WO2010058941A2 - 이온성 액체를 이용한 금속 나노와이어의 제조방법 - Google Patents
이온성 액체를 이용한 금속 나노와이어의 제조방법 Download PDFInfo
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- WO2010058941A2 WO2010058941A2 PCT/KR2009/006767 KR2009006767W WO2010058941A2 WO 2010058941 A2 WO2010058941 A2 WO 2010058941A2 KR 2009006767 W KR2009006767 W KR 2009006767W WO 2010058941 A2 WO2010058941 A2 WO 2010058941A2
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- WIPO (PCT)
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- ionic liquid
- metal
- coo
- producing
- methylimidazolium
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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
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- 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
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- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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]
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- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
- B22F2301/255—Silver or gold
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Definitions
- the present invention relates to a method for producing a nano-sized metal wire, more specifically to uniformly preparing metal nanowires having a diameter-to-length ratio of at least 50 by using an ionic liquid in a polyol reduction reaction using a metal salt as a precursor. It is about a method.
- Vacuum electrode metal oxides such as indium tin oxide (ITO) are widely used as the most widely used transparent electrode materials, but these metal oxides have to be post-processed at a high temperature to exhibit high electrical conductivity. It is difficult to apply to a plastic substrate having a relatively low heat resistance because it requires. In addition, even if the metal oxide film is formed on the plastic substrate through the low temperature deposition process, there is a problem that cracks easily occur in the metal oxide film due to warpage or other physical deformation, and it may be replaced due to the high production cost of the vacuum deposition method. Much research is being conducted on transparent electrode materials that can be used.
- ITO indium tin oxide
- a method of forming a transparent conductive film having high electrical conductivity and optical transparency may be proposed by preparing a metal including silver and dispersing it in a solution and applying it to a plastic film.
- the physical properties of the metal nanostructures are required to be easily prepared on a solution-based way to produce a large amount of metal nanostructures, and in order to form an effective conductive network, the metal nanostructures have a diameter-to-length wire shape. desirable.
- a metal salt precursor in the presence of polyvinylpyrrolidone, polyols including ethylene glycol as reducing agents have been reported to produce metal nanowires. (Chem. Mater. 14, 4736-4745).
- the technique has an advantage that the metal nanostructure can be relatively easily prepared on a solution basis through a reaction that can be referred to as a "polyol reduction method.”
- the metal nanostructures manufactured by this method have the shape of nanowires, structures having the shape of nanoparticles as well as nanowires are often mixed, and it is difficult to form nanostructures reproducibly according to reaction conditions. There are disadvantages.
- the problem to be achieved by the present invention is not limited to the above-mentioned problem, another task that is not mentioned will be clearly understood by those skilled in the art from the following description.
- the present invention is characterized in that the metal element produced by the polyol reduction reaction by mixing and reacting the metal salt and the reducing solvent in the presence of the ionic liquid is produced in the form of nanowires through interaction with the ionic liquid.
- the metal salt is composed of a metal cation and an organic or inorganic anion, and includes AgNO 3 , Ag (CH 3 COO) 2 , AgClO 4 , Au (ClO 4 ) 3 , PdCl 2 , PtCl 2, and the like.
- the metal salt is converted into metal elements such as silver, gold, palladium and platinum through a reduction reaction.
- the reducing solvent is a polar solvent capable of dissolving a metal salt, and refers to a solvent such as diol, polyol or glycol having at least two hydroxyl groups in a molecule. Specific examples thereof include ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, glycerin, glycerol, and the like.
- the polyol reducing solvent serves to induce a reduction reaction of the metal salt to generate metal elements.
- the ionic liquid is a compound composed of an organic cation including an imidazolium group and an organic or inorganic anion, characterized in that the monomer form represented by the following formula (1) or the polymer form represented by the following formula (2).
- R 1 , R 2 and R 3 are the same or different and each represent hydrogen or a hydrocarbon group having 1 to 16 carbon atoms, and may contain a hetero atom.
- X ⁇ represents an anion of an ionic liquid.
