US20130205950A1 - Method for producing nanoparticles from a noble metal and use of the nanoparticles thus produced - Google Patents

Method for producing nanoparticles from a noble metal and use of the nanoparticles thus produced Download PDF

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US20130205950A1
US20130205950A1 US13/813,566 US201113813566A US2013205950A1 US 20130205950 A1 US20130205950 A1 US 20130205950A1 US 201113813566 A US201113813566 A US 201113813566A US 2013205950 A1 US2013205950 A1 US 2013205950A1
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nanoparticles
noble metal
silver
accordance
platinum
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Robert Jurk
Marco Fritsch
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • 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
    • 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
    • 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
    • C09D11/32—Inkjet printing inks characterised by colouring agents
    • C09D11/322—Pigment inks
    • 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
    • C09D11/52—Electrically conductive inks
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0466—Alloys based on noble metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/02—Alloys based on gold
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/04—Alloys based on a platinum group metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver
    • 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 invention relates to a method for producing nanoparticles from a noble metal and to the use of the nanoparticles produced using the method for the production of printable suspensions, inks or pastes for printing or for forming functional layers (e.g. electrically conductive layers) or decorative (e.g. optically reflective layers) surfaces.
  • Nanoparticles of silver, gold or platinum should be produced using the method. The catalytic effect of these noble metals can also be utilized.
  • Nanoparticles of noble metals, in particular silver are used for producing inks which can be applied to substrates using various application methods. Since the sintering behavior of such inks, and in this respect in particular the temperature required for a sufficient sintering, is influenced by the particle size and also by the particle size distribution, it is of great interest to be able to produce such nanoparticles from noble metal with a predefinable particle size and, optionally, also particle size distribution.
  • a chemical compound of the respective noble metal should be dissolved in an aqueous solution or the coarse-grain noble metal should be dissolved in an acid mixture.
  • At least one surfactant or an aqueous or alcohol solution containing at least one surfactant should be added to the respective solution; with silver and platinum a reductant should additionally be added.
  • the influencing of the particle size of the nanoparticles produced using the method takes place with the parameters: concentration of the chemical compound or of the noble metal; temperature; and the fraction of surfactant.
  • concentration of the chemical compound or of the noble metal concentration of the chemical compound or of the noble metal
  • temperature temperature; and the fraction of surfactant.
  • the pH or the setting of specific pH values in individual method steps can also have an influence on the synthesis.
  • the noble metal particles precipitated from the respective solution are centrifuged out.
  • the particular size can be reduced with a smaller concentration of the chemical compound used or of the noble metal in the respective solution and/or at an increased temperature and/or an increased fraction of surfactant.
  • An increased pH can in particular result in smaller particle sizes in the production of nanoparticles from silver or platinum.
  • noble metals can be dissolved in a mixture of hydrochloric acid and nitric acid for the production of nanoparticles from gold or platinum.
  • the mixture ratio should in this respect be 75% by weight hydrochloric acid, 25% by weight nitric acid.
  • This acid mixture is also known as aqua regia. Tetrachloroauric acid or hexachloroplatinic acid then forms on the dissolving.
  • Pure platinum in the form of nanoparticles can precipitate by reduction by an addition of hydrazine hydrate.
  • Nitric acid of at least 50% can be used for this.
  • the nitric acid should be heated and should have a temperature in the range 100° C. to 150° C., preferably 120° C.
  • AgNO 3 is formed and a surfactant and additionally hydroxylamine can again be added, preferably in aqueous solution, as a reductant.
  • the method is simplified by the use of the pure noble metals gold, silver and platinum which are dissolved directly in acid, and the costs can also be reduced since the use of suitable chemical compounds of these noble metals whose purchasing costs are higher than those of the pure noble metals can be dispensed with. In addition, smaller losses of noble metal occur since the fractions not converted into nanoparticles can be used again.
  • the use of the surfactant(s) has the result that an agglomeration of the individual nanoparticles can be avoided.
