WO2015111095A1 - 銀ナノ粒子の製造方法 - Google Patents
銀ナノ粒子の製造方法 Download PDFInfo
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- WO2015111095A1 WO2015111095A1 PCT/JP2014/000316 JP2014000316W WO2015111095A1 WO 2015111095 A1 WO2015111095 A1 WO 2015111095A1 JP 2014000316 W JP2014000316 W JP 2014000316W WO 2015111095 A1 WO2015111095 A1 WO 2015111095A1
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- silver
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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
- B22F1/0545—Dispersions or suspensions of nanosized particles
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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
- B22F1/0551—Flake form nanoparticles
-
- 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
- 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
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Definitions
- the present invention relates to a method for producing silver nanoparticles, and more particularly to a method for producing plate-like silver nanoparticles.
- LSPR Localized Surface Plasmon Resonance
- the silver nanoparticles having the above-mentioned light absorption characteristics are expected to be used as optical materials.
- the wavelength region where LSPR is expressed depends on the size of the crystal particles. There is a need for a method for producing particles with high productivity and high reproducibility.
- Patent Document 1 discloses a first step of preparing an aqueous solution containing a silver salt, a polycarboxylate salt, a dispersant, and hydrogen peroxide, and adding a predetermined amount of a reducing agent to the adjusted aqueous solution. And a second step of forming plate-shaped silver nanoparticles of a predetermined size.
- the silver concentration of the starting solution cannot be made higher than 0.1 mM by the method described in Patent Document 1 described above (hereinafter referred to as the conventional method). Furthermore, when the present inventor reexamined the conventional method, in the conventional method, the reproducibility of the size and distribution of the plate-like silver nanoparticles is extremely bad, and the scale-up is very difficult, and the productivity is low. It turns out that there is a limit to improvement.
- This invention is made
- the present inventor made a hypothesis on the mechanism by which plate-like silver nanoparticles are formed by the scheme of the conventional method (details will be described later). Then, in light of the hypothesis, the problem of the conventional method was revealed and an attempt was made to improve it. As a result, the inventors succeeded in simultaneously achieving improvement in productivity (high concentration of the final product and acquisition of good scale-up property) and high reproducibility, leading to the present invention.
- a first step of preparing a silver ion aqueous solution containing a crystal habit controlling agent as a starting solution, and a reducing agent is added while stirring the starting solution to obtain an aqueous dispersion of silver crystals.
- a method for producing silver nanoparticles comprising a second step and a third step of adding an oxidizing agent while stirring the aqueous dispersion.
- the schematic diagram showing the manufacturing process of silver nanoparticle The conceptual diagram for demonstrating the mechanism in which a plate-shaped silver nanoparticle grows selectively.
- FIG. 1 is a schematic diagram showing a method for producing silver nanoparticles according to an embodiment of the present invention. As shown in FIG. 1, the manufacturing method of this embodiment is roughly divided into three steps. In the following, description will be given in order.
- a silver ion aqueous solution containing a crystal habit controlling agent is prepared as a starting solution.
- a silver ion aqueous solution containing a crystal habit controlling agent is prepared by adding silver salt and a crystal habit controlling agent to water (preferably pure water, more preferably ultrapure water) while stirring well. .
- the silver salt in the present embodiment may be a water-soluble compound, and a suitable example of the silver salt used in the present embodiment is silver nitrate (AgNO 3 ).
- the productivity of the plate-like silver nanoparticles primarily depends on the silver concentration of the starting solution.
- the silver concentration of the starting solution can be set to 0.2 mM or higher, and can be set to a high concentration of 0.5 mM or higher according to the target productivity.
- the crystal habit controlling agent in the present embodiment may be any compound that exhibits selective adsorptivity to the (111) plane of the silver crystal
- suitable examples of the crystal habit controlling agent used in the present embodiment include: , Low molecular organic acids or salts thereof.
- the low molecular organic acid a polycarboxylic acid having two or more carboxylic acid groups can be exemplified, and as a suitable example thereof, citric acid can be exemplified.
- the silver salt and the crystal habit controlling agent described above it is preferable to add the silver salt and the crystal habit controlling agent described above to water in the form of an aqueous solution adjusted to an appropriate concentration.
- the reducing agent is added to the starting solution prepared by the above-mentioned procedure while stirring well.
- the added reducing agent reduces the silver ions in the starting solution and forms very fine silver crystals.
- the reducing agent in the present embodiment may be a compound that can reduce silver ions to metallic silver, and an appropriate reducing agent that matches the redox potential (+0.799) of silver can be used.
- Preferable examples of the reducing agent used in the present embodiment include borohydride metal salts, and more preferable examples include sodium tetrahydroborate (NaBH 4 ).