- ionic liquid cation in the form of monomer represented by Formula 1 include 1,3-dimethylimidazolium, 1,3-diethylimidazolium, 1-ethyl-3-methylimidazolium, 1-butyl 3-methylimidazolium, 1-hexyl-3-methylimidazolium, 1-octyl-3-methylimidazolium, 1-decyl-3-methylimidazolium, 1-dodecyl-3-methyl Midazolium, 1-tetradecyl-3-methylimidazolium, and the like
- specific examples of the ionic liquid cation in the polymer form represented by Chemical Formula 2 include poly (1-vinyl-3-alkylimidazolium), poly (1-allyl-3-alkylimidazolium), poly (1- (meth) acryloyloxy-3-alkylimidazolium), and the like.
- the ionic liquid anion of the formula (I) or (II) is as far as it satisfies the ionic liquid is not particularly restricted but, 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 -, 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 - , etc. Can be mentioned.
- the ionic liquid may be composed of an ionic liquid having various physical and chemical properties according to a combination of cations and anions.
- the ionic liquid has a high compatibility with metal salts and reducing solvents. It is advantageous to manufacture.
- the ionic liquid is used to help the metal element to grow one-dimensional growth by chemically interacting with the metal ion or metal element when the metal salt is converted to the metal element by the polyol reduction reaction, the final uniform shape Allow metal nanowires to be prepared.
- Specific manufacturing method of the metal nanowire of the present invention is as follows. First, the metal salt, the reducing solvent, and the ionic liquid are mixed at an appropriate ratio and stirred at room temperature for a predetermined time. When uniform mixing is achieved, the metal nanowires are manufactured by continuing the reaction by raising the reaction temperature of the mixture to 150-200 degrees Celsius.
- the metal nanostructures thus prepared have almost no nanoparticle shape, and have a nanowire shape having an average diameter of 0.01 to 0.1 micron and an average length of 5 to 100 microns.
- the metal nanowire of the present invention in addition to the metal salt, the reducing solvent and the ionic liquid, it is also possible to prepare by mixing an ionic additive such as quaternary ammonium salt.
- the dispersing agent may be further added as a method for preventing the nanowires from being bundled together in a bundle form and reducing the diameter of the nanowires.
- the types of dispersants are not limited, Triton X-100, Triton X-200, BASF's P123, F127, F68, L64 and methyl-beta-cyclocoldtrin, methylcellulose, ethylcellulose, poly Vinylpyrrolidone, cetyltrimethylammonium bromite (CTAB), sodium dodecyl sulfate (SDS), polystyrenesulfonate (PSSA), poly (sodium-4-styrenesulfonate) (PSSNa), dodecylbenzenesulfonate (DBSA ) May be added in a weight ratio of 0.1 to 100% based on the weight of the metal salt.
- metal nanowires having a diameter-to-length ratio of at least 50 can be produced uniformly and reproducibly, thereby forming an effective conducting network with a small content. It is suitable for use as a material for transparent electrodes.
- the metal nanowires prepared according to the present invention can be used as transparent electrode materials in the fields of flat panel displays, touch panels, solar cells and the like.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
Claims (9)
- 금속 나노와이어를 제조하는 방법에 있어서,이온성 액체의 존재하에서 금속염 및 환원용매를 혼합, 반응시킴으로써 폴리올 환원반응을 통해 생성되는 금속원소가 이온성 액체와의 상호작용을 통해 나노와이어 형상으로 제조되는 것,을 특징으로 하는 금속 나노와이어를 제조하는 방법.
- 제 2항에 있어서,상기 단량체 형태의 이온성 액체 양이온으로는 1,3-다이메틸이미다졸륨, 1,3-다이에틸이미다졸륨, 1-에틸-3-메틸이미다졸륨, 1-부틸-3-메틸이미다졸륨, 1-헥실-3-메틸이미다졸륨, 1-옥틸-3-메틸이미다졸륨, 1-데실-3-메틸이미다졸륨, 1-도데실-3-메틸이미다졸륨,1-테트라데실-3-메틸이미다졸륨을 포함하거나, 또는상기 단량체 형태의 상기 이온성 액체의 음이온으로는 Br-, Cl-, I-, BF4 -, PF6 -, ClO4 -, NO3 -, AlCl4 -, Al2Cl7 -, AsF6 -, SbF6 -, CH3COO-, CF3COO-, CH3SO3 -, CF3SO3 -, (CF3SO2)2N-, (CF3SO2)3C-, (CF3CF2SO2)2N-, C4F9SO3 -, C3F7COO-, (CF3SO2)(CF3CO)N-을 포함하거나. 또는상기 단량체가 상기 양이온과 상기 음이온 모두를 포함하는 것,을 특징으로 하는 금속 나노와이어의 제조방법.
