WO2007148460A1 - PROCÉDÉ DE PRODUCTION DE NANOPARTICULES DE DIAMÈTRE PARTICULAIRE ÉGAL OU INFÉRIEUR À 200 nm - Google Patents

PROCÉDÉ DE PRODUCTION DE NANOPARTICULES DE DIAMÈTRE PARTICULAIRE ÉGAL OU INFÉRIEUR À 200 nm Download PDF

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Publication number
WO2007148460A1
WO2007148460A1 PCT/JP2007/056470 JP2007056470W WO2007148460A1 WO 2007148460 A1 WO2007148460 A1 WO 2007148460A1 JP 2007056470 W JP2007056470 W JP 2007056470W WO 2007148460 A1 WO2007148460 A1 WO 2007148460A1
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Prior art keywords
nanoparticles
raw material
metal
particle size
less
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PCT/JP2007/056470
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English (en)
Japanese (ja)
Inventor
Masato Watanabe
Hiroshi Sugai
Hitoshi Takamura
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3R Corporation
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Publication of WO2007148460A1 publication Critical patent/WO2007148460A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122—Incoherent waves
    • B01J19/123—Ultraviolet light
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0004—Preparation of sols
    • B01J13/0043—Preparation of sols containing elemental metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/121—Coherent waves, e.g. laser beams
    • 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
    • B22F1/0545—Dispersions or suspensions of nanosized particles
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0879—Solid
    • 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