- the reducing agent is preferably added to the aqueous silver ion solution containing the crystal habit controlling agent in the form of an aqueous solution adjusted to an appropriate concentration at ice temperature.
- an oxidizing agent is added to the aqueous dispersion containing fine silver crystals obtained by the above-described procedure while stirring well.
- the oxidizing agent in the present embodiment may be a compound that can oxidize and re-ionize metallic silver, and an appropriate oxidizing agent corresponding to the redox potential (+0.799) of silver can be used.
- an appropriate oxidizing agent corresponding to the redox potential (+0.799) of silver can be used.
- hydrogen peroxide (H 2 O 2 ) can be mentioned.
- the oxidizing agent is preferably added to an aqueous dispersion containing fine silver crystals in the form of an aqueous solution adjusted to an appropriate concentration.
- the oxidant is added intermittently in several batches while the aqueous dispersion containing fine silver crystals is well stirred, or the oxidant is continuously added while controlling the addition flow rate. It is desirable to optimize the solubility of metallic silver in the aqueous dispersion at an appropriate time, for example by adding it.
- a silver colloid dispersion liquid containing plate-shaped silver nanoparticles as a main component at a high concentration can be obtained.
- parameters such as the concentration of silver ions and crystal habit controlling agent in the first step, the amount of reducing agent added in the second step, the stirring efficiency, the reaction temperature, etc. are appropriately set. By this, the size of the plate-like silver nanoparticles in the final product can be controlled. The reason for this will be described later. Moreover, in this embodiment, it is desirable to maintain the carboxylic acid group of the crystal habit controlling agent described above in a dissociated state, and it is desirable that the pH of the reaction system be 4 or more throughout all the steps described above.
- plate-shaped silver nanoparticles can be produced with high productivity and high reproducibility. Further, in this embodiment, since a crystal habit controlling agent (for example, citric acid) having a function as a dispersant is used, it is not necessary to add another compound in the use of the dispersant, and as a result, the final production It is possible to minimize the contamination of unnecessary organic substances in the product (aqueous dispersion containing plate-like silver nanoparticles).
- a crystal habit controlling agent for example, citric acid
- FIG. 2 is a conceptual diagram for explaining a hypothesis established by the present inventor regarding a mechanism for selectively obtaining plate-like silver nanoparticles. Below, the formation mechanism of a plate-shaped silver nanoparticle is demonstrated along each process, referring FIG. 1 and FIG. 2 simultaneously.
- polyvinyl pyrrolidone PVP
- a crystal habit controlling agent having a function as a dispersant is used. Do not add polymer components such as PVP to the solution.
- the silver ions in the aqueous solution are reduced as shown in FIG.
- Very fine metallic silver crystals of the order of several nanometers are formed.
- microcrystals that can collide and coalesce with each other during water dispersion almost simultaneously with the formation of fine metallic silver crystals, and later become plate-like silver nanoparticles. (Parallel double twin 10) is formed with a certain probability.
- a reducing agent a silver ion aqueous solution containing a crystal habit controlling agent
- a fine silver parallel double twin 10 is composed of two twin planes (plane defects) parallel to the (111) plane of the silver crystal and parallel to each other.
- the main plane is the (111) plane, and the crystal structure of silver is face-centered cubic. Therefore, the (100) plane is necessarily exposed on a part of the side surface crystallographically.
- the crystal habit controlling agent 12 is immediately adsorbed on the (111) plane and inhibits crystal growth in the direction perpendicular to the (111) plane, that is, the main plane.
- the amount of adsorption of the crystal habit controlling agent 12 on the (100) plane existing on the side surface is smaller than that on the (111) plane, so that the effect of inhibiting the crystal growth is weaker.
- a silver crystal having 10 as a nucleus grows anisotropically almost only in the lateral direction.
- the solubility of metallic silver in the aqueous dispersion increases, and a part of the fine silver crystals dissolves (reionizes).
- Ostwald ripening proceeds, the larger crystals become larger, and the smaller crystals become smaller.
- the parallel double twin 10 formed in the second step is not affected by the crystal habit controlling agent 12 on the (100) side of the side surface.
- the growth rate has an advantage over other fine silver crystals that are mixed, and in the initial stage of the third step, the size increases faster than other silver crystals.
- FIG. 2 (c) a plate-like crystal derived from a larger parallel double twin 10 is selectively grown.
- FIG. 2 (d) the plate-like silver nanoparticles 20 with the major axis of the main plane increasing in size survive as the main component.
- the formation mechanism of the plate-like silver nanoparticles in the present invention has been described above.