- 제 2항 또는 제 3항에 있어서,상기 고분자 형태의 이온성 액체의 양이온으로는 폴리(1-비닐-3-알킬이미다졸륨), 폴리(1-알릴-3-알킬이미다졸륨), 폴리(1-(메트)아크릴로일록시-3-알킬이미다졸륨)을 포함하거나,상기 이온성 액체의 음이온으로는 Br-, Cl-, I-, BF4 -, PF6 -, ClO4 -, NO3 -, AlCl4 -, Al2Cl7 -, AsF6 -, SbF6 -, CH3COO-, CF3COO-, CH3SO3 -, CF3SO3 -, (CF3SO2)2N-, (CF3SO2)3C-, (CF3CF2SO2)2N-, C4F9SO3 -, C3F7COO-, (CF3SO2)(CF3CO)N-을 포함하거나, 또는상기 고분자 형태의 이온성 액체가 상기 양이온과 상기 음이온 모두를 포함하는 것,을 특징으로 하는 금속 나노와이어의 제조방법.
- 제 1항 내지 제 4항 중 어느 한 항에 있어서, 상기 금속 나노와이어가 직경 대 길이비가 최소 50 이상 것을 특징으로 하는 금속 나노와이어의 제조 방법.
- 제 1항 내지 제 5항 중 어느 한 항에 있어서, 상기 금속염은 금속 양이온 및 유기 또는 무기 음이온으로 이루어진 것으로서, AgNO3, Ag(CH3COO)2, AgClO4, Au(ClO4)3, PdCl2, PtCl2 을 포함하는 것을 특징으로 하는 금속 나노와이어의 제조 방법.
- 제 1항 내지 제 6항 중 어느 한 항에 있어서, 환원용매는 분자내에 히드록시기를 적어도 2개 이상 가지는 다이올, 폴리올 또는 글리콜등의 용매로서 에틸렌 글리콜, 1,2-프로필렌글리콜, 1,3-프로필렌글리콜, 글리세린, 글리세롤을 포함하는 것임을 특징으로 하는 금속 나노와이어의 제조 방법.
- 제 1항 내지 제 7항 중 어느 한 항에 있어서, Triton X-100, Triton X-200, 바스프사의 P123, F127, F68, L64 및 메틸-베타-시클로덱스트린 (methyl-β-cyclodextrin), 메틸셀룰로오즈, 에틸셀룰로오즈, 폴리비닐피롤리돈, 세틸트리메틸암모늄브로마이트 (CTAB), 소디움도데실설페이트 (SDS), 폴리스티렌설포네이트 (PSSA), 폴리(소디움-4-스티렌설포네이트) (PSSNa), 도데실벤젠설포네이트 (DBSA)을 포함하는 분산제를 추가로 포함하는 것을 특징으로 하는 금속 나노와이어의 제조 방법.
- 제 1항 내지 제 8항 중 어느 한 항에 있어서, 금속염, 이온성 액체 및 환원용매의 혼합비율은 환원용매에 대해 금속염 0.01 내지 1 몰농도 및 이온성 액체 (고분자 형태의 이온성 액체인 경우에는 반복단위 기준으로) 0.01 내지 1 몰농도임을 특징으로 하는 금속 나노와이어의 제조방법.