  • surfactants can be used which are selected from alkoxylates, alkylolamides, esters, amine oxides, alkyl polyglucosides, alkylphenols, arylalkyl phenols, water-soluble homopolymers, water-soluble statistical copolymers, water-soluble block copolymers, water soluble graft copolymers, polyvinyl alcohols, copolymers of polyvinyl alcohols and polyvinyl acetates, polyvinylpyrrolidones, cellulose, starch, gelatins, gelatin derivatives, amino acid polymers, polylysine, polyasparagine acid, polyacrylates, polyethylene sulfonates, polystyrene sulfonates, polymethacrylates, condensation products of aromatic sulfonic acids with formaldehyde, napththalenesulfonates, lignosulfonates, copolymerizates of acrylic monomers,
  • polyvinylpyrrolidones, block copolyethers and block copolyethers with polystyrene blocks, hydroxyl functional carboxylic acid esters with pigment-affinic groups, copolymers with pigment-affinic groups, preferably acidic groups, alkylolammonium salts of a block copolymer with pigment-affinic groups, preferably acidic groups, and/or mixtures or solutions hereof are particularly preferred.
  • Block copolymers with pigment-affinic groups such as polystyrene blocks (e.g. Disperbyk 190 of the company BYK-Chemie, Wesel), alkylolammonium salts of a copolymer with acidic groups (e.g. Disperbyk 180 of the company BYK-Chemie, Wesel) or polyvinylpyrrolidones (e.g. PVP of the company Fluka) or mixtures thereof can particularly preferably be used as surfactants.
  • Dysperbyk 180 is an alkylammonium salt of a copolymer with acidic groups.
  • Dysperbyk 190 is an aqueous solution of a high-molecular block copolymer with pigment-affinic groups.
  • Hydroxylamine is advantageous for the production of nanoparticles from silver and hydrazine hydrate or sodium borohydride can advantageously be used as a reductant for the production of nanoparticles from platinum.
  • the pH in the respective solution can be set during the synthesis using added NaOH or added NH 3 .
  • a setting of the pH is also possible using piperidine and thus free of sodium.
  • the reaction vessel is cooled to room temperature while stirring continuously and is subsequently centrifuged.
  • a separation of coarse particles larger than 300 nm at an acceleration of 800 g for 10 min. is suitable for the described reaction conditions.
  • centrifuging takes place for 2 hours at a maximum acceleration of the centrifuge, e.g. at 4600 g.
  • a yield of 75-80% of the silver mass used in nanoparticles is thus possible.
  • the coarse particles can furthermore be burnt out of the adhering organic dispersant and can be returned to AgNO 3 again by subsequent conversion using boiling HNO 3 .
  • a variation of the particle size of the nanoparticles to be obtained is possible by a variation of the concentration of the raw materials used.
  • Table 1 provides an overview of 4 different synthesis approaches using the obtained mean particle sizes and the particle morphology in FESEM. REM images of nanoparticles in accordance with examples 1.1 and 1.2 from Table 1 are shown in FIG. 1 .
  • the particles produced from the synthesis in accordance with Example 1 are further processed to a silver particle ink.
  • the centrifuge sediment after 2 h of centrifuging at 4600 g is charged with as little water as possible for this purpose and is provided in a ball mill with 10% by weight PEG (polyethylene glycols) and 0.05% by weight Disperbyk 348 (figures with respect to the mass of the sediment) and dispersed over a time period of 0.5 hours.
  • PEG polyethylene glycols
  • Disperbyk 348 figures with respect to the mass of the sediment
  • the viscosity of the ink amounts to 21 mPas at a shear rate of 100/s and at 25° C. in the cylinder beaker system (TA Instruments, DA100).
  • the solid content of the ink is calculated using a density measurement and amounted to 54% by weight at a density of 2.05 g/cm 3 .
  • An FESEM shot on polished Al is shown in FIG. 2 .
  • This ink was deposited on silicon with the aid of a Dimatix SQ128 printhead.
  • the layer thickness in a single print amounted to 2.5 ⁇ m, with a line width of 37 ⁇ m-40 ⁇ m.
  • layers thicknesses between 18 ⁇ m and 20 ⁇ m are achieved, with line widths of 60 ⁇ m-65 ⁇ m.