- the number ratio of the parallel double twins 10 to the total microcrystals at the end of the second step is the final product. This is the primary factor that determines the size of the plate-like silver nanoparticles 20. That is, as the number ratio of the parallel double twins 10 increases, the size of the plate-like silver nanoparticles 20 in the final product decreases, and as the number ratio of the parallel double twins 10 decreases, the plate in the final product decreases. The size of the silver nanoparticles 20 becomes larger.
- the number ratio of the parallel double twins 10 to the total microcrystals at the time when the second step is completed is the concentration of silver ions and crystal habit controlling agent in the first step, silver ions and crystals in the first step. It varies within a range from several% to several tens% depending on conditions such as the molar ratio of the soot control agent, the amount of the reducing agent added in the second step, the reaction temperature, and the stirring efficiency. In other words, if the reverse is true, by appropriately controlling these conditions, the number ratio of the parallel double twins 10 can be controlled, and as a result, plate-like silver nanoparticles of the targeted size can be obtained. Can do.
- PVP polyvinyl pyrrolidone
- the problems in the conventional method have been described.
- the present inventors have reconstituted the plate-like silver nanoparticles at an unprecedented high concentration and with high reproducibility.
- the present inventors have succeeded in manufacturing, and at the same time, have found that the reconstructed manufacturing method has ease of scale-up, and have reached the present invention.
- the manufacturing method of the plate-shaped silver nanoparticle of this invention was demonstrated, as the use, the sensitization in optical spectroscopy, such as a reagent (especially diagnostic agent (biosensor), surface enhancement Raman spectroscopy), etc. Agents), paints, antistatic films, conductive films, antireflection films, antibacterial films, catalyst carrier films, and the like.
- a thin film containing plate-like silver nanoparticles has a function of trapping light
- photoelectric conversion is achieved by forming a thin film containing plate-like silver nanoparticles on the light-receiving surface of a photoelectric conversion element such as a solar cell. The rate can be improved.
- plate-like silver nanoparticles tuned according to the light absorption band of the dye are encapsulated in a thin film
- organic thin-film solar cells Can encapsulate plate-like silver nanoparticles whose LSPR is tuned according to the light absorption band of the p-type semiconductor in a thin film, thereby improving the photoelectric conversion rate due to the electric field enhancement effect.
- the present invention has been described so far with the embodiment of the method for producing silver nanoparticles, the scope of the present invention is not limited to silver, for example, copper, gold, platinum, palladium, rhodium, etc.
- the same method as described above to the noble metal, plate-shaped metal nanoparticles can be produced.
- Silver nanoparticles were prepared by the following procedure.
- all the used reagents are those of a special grade manufactured by Wako Pure Chemical Industries.
- the absorbance at the peak of 750 nm measured with a cell length of 2 mm for sample 4 is “1.35”, which is “6.75” when converted to a cell length of 1 cm.