Definitions

  • the present invention relates to a method for producing nanoparticles having a particle size of 200 or less.
  • the method in this case is a method (polyol process) in which a solution containing a reducing agent such as polyhydric alcohol and a metal raw material such as an organic metal or metal salt is heated and refluxed to synthesize nanoparticles (polyol process).
  • a solution containing a reducing agent such as polyhydric alcohol and a metal raw material such as an organic metal or metal salt is heated and refluxed to synthesize nanoparticles.
  • This is a method based on decomposition by Such a wet method can produce high-quality nanoparticles that cannot be obtained by the dry method described above, but it involves complicated processes such as a purification step by centrifugation after synthesis and many technical know-hows. Mass production is difficult because it is required.
  • Some companies have gasified an inorganic raw material and synthesized nanoparticles by irradiating the gas with an infrared laser beam such as a carbon dioxide laser, and started supplying it to the plant.
  • an infrared laser beam such as a carbon dioxide laser
  • a gas that absorbs infrared light such as ethylene
  • This absorbing gas absorbs the energy of the laser beam and converts it into thermal energy. It is called “Laser Pyrolysis” because it is based on the principle that nanoparticles are synthesized by thermal decomposition!
  • liquid complexes such as metal carbo- hydrate are often used as raw materials, and it is difficult to remove carbon from the complex or absorbed gas, resulting in metal carbide nanoparticles.
  • metal carbo- hydrate are often used as raw materials, and it is difficult to remove carbon from the complex or absorbed gas, resulting in metal carbide nanoparticles.
  • This production method is a production method in which, for example, a metal zinc target is placed in a solvent containing a dispersant (surfactant) and laser ablation is performed in a liquid.
  • This manufacturing method is based on the fact that nanoparticles are formed by the so-called ablation phenomenon, in which a target metal material is irradiated with laser light and emitted as a single atom, ion, or cluster in a solution.
  • the principle is basically the same as that of abrasion (for example, see Patent Documents 2 and 3).
  • Non-Patent Document 1 Xiang Xin Bi et al., “Journal of Materials” Research No. 8-7 (J. Mater. Res., Vol. 8, no.7) “, (USA) (1993) p.166 6.
  • Patent Document 1 Japanese Patent No. 3268793
  • Patent Document 2 JP 2004-283924 A
  • Patent Document 3 Japanese Patent Laid-Open No. 2005-264089
  • Non-Patent Document 1 and Patent Document 1 have a problem that the recovery efficiency of the produced nanoparticles is not good.
  • a special “laser single light absorption gas” that plays a role of absorbing laser light and converting it into heat is required.
  • a multi-component alloy or multi-component nanoparticle of any composition can be prepared. There was a problem that manufacturing was difficult.
  • the present invention has been made paying attention to such a problem, and is excellent in recovery efficiency, and easily manufactures high-quality organic nanoparticle colloid solutions and multicomponent alloys or multicomponent compounds of any composition.
  • An object of the present invention is to provide a method for producing nanoparticles having a particle diameter of 200 ° or less.
  • liquid-phase metal raw materials such as metal salt or metal complex solution are irradiated with high-intensity light typified by laser light.
  • high-quality inorganic nanoparticles with a narrow particle size distribution can be obtained very easily.
  • the method for producing nanoparticles having a particle size of 200 or less according to the present invention is characterized by irradiating the raw material liquid with high energy light having a wavelength of less than 400 nm.
  • nanoparticles of a multi-component compound or a high-quality inorganic nano-particle colloid solution or a multi-component alloy of any composition it is possible to easily produce nanoparticles of a multi-component compound or a high-quality inorganic nano-particle colloid solution or a multi-component alloy of any composition.
  • the inorganic nanoparticle colloid solution having excellent recovery efficiency and the multicomponent alloy of any composition or the multicomponent compound nanoparticles can be easily produced, and the particle size is 200 nm or less.
  • a method for producing nanoparticles can be provided.
  • nanoparticles having a particle size of 200 nm or less can be produced.
  • the raw material solution may be a solution in which the raw material of the nanoparticles to be produced is dissolved or a liquid phase raw material.
  • the raw material may be organic or inorganic. For example, it can be selected from carbon compounds, silicon compounds, metal salts, metal compounds, metal complexes, and the like. However, if the raw material is a metal, it is preferable that it also has a metal salt strength. Yes. This is because, in general, the production efficiency of nanoparticles obtained as a result of obtaining a solution having a higher concentration than that of a metal complex is often higher with metal salts.
  • the solvent may be a polar solvent such as water or alcohol, or a nonpolar solvent such as an ether as long as the raw material can be dissolved.
  • a polar solvent such as water or alcohol
  • a nonpolar solvent such as an ether
  • the liquid phase raw materials they can be used as irradiated raw materials without being dissolved.
  • the liquid phase raw material for example, a complex or compound itself in a liquid phase, such as iron pentacarbon, nickel pentacarbon, and silicon tetrachloride, can be used.
  • a higher concentration of the raw material solution is preferable because it increases the efficiency of the produced nanoparticles.
  • the high-energy light with a wavelength of less than 400 nm to be irradiated may be any wavelength as long as the wavelength is less than 400 nm, but a laser beam with a wavelength of 193 nm to 300 nm is particularly preferable.
  • a laser beam having a wavelength is preferred.
  • “high energy light” means energy light of lmj or more, energy light of lOOmJ to lOOOmJ is preferable, and energy light of 500 mJ is particularly preferable.
  • the irradiation time is not limited, but when the raw material solution is an ethanol solution having a metal component concentration of a metal salt, metal compound or metal complex of 1 weight percent, it is usually preferably 1 minute to 60 minutes.