  • the printed structures were burnt in a tube furnace at a heating rate of 10 K/min up to a temperature of 380° C.
  • the electrical resistance of the printed structure is simultaneously determined via a 4-point measurement in this process.
  • the printed layer was previously dried at 180° C. for 0.5 h. This already allows it to become electrically conductive.
  • a commercial gold powder (Heraeus 200-03) were completely dissolved in at least 20 ml 75% by weight HCl with 25% by weight HNO3 at 50° C. Since contaminants are to be avoided, no metallic devices should be used for this purpose.
  • the solution was passed through a hard paper filter. 800 ml deionized water was mixed with the surfactants Disperbyk 180 and Disperbyk 190 using a magnetic stirrer in a glass beaker. The quantity of added surfactant in each case corresponded to 60% by weight of the previously converted gold mass.
  • the acid solution was subsequently added into the water-surfactant mixture and was titrated to a neutral pH via the addition of NaOH (3 . . . 5 mol).
  • a pH electrode was used for this purpose. The pH was first stabilized at pH 7 and then increased step-wise to a pH of 10 after a further 5 to 7 minutes. Gold nanoparticles were precipitated in the solution by this increase in the pH with a stabilization at pH 10.
  • Coarser particles were separated by the use of a centrifuge with 2000 r.p.m. (800 times the force of gravity g) for 10 min. and can thus be recycled.
  • a separation of finer particles with a mean particle size d 50 of ⁇ 80 nm should be centrifuged again. In this respect, centrifuging should be carried out at a speed of 4700 r.p.m. (4600 times the force of gravity g) over a time period of 2 hours.
  • the remaining gold particle sludge was washed with water to reduce the sodium content in the solution.
  • residues of sodium chloride were present from the synthesis which can be reduced by further washing of the solution containing particles. Particles having a size which were suitable for the production of printable ink jet ink were thus able to be obtained.
  • the gold sludge was first topped up with water after the centrifuge treatment so that a gold solid content of 25% by weight in the solution was achieved.
  • the density of the ink was then at 1.3 g/cm 3 .
  • the surface tension was lowered to 30 nNm by adding 0.05% by weight Byk 348.
  • the produced gold nanoparticle ink was printed on silicon wafers and on aluminum oxide substrates in 21 mm long meander test structures using a commercial ink jet device with a Dimatiax SE128 printhead.
  • the achieved line width amounted to 120 ⁇ m and the layer thickness in a simple print 1.5 ⁇ m.
  • a considerable sintering a rose with a drop of the electrical resistance to 4.7 ohm.
  • a specific electrical resistance of the printed gold track of 9.53 ⁇ ohm-cm results from this which corresponds to a value of less than five times that of pure bulk gold at 2.21 ⁇ ohm-cm.
  • the initially produced acid mixture in which the gold was contained was added to the surfactant-water mixture and the whole was homogenized.
  • a pH sensor was used for monitoring the pH.
  • This mixture was then heated to 60° C. and then 3-5 mol NaOH was added. After reaching a pH of 7, it then fell to a pH between 1.5 and 2. The pH reached is influenced by the surfactant fraction.
  • the synthesis reaction came to an end; gold particles were precipitated.
  • the finer nanoparticles were then able to be separated by means of centrifuging, analog to Example 2.
  • the sediment can be separated by centrifuging and can subsequently be washed a multiple of times to completely remove Na and NaCl.
  • the non-used coarse fraction of the sediment can be recycled. Larger gold losses are thereby avoided.
  • a first step 10 g of a commercial platinum powder were completely dissolved in at least 16 ml of a mixture of 75% by weight HCl with 25% by weight HNO 3 at a temperature at the boiling point of nitric acid at approx. 86° C. Since other metals would likewise dissolve in the acid mixture and would effect a contamination of the platinum, no metallic devices should be used.
  • the solution was passed through a hard paper filter. 500 ml deionized water was mixed with surfactant (Disperbyk 180 and Disperbyk 190) using a magnetic stirrer in a glass beaker. The quantity of added surfactant corresponded to