒を１ミクロンのフィルタでろ過した後、走査電子顕微鏡で観察した結果、図３に示すように、約５ミクロンの八面体状を有する銀粒子が形成されたことを確認した。
(Example 6)
A metal structure was produced in the same manner as in Example 1 except that 1-butyl-3-methylimidazolium bromide was used as the ionic liquid. The reaction solvent finally produced was filtered with a 1 micron filter and then observed with a scanning electron microscope. As a result, as shown in FIG. 3, silver particles having an octahedral shape of about 5 microns were formed. confirmed.
本発明により製造された金属ナノ構造体は、平板ディスプレイ、タッチパネル、太陽光電池などの種々の産業分野において使用が可能である。 The metal nanostructure produced by the present invention can be used in various industrial fields such as a flat panel display, a touch panel, and a solar battery.
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| TW201100558A (en) | 2011-01-01 |
| CN102369154A (en) | 2012-03-07 |
| WO2010117204A3 (en) | 2011-01-20 |
| CN102369154B (en) | 2015-02-18 |
| WO2010117204A2 (en) | 2010-10-14 |
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| JP6041138B2 (en) | 2016-12-07 |
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