US20070056402A1 - Metal nanoparticles and method for manufacturing thereof - Google Patents
Metal nanoparticles and method for manufacturing thereof Download PDFInfo
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- US20070056402A1 US20070056402A1 US11/520,731 US52073106A US2007056402A1 US 20070056402 A1 US20070056402 A1 US 20070056402A1 US 52073106 A US52073106 A US 52073106A US 2007056402 A1 US2007056402 A1 US 2007056402A1
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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
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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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
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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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
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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 of producing metal nanoparticles, in particular, to a method of producing metal nanoparticles with the solution method.
- the chemical synthesis method includes the vapor-phase method and the solution (colloid) method, where the vapor-phase method which uses plasma or gas evaporation has shortcomings in that it requires highly expensive equipments, so the solution method which is possible to generate uniform particles with low cost is generally used.
- a method of producing metal nanoparticles by the solution method up to now comprises dissociating metal compound and then producing metal nanoparticles in the form of hydrosol using a reducing agent or a surfactant.
- the production of metal nanoparticles by this existing solution method provides a very low yield rate, as it is limited by the concentration of the metal compound solution. That is, it is possible to form metal nanoparticles of uniform size only when the concentration of the metal compound is less than mM.
- the un-reactant remaining after completion of the reaction reduces the yield rate, and a vast amount of loss which occurs during the separation step of formed metal nanoparticles results in further reduction of the yield rate.
- the dispersion stability is important, but the existing method provides a very low dispersion rate of 0.1 weight %.
- the present invention provides a method of producing metal nanoparticles, having a high yield rate and uniform size achieved by employing a heterologous reducing agent that considerably reduces un-reactant, and using ethylene glycol that allows effective separation of desired metal- nanoparticles.
- the present invention provides metal nanoparticles having high dispersion stability achieved by capping with polyvinyl pyrrolidone(PVP) and conductive ink including these metal nanoparticles.
- One aspect of the invention may provide a method of producing nanoparticles comprising, (a) mixing ethylene glycol, capping molecules and a reducing agent, (b) reacting a mixture of a metal precursor and an alcohol-based compound with the mixture of (a), and (c) adding acetone and ethylene glycol to the reaction solution of (b).
- the ethylene glycol in the step (a) may be mixed in 100 to 200 parts by weight with respect to 10 parts by weight of the metal precursor.
- the mixed solution of the metal precursor and the alcohol-based compound may react with the mixture of (a) by adding together within a short period of time, and a step of recovering metal nanoparticles by centrifuging the reaction solution after the step (c) may further be included.
- the capping molecule may be preferably polyvinyl pyrrolidone and according to a preferred embodiment, the polyvinyl pyrrolidone may be mixed in 30-70 parts by weight with respect to 10 parts by weight of the metal precursor.
- the reducing agent may include one or more compounds selected from the group consisting of glucose, ascorbic acid, tannic acid, dimethylformamide, tetrabuthylammonium borohydride, NaBH 4 , LiBH 4 and N 2 H 4 .
- the reducing agent is preferably glucose and mixed in a mole ratio of 0.2 to 0.5 with respect to the metal precursor.
- the metal precursor may include one or more metals selected from the group consisting of gold, silver, copper, nickel, zinc, platinum, palladium, rhodium, ruthenium, iridium, osmium, tungsten, tantalum, titanium, aluminum, cobalt, iron and a mixture thereof.
- the metal precursor is one or more compounds selected from the group consisting of AgNO 3 , AgBF 4 , AgPF 6 , Ag 2 O, CH 3 COOAg, AgCF 3 SO 3 , AgClO 4 , AgCl, and CH 3 COCH ⁇ COCH 3 Ag.
- the alcohol-based compound may be one or more compounds selected from the group consisting of methanol, ethanol, ethylene glycol and diethylene glycol.
- the alcohol-based compound may be mixed in 30-50 parts by weight with respect to 10 parts by weight of the metal precursor.
- the ethylene glycol in the step (c) may be added in 2-10 parts by weight with respect to 1 part by weight of the capping molecule, and preferably, a reaction time in the step (b) ranges from 30 minutes to 4 hours.
- Another aspect of the invention may provide metal nanoparticles produced by the method for producing metal nanoparticles set forth above.
- the metal nanoparticles may be metal nanoparticles capped with the polyvinyl pyrrolidone, and according to a preferred embodiment, the particles of polyvinyl pyrrolidone are 5-10 weight %.