  • the yield of this method is extremely high.
  • a laser beam of 500 mJ having a wavelength of 248 nm is irradiated to an ethanol solution of a metal salt, a metal compound or a metal complex with a concentration power ⁇ weight percent
  • Nanoparticles of 200 ° or less can be produced in a yield such that 80 to 99 weight percent of the metal component in the raw material liquid is the metal content of the produced nanoparticles.
  • Nanoparticles having a particle size of 2 OOnm or less can be produced by irradiating the raw material solution with high-energy energy having a wavelength of less than 400nm.
  • nanoparticles having an average particle size of lOOnm to 200nm can be preferably produced.
  • nanoparticles having a particle size of 10 nm or less, preferably 0.5 nm or more and 5 nm or less can be produced.
  • nanoparticles having an average particle size force of 2 nm or more and 3 ions or less can be produced.
  • the particle size of the produced nanoparticles can be adjusted within a range of particle size of 200 nm or less.
  • This method is particularly suitable for the production of inorganic nanoparticles or inorganic / organic composite nanoparticles having a particle size of 200 or less.
  • This method can also produce alloy nanoparticles, silicon nanoparticles, silicon dioxide nanoparticles, polymer nanoparticles, and diamond nanoparticles.
  • laser light is preferable. Even when laser light is not used, nanoparticles can be produced, but the production efficiency is significantly reduced.
  • a far-infrared carbon dioxide laser in the laser pyrolysis method can also be used. However, the most desirable is ultraviolet excimer laser light with a short wavelength and high photon energy. The average particle size of the nanoparticles obtained at this time is small, and at the same time, the particle size distribution is narrow and good quality.
  • a metal salt, a metal compound, a metal complex, or the like when used as a raw material, a metal ion or complex in a liquid phase is directly decomposed and reduced by high-intensity light energy, so that the nanoparticles can be reduced. It is based on the principle of generation and is also different from “liquid phase laser ablation”, in which a solid metal target material is irradiated with laser light.
  • nanoparticles can be generated only by irradiating the raw material with high-energy light (high-intensity light) having a wavelength of less than 400 nm typified by laser light.
  • high-energy light high-intensity light
  • nano-particle dispersant By adding a nano-particle dispersant, nano-particles with a small particle size can be obtained by suppressing the grain growth, and also after the synthesis, it has high stability.
  • the dispersant is added to the raw material liquid as described above, the inorganic nanoparticle composite surface is obtained because the organic dispersant covers the surface of the inorganic nanoparticle.
  • Various commercially available surfactants can be used as the dispersing agent at this time.
  • a polar solvent such as water and a solvent such as ethanol
  • a water-soluble polymer such as PVP, or taenic acid
  • carboxylic acids such as oleic acid, amines such as oleylamine, and thiols such as dodecanethiol can be typically used.
  • an oxidizing agent it is possible to easily synthesize oxide nanoparticles.
  • the raw material is an easily oxidizable element other than a noble metal, it is allowed to stand for a certain period of time after synthesis without adding an oxidizer, thereby generating natural acid nanoparticles. can do. Therefore, this method is suitable for the production of iron oxide nanoparticles!
  • the raw material liquid may be a mixture of raw material liquids of a plurality of different elements.
  • the raw material liquid that is, the liquid phase
  • a multi-component alloy or a multi-component compound having an arbitrary composition may be generated. Easy.
  • the raw material liquid may flow.
  • a liquid raw material liquid is used, nanoparticles can be produced by irradiating a fluid raw material. This makes it possible to efficiently and flexibly design plant process lines for mass production, such as raw material supply, mixing, reaction, and recovery processes. In order to increase the yield, it is preferable to stir the raw material solution to be irradiated.
  • the high-energy light applied to the raw material liquid can be transmitted through the raw material liquid as it is, or it can be reflected and transmitted repeatedly.
  • this method of irradiating a raw material solution with high-energy energy having a wavelength of less than 400 nm is a technique for producing various inorganic and carbon-based nanoparticles extremely easily in a short time.
  • the applicable industrial fields are wide-ranging and attract attention in medical diagnostic fields such as POC.
  • Applicable to precious metal nanoparticles such as gold and silver modified with antibodies, hard magnetic nanoparticles that can be used as ultra-high-density magnetic recording medium materials, and nanoparticles that are used in various catalytic fields. It is. In particular, these applications are preferable because particles as small as 2 to 3 nm can be obtained.
  • it can be applied to single-electron devices or devices using the surface plasmon phenomenon in the visible region of noble metals.
  • Tables 1 and 2 show the preparation tables for the precursor solutions used to synthesize Pt and Fe nanoparticles.
  • Table 1 shows the precursor solution for producing Pt nanoparticles
  • Table 2 shows the precursor solution for producing Fe nanoparticles.
  • Dispersant-Solvent C2H5OH 39.5 g 50mL Weight% 0.12 (Fe) wt%
  • Dispersant Oleic Acia 5 mM 0.25 mmol 70.6 mg 79.3 Solvent C2H5OH 39.5 g 50 mL Weight% 0.12 (Fe) wt%
  • the raw material liquid was irradiated with high-energy light having a wavelength of less than 400 nm to produce nanoparticles having a particle size of 200 nm or less.
  • the raw material solution is a solution of salt ⁇ platinum (IV) acid hexahydrate (H Pt (IV) Cl • 6H ⁇ ) in ethanol (CH OH) Used as. Also minutes
  • the raw material solution is a complex of iron (III) acetylylacetonate (FeOllXC H 0;)) dissolved in ethanol (CH OH). Used as
  • KrF excimer laser light was used as the high-tech energy to irradiate.
  • the irradiation conditions are summarized in Table 3.
  • FIG. 1 is a graph showing the particle size distribution of Pt and Fe nanoparticles by a dynamic light scattering (DLS) method of an example of the present invention.
  • DLS dynamic light scattering