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US13/130,045 US9233421B2 (en) | 2008-11-18 | 2009-11-17 | Method for manufacturing metallic nanowires using ionic liquids |
EP09827706.4A EP2360116A4 (en) | 2008-11-18 | 2009-11-17 | PROCESS FOR THE PRODUCTION OF METAL NANOWIRES USING IONIC LIQUIDS |
JP2011536260A JP5611220B2 (ja) | 2008-11-18 | 2009-11-17 | イオン性液体を用いた金属ナノワイヤの製造方法 |
CN200980145473.8A CN102245499B (zh) | 2008-11-18 | 2009-11-17 | 利用离子液体制造金属纳米线的方法 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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KR10-2008-0114906 | 2008-11-18 | ||
KR1020080114906A KR101089299B1 (ko) | 2008-11-18 | 2008-11-18 | 이온성 액체를 이용한 금속 나노와이어의 제조방법 |
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WO2010058941A2 true WO2010058941A2 (ko) | 2010-05-27 |
WO2010058941A3 WO2010058941A3 (ko) | 2010-08-19 |
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PCT/KR2009/006767 WO2010058941A2 (ko) | 2008-11-18 | 2009-11-17 | 이온성 액체를 이용한 금속 나노와이어의 제조방법 |
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US (1) | US9233421B2 (ko) |
EP (1) | EP2360116A4 (ko) |
JP (1) | JP5611220B2 (ko) |
KR (1) | KR101089299B1 (ko) |
CN (1) | CN102245499B (ko) |
TW (1) | TWI464274B (ko) |
WO (1) | WO2010058941A2 (ko) |
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JP2014523047A (ja) * | 2011-07-12 | 2014-09-08 | エルジー イノテック カンパニー リミテッド | タッチパネル及び電極製造方法 |
US20150321257A1 (en) * | 2012-12-14 | 2015-11-12 | Soloe Tech Co., Ltd. | Method for manufacturing silver nanowires using ionic liquid |
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CN106807935B (zh) * | 2015-12-01 | 2019-11-12 | 中国科学院大连化学物理研究所 | 一种被有机配体保护的金纳米颗粒的活化方法 |
WO2017159537A1 (ja) * | 2016-03-14 | 2017-09-21 | ユニチカ株式会社 | ナノワイヤーおよびその製造方法、ナノワイヤー分散液ならびに透明導電膜 |
WO2017217628A1 (ko) * | 2016-06-14 | 2017-12-21 | 충남대학교산학협력단 | 금속 나노입자-고분자 복합체 박막의 제조방법 |
KR101884299B1 (ko) * | 2016-07-04 | 2018-08-23 | 서울대학교산학협력단 | 용액공정을 통한 금 나노 와이어의 제조방법 및 이에 의해 제조된 금 나노 와이어 |
KR101934183B1 (ko) | 2017-02-28 | 2018-12-31 | 국민대학교산학협력단 | 고압수열합성법을 이용하여 은 나노와이어를 제조하는 방법 및 이를 이용한 투명 전도성 전극 필름 |
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JP2014505963A (ja) * | 2010-12-07 | 2014-03-06 | ロディア オペレーションズ | 導電性ナノ構造、そのようなナノ構造を作製するための方法、そのようなナノ構造を含有する導電性ポリマーフィルム、およびそのようなフィルムを含有する電子デバイス |
JP2014523047A (ja) * | 2011-07-12 | 2014-09-08 | エルジー イノテック カンパニー リミテッド | タッチパネル及び電極製造方法 |
US20150321257A1 (en) * | 2012-12-14 | 2015-11-12 | Soloe Tech Co., Ltd. | Method for manufacturing silver nanowires using ionic liquid |
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WO2010058941A3 (ko) | 2010-08-19 |
US20110219913A1 (en) | 2011-09-15 |
KR101089299B1 (ko) | 2011-12-02 |
CN102245499B (zh) | 2015-02-18 |
KR20100055983A (ko) | 2010-05-27 |
TW201028483A (en) | 2010-08-01 |
CN102245499A (zh) | 2011-11-16 |
EP2360116A4 (en) | 2014-02-19 |
EP2360116A2 (en) | 2011-08-24 |
JP2012509396A (ja) | 2012-04-19 |
JP5611220B2 (ja) | 2014-10-22 |
US9233421B2 (en) | 2016-01-12 |
TWI464274B (zh) | 2014-12-11 |
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