- Another aspect of the invention may provide conductive ink including metal nanoparticles set forth above.
- FIG. 1 is data representing the result of TGA analysis for the metal nanoparticles produced according to an embodiment of the invention
- FIGS. 2 and 3 are FE-SEM images of the metal nanoparticles produced according to preferred embodiments of the invention.
- FIG. 4 is a graph that represents the result of UW-VIS spectroscopy(UV spectrum) of the metal nanoparticles produced according to a preferred embodiment of the invention.
- FIG. 5 is a graph that represents the result of particle size analysis of the metal nanoparticles produced according to a preferred embodiment of the invention.
- the invention include a step of mixing ethylene glycol, capping molecules, and a reducing agent.
- ethylene glycol along with the reducing agent reduces the metal precursor to prevent formation of un-reactants and allow production of metal nanoparticles in a high yield rate.
- Ethylene glycol may be also used as a solvent that dissolves the metal precursor.
- ethylene glycol is added with excess amount of acetone so that removes un-reacted PVP and terminates the reaction. So far, though ethylene glycol has been used to act as both a solvent and a reducing agent, it performs poor in the reducing capacity, to result in a low yield rate. But in the invention, ethylene glycol plays various roles mentioned above and is used as an important compound for producing metal nanoparticles at a high concentration and a high yield rate.
- the capping molecules refer to molecules that allow metal particles to grow stably in a solvent and form nano-sized particles by encapsulating the metal particles. Any known compounds may be used as such capping molecules, and compounds having oxygen, nitrogen, and sulfur atoms may be typically used. More specifically, compounds having thiol group(—SH), amine group(—NH2), carboxyl group(—COOH) may be used as capping molecules, and according to an embodiment of the invention, PVP(Polyvinyl pyrrolidone) is preferable. This is because the PVP strongly adheres to metal nanoparticles to enhance the dispersion stability of metal nanoparticles thus obtained, and allows the metal nanoparticles to have a high dispersion rate when they are re-dispersed.
- PVP Polyvinyl pyrrolidone
- a reducing agent may be added to increase the yield rate of metal nanoparticles in the invention.
- this reducing agent may include borate hydroxides such as NaBH 4 , LiBH 4 , and tetrabutylammonium borohydride(TBAB), hydrazines such as N 2 H 4 , glucose, acids such as ascorbic acid, tannic acid etc., and dimethylformamide(DMF) etc.
- glucose is used since it is low in price, environment-friendly, and easily dissolved in water or an alcohol-based compound.
- Glucose is used as a reducing agent because when a hydroxyl group of glucose is oxidized, it may release electrons during its conversion to the corresponding aldehyde.
- ethylene glycol is added to dissolve PVP while functioning as a reducing agent, where ethylene glycol is preferably added in 100-200 parts by weight with respect to 10 parts by weight of the metal precursor since this is the most optimal amount for reducing the metal precursor with the reducing agent.
- ethylene glycol is preferably added in 100-200 parts by weight with respect to 10 parts by weight of the metal precursor since this is the most optimal amount for reducing the metal precursor with the reducing agent.
- the addition of more than 200 parts by weight of ethylene glycol does not result in a increased yield of nanoparticles, the addition of more ethylene glycol than the desired amount is not economical.
- the capping molecules be added in 30-70 parts by weight with respect to 10 parts by weight of the metal nanoparticles. If the capping molecule is added less than 30 parts by weight, metal nanoparticles thus formed become larger than nano size and lack of uniformity and further deteriorates the dispersion stability since it is impossible to obtain fully capped metal nanoparticles. On the other hand, if the capping molecules is added more than 70 parts by weight, the yield rate does not increase as much as of that extent, which just results in an increase of unit cost.
- PVP is used as a capping molecule, it is preferable that the PVP be mixed in 30-50 parts by weight with respect to 10 parts by weight of the metal precursor.
- the reducing agent is added in a mole ratio of 0.2-0.5 with respect to 1 mole of the metal precursor. Because the addition within this ratio allows the formation of uniform metal nanoparticles and reduces un-reactant to increase the yield rate. When the reducing agent is added more than 0.5 mole ratio, it results in precipitation of metal particles and unequal growth of particles.
- glucose used as a reducing agent, it is preferable that it be mixed in 1-4 parts by weight with respect to 10 parts by weight of the metal precursor.