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electromagnetism (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Optics & Photonics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

L'invention concerne un procédé de production de nanoparticules dont le diamètre particulaire est égal ou inférieur à 200 nm, avec un excellent rendement de récupération et qui permet de produire facilement une solution colloïdale de bonne qualité de nanoparticules inorganiques et de nanoparticules d'alliage ou de composé multinaire ayant une quelconque composition désirée. Une matière brute liquide est soumise à des rayonnements avec une lumière d'énergie élevée dont la longueur d'onde est inférieure à 400 nm pour produire des nanoparticules dont le diamètre particulaire est égal ou inférieur à 200 nm. Lorsque les nanoparticules à produire sont en platine, la matière brute liquide est celle que l'on obtient en dissolvant l'acide hexachloroplatine (IV) hexahydraté (H2Pt(IV)Cl6·6H2O) dans l' éthanol (C2H5OH).
PCT/JP2007/056470 2006-06-21 2007-03-27 PROCÉDÉ DE PRODUCTION DE NANOPARTICULES DE DIAMÈTRE PARTICULAIRE ÉGAL OU INFÉRIEUR À 200 nm WO2007148460A1 (fr)

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JP2006-170804 2006-06-21
JP2006170804A JP2008000654A (ja) 2006-06-21 2006-06-21 粒径２００ｎｍ以下のナノ粒子の製造方法

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102974836A (zh) * 2012-11-28 2013-03-20 天津大学 激光制备银/碳复合纳米环结构的方法
WO2016185728A1 (fr) * 2015-05-20 2016-11-24 国立大学法人山形大学 Procédé de fabrication d'une dispersion de nanoparticules d'argent et procédé de fabrication d'encre à nanoparticules d'argent

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI499466B (zh) * 2007-03-22 2015-09-11 Hitachi Chemical Co Ltd 金屬微粒子與其製造方法以及金屬微粒子分散液與其製造方法
CN103008680A (zh) * 2012-12-07 2013-04-03 天津大学 激光化学法合成银-碳复合纳米线的方法
CN103341635B (zh) * 2013-06-21 2016-06-22 中国计量学院 一种通过激光生成水合电子来制备纳米金颗粒的方法
CN105834434B (zh) * 2016-04-27 2017-12-05 广东工业大学 一种粒径分布可控的铜微纳颗粒的化学激光复合制备方法
WO2019078100A1 (fr) * 2017-10-16 2019-04-25 国立大学法人山形大学 Procédé de production d'un composite comprenant un métal revêtu de microparticules solides

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0679168A (ja) * 1992-09-07 1994-03-22 Hitoshi Kasai 有機超微粒子の製法
JP2005314712A (ja) * 2004-04-27 2005-11-10 Osaka Gas Co Ltd 金属微粒子生成用組成物および金属微粒子

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0679168A (ja) * 1992-09-07 1994-03-22 Hitoshi Kasai 有機超微粒子の製法
JP2005314712A (ja) * 2004-04-27 2005-11-10 Osaka Gas Co Ltd 金属微粒子生成用組成物および金属微粒子

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102974836A (zh) * 2012-11-28 2013-03-20 天津大学 激光制备银/碳复合纳米环结构的方法
WO2016185728A1 (fr) * 2015-05-20 2016-11-24 国立大学法人山形大学 Procédé de fabrication d'une dispersion de nanoparticules d'argent et procédé de fabrication d'encre à nanoparticules d'argent
JPWO2016185728A1 (ja) * 2015-05-20 2018-04-26 国立大学法人山形大学 銀ナノ粒子分散体の製造方法及び銀ナノ粒子インクの製造方法
US10821506B2 (en) 2015-05-20 2020-11-03 National University Corporation Yamagata University Method for producing silver nanoparticle dispersion and method for producing silver nanoparticle ink

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