- This value corresponds to about 7 times the absorbance of the colloidal dispersion mainly composed of plate-like silver nanoparticles produced by the conventional method, and the colloidal dispersion mainly composed of plate-like silver nanoparticles. Has never been reported to have been obtained at such high concentrations.
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- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
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Abstract
Description
第1の工程では、出発溶液として、晶癖制御剤を含む銀イオン水溶液を調整する。具体的には、水(好ましくは純水、より好ましくは超純水)をよく攪拌しながら、これに銀塩と晶癖制御剤を加えることよって晶癖制御剤を含む銀イオン水溶液を調整する。
続く第2の工程では、上述した手順で調整した出発溶液をよく攪拌しながら、これに還元剤を添加する。添加された還元剤により、出発溶液中の銀イオンが還元され、非常に微小な銀の結晶が形成される。本実施形態における還元剤は、銀イオンを金属銀に還元することができる化合物であればよく、銀の酸化還元電位(+0.799)に見合った適切な還元剤を用いることができる。本実施形態で用いる還元剤の好適な例としては、水素化ホウ素金属塩を挙げることでき、さらにその好適な例としては、テトラヒドロホウ酸ナトリウム(NaBH4)を挙げることができる。なお、還元剤は、氷温で適切な濃度に調整した水溶液の形で晶癖制御剤を含む銀イオン水溶液に添加することが好ましい。
続く第3の工程では、上述した手順で得られた微小な銀結晶を含む水分散液をよく攪拌しながら、これに酸化剤を添加する。本実施形態における酸化剤は、金属銀を酸化して再イオン化することができる化合物であればよく、銀の酸化還元電位(+0.799)に見合った適切な酸化剤を用いることができる。本実施形態で用いる酸化剤の好適な例としては、過酸化水素(H2O2)を挙げることができる。なお、酸化剤は、適切な濃度に調整した水溶液の形で微小な銀結晶を含む水分散液に添加することが好ましい。
以下の手順で銀ナノ粒子を作製した。なお、使用した全ての試薬は、和光純薬工業社製の特級グレードのものである。
分光光度計(V-570UV/Vis/NIR,日本分光社製)を用いて、上述した手順で作製したサンプル1~4の吸収スペクトルを測定した。なお、測定において、セル長を2mmとし、超純水をリファレンスとして、サンプルを希釈せずに測定を行った。図3は、サンプル1~4の吸収スペクトル測定結果をまとめて示す。
12…晶癖制御剤
20…銀ナノ粒子
Claims (10)
- 出発溶液として晶癖制御剤を含む銀イオン水溶液を調整する第1の工程と、
前記出発溶液を攪拌しながら還元剤を添加して銀結晶の水分散液を得る第2の工程と、
前記水分散液を攪拌しながら酸化剤を添加する第3の工程と、
を含む銀ナノ粒子の製造方法。 - 前記第3の工程において前記水分散液中における金属銀の溶解度が適時最適化されるように前記酸化剤を添加する、
請求項1に記載の製造方法。 - 前記晶癖制御剤は、低分子有機酸またはその塩を含む、請求項1または2に記載の製造方法。
- 前記低分子有機酸は、2以上のカルボン酸基を有するポリカルボン酸である、請求項3に記載の製造方法。
- 前記ポリカルボン酸は、クエン酸である、請求項4に記載の製造方法。
- 前記還元剤は、テトラヒドロホウ酸ナトリウムである、請求項1~5のいずれか一項に記載の製造方法。
- 前記酸化剤は、過酸化水素である、請求項1~6のいずれか一項に記載の製造方法。
- 前記第3の工程において、前記水分散液中にプレート状の銀ナノ粒子を選択的に残存させる、請求項1~7のいずれか一項に記載の製造方法。
- 請求項1~8のいずれか一項に記載された製造方法を用いて製造された銀ナノ粒子。
- 請求項9に記載された銀ナノ粒子のコロイド分散液。
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US15/111,998 US20170021426A1 (en) | 2014-01-23 | 2014-01-23 | Method for manufacturing silver nanoparticles |
JP2014526309A JP5970638B2 (ja) | 2014-01-23 | 2014-01-23 | 銀ナノ粒子の製造方法 |
PCT/JP2014/000316 WO2015111095A1 (ja) | 2014-01-23 | 2014-01-23 | 銀ナノ粒子の製造方法 |
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WO2019065316A1 (ja) | 2017-09-29 | 2019-04-04 | 日本ペイントホールディングス株式会社 | 塗料組成物及び塗膜 |
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JP2017156104A (ja) * | 2016-02-29 | 2017-09-07 | 西松建設株式会社 | 光増強素子とその製造方法ならびに分光分析用キットおよび分光分析方法 |
CN112091233B (zh) * | 2020-11-19 | 2021-02-19 | 西安宏星电子浆料科技股份有限公司 | 一种银纳米粒子的合成方法 |
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JP2009269935A (ja) * | 2008-04-30 | 2009-11-19 | Sumitomo Metal Mining Co Ltd | 金色系金属光沢を有する銀膜 |
JP2012036481A (ja) * | 2010-08-11 | 2012-02-23 | Mitsui Mining & Smelting Co Ltd | 扁平銀粒子及びその製造方法 |
WO2013146447A1 (ja) * | 2012-03-27 | 2013-10-03 | 富士フイルム株式会社 | 銀粒子含有膜およびその製造方法、ならびに、熱線遮蔽材 |
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US8574338B2 (en) * | 2010-11-17 | 2013-11-05 | E I Du Pont De Nemours And Company | Reactor and continuous process for producing silver powders |
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- 2014-01-23 US US15/111,998 patent/US20170021426A1/en not_active Abandoned
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JP2009269935A (ja) * | 2008-04-30 | 2009-11-19 | Sumitomo Metal Mining Co Ltd | 金色系金属光沢を有する銀膜 |
JP2012036481A (ja) * | 2010-08-11 | 2012-02-23 | Mitsui Mining & Smelting Co Ltd | 扁平銀粒子及びその製造方法 |
WO2013146447A1 (ja) * | 2012-03-27 | 2013-10-03 | 富士フイルム株式会社 | 銀粒子含有膜およびその製造方法、ならびに、熱線遮蔽材 |
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WO2019065316A1 (ja) | 2017-09-29 | 2019-04-04 | 日本ペイントホールディングス株式会社 | 塗料組成物及び塗膜 |
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