- the mixed solution After thoroughly dissolving PVP and the reducing agent in ethylene glycol, the mixed solution is heated up to 100-140° C. If a mixture of the metal precursor and ethylene glycol is added at this temperature, uniform metal nanoparticles may be obtained with desired size. If the heating-up is performed after adding the mixture of the metal precursor and ethylene glycol to the mixed solution of ethylene glycol, PVP and the reducing agent, it causes unequal formation of metal nanoparticles and undesirable large size of particles.
- metal precursor that is known and used for the production of metal nanoparticles, may be used without limitation in the present invention, preferably that is suitable for the alcohol reduction method.
- the metal precursor may include one or more metals selected from the group consisting of gold, silver, copper, nickel, zinc, platinum, palladium, rhodium, ruthenium, iridium, osmium, tungsten, tantalum, titanium, aluminum, cobalt, iron and a mixture thereof.
- nitrates may include inorganic acid salts such as nitrates, carbonates, chlorides, phosphates, borates, oxides, sulfonates, and sulfates, etc., and organic acid salts, such as stearates, myristates, and acetates, etc.
- organic acid salts such as stearates, myristates, and acetates, etc.
- nitrates may be more preferable, as they are economical and widely used.
- the metal precursor may include silver precursors such as AgNO 3 , AgBF 4 , AgPF 6 , Ag 2 O, CH 3 COOAg, AgCF 3 SO 3 , AgClO 4 , AgCl, and CH 3 COCH ⁇ COCH 3 Ag, copper salts such as of Cu(NO 3 ), CuCl 2 , and CuSO 4 , and nickel salts such as of NiCl 2 , Ni(NO 3 ) 2 , and NiSO 4 , etc.
- silver precursors such as AgNO 3 , AgBF 4 , AgPF 6 , Ag 2 O, CH 3 COOAg, AgCF 3 SO 3 , AgClO 4 , AgCl, and CH 3 COCH ⁇ COCH 3 Ag
- copper salts such as of Cu(NO 3 ), CuCl 2 , and CuSO 4
- nickel salts such as of NiCl 2 , Ni(NO 3 ) 2 , and NiSO 4 , etc.
- the solution of the metal precursor is preferably added once within a short time to the mixed solution set forth above. That is because when the metal precursor is added several times, the size of metal nanoparticles varies with addition time, which results in formation of metal nanoparticles having an uninformed particle distribution.
- the alcohol-based compound refers to a compound having alcohol group(—OH), but not limited to these, of which example may include methanol, ethanol, ethylene glycol, and diethylene glycol.
- These alcohol-based solvents may readily be mixed with PVP or ethylene glycol that is used as a reducing agent.
- These alcohol-based compounds may be preferably mixed in 30-50 parts by weight with respect to 10 parts by weight of the metal precursor, which is enough amount to dissolve the metal precursor.
- the reaction set forth above is preferably performed for 30 minutes to 4 hours. An excess reaction over 4 hours is not preferable because it causes precipitation of the metal particles on the wall of a reaction chamber.
- the compounds react with each other, the cores of particles are formed and then the cores grow to form metal nanoparticles.
- ethylene glycol is added again and subsequently excess amount of acetone is added. They separate out metal nanoparticles from by-products and unreactants of the reaction by using difference of solubility.
- the acetone is preferably used in 200-300 parts by weight with respect to 100 parts by weight of total weight of the solution in the previous step.
- acetone methanol, ethanol, or a mixed solution thereof may be used.
- the additionally annexed ethylene glycol is preferably added in more than 2 parts by weight with respect to 1 part by weight of the capping molecule, more preferably 2-10 parts by weight.
- the metal nanoparticles capped with PVP may be selectively separated from the unreactants and the by-products by using difference of solubility.
- the metal nanoparticles are not readily separated from the by-products when using acetone alone in the end stage of the reaction, the additional annexing of ethylene glycol is required.
- ethylene glycol should be added in the end stage of the reaction.
- the dispersion stability is more than 98%.
- the dispersion stability becomes very low of 0.1 weight %.
- FIG. 1 is data representing the result of TGA analysis (Thermo Gravimetric Analysis) for the metal nanoparticles produced according to an embodiment of the invention.
- TGA analysis Thermo Gravimetric Analysis
- FIGS. 2 and 3 are FE-SEM images of the metal nanoparticles produced according to preferred embodiments of the invention.
- FIG. 4 is a graph that represents the result of UV-VIS spectroscopy(UV spectrum) of the metal nanoparticles produced according to preferred embodiments of the invention.
- FIG. 5 is a graph that represents the result of particle size analysis of the metal nanoparticles produced according to preferred embodiments of the invention. This particle size analysis shows that average 10-30 nm of the metal nanoparticles may be obtained and the particle distribution rate are even.
- PVP 30 g and glucose 6.5 g were thoroughly dissolved in ethylene glycol 200 g and the mixture was poured to a flask. The temperature was raised up to 120° C. Silver nitrate 20 g was thoroughly dissolved in 60 g of ethylene glycol and the mixture was then promptly added into the reaction flask and agitated for 35 minutes. 200 g of ethylene glycol was added to the reaction product, 1200 ml of acetone was added and silver nanoparticles were selectively separated through centrifugation. When the silver nanoparticles were completely dried, 10.3 g of powder was obtained. As shown in FIG. 1 , the examination of particle distribution through FE-SEM confirmed that uniform nanoparticles of 16 nm were generated.
- PVP 30 g and glucose 1 g were thoroughly dissolved in ethylene glycol 200 g and the mixture was poured to the reaction flask. The temperature was raised up to 120° C. Silver nitrate 10 g was thoroughly dissolved in 50 g of ethylene glycol and the mixture was then promptly put into a flask and agitated for 30 minutes. After cooling to room temperature, 200 g of ethylene glycol was added to the reaction product, 1500 ml of acetone was added and silver nanoparticles were selectively separated through centrifugation. When the silver nanoparticles were completely dried, 5 g of powder was obtained. As shown in FIG. 2 , the examination of particle distribution through FE-SEM confirmed that uniform nanoparticles of 25 nm were generated.
- the metal nanoparticles obtained from the examples had more than 50% of yield rate, while the yield rate of the metal nanoparticles from the comparison example was lower than this.
- the method of production of metal nanoparticles according to the present invention significantly can reduce the unreactant to produce uniform metal nanoparticles with a high yield rate.
- the method of production of metal nanoparticles according to the present invention can separate desired metal nanoparticles efficiently with ethylene glycol.
- the metal nanoparticles of the invention have high dispersion stability as they are capped with polyvinyl pyrrolidone(PVP).
- the invention also provides conductive ink including these metal nanoparticles.
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Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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KR20050085708A KR100716201B1 (ko) | 2005-09-14 | 2005-09-14 | 금속 나노 입자 및 이의 제조방법 |
KR10-2005-0085708 | 2005-09-14 |
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Cited By (33)
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US20080034921A1 (en) * | 2005-01-14 | 2008-02-14 | Cabot Corporation | Production of metal nanoparticles |
US20080078302A1 (en) * | 2006-09-29 | 2008-04-03 | Jong Taik Lee | Ink for ink jet printing and method for preparing metal nanoparticles used therein |
US20090025510A1 (en) * | 2007-07-23 | 2009-01-29 | Samsung Electro-Mechanics Co., Ltd. | Method for manufacturing nickel nanoparticles |
US20090266202A1 (en) * | 2006-07-28 | 2009-10-29 | National Taiwan University | Method for manufacturing metal nanoparticle |
US20100251856A1 (en) * | 2009-04-03 | 2010-10-07 | Venugopal Santhanam | Methods for preparing metal and metal oxide nanoparticles |
US20110042210A1 (en) * | 2009-08-19 | 2011-02-24 | Samsung Electro-Mechanics Co., Ltd. | Method for preparing metal nanoparticles using metal seed and metal nanoparticles comprising metal seed |
US20110042125A1 (en) * | 2009-08-19 | 2011-02-24 | Samsung Sdi Co., Ltd. | Conductive ink, method of preparing metal wiring using conductive ink, and printed circuit board prepared using method |
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US20110313059A1 (en) * | 2009-03-02 | 2011-12-22 | Magda Blosi | Process for preparing stable suspensions of metal nanoparticles and the stable colloidal suspensions obtained thereby |
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Also Published As
Publication number | Publication date |
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KR100716201B1 (ko) | 2007-05-10 |
JP4520969B2 (ja) | 2010-08-11 |
KR20070031060A (ko) | 2007-03-19 |
JP2007084930A (ja) | 2007-04-05 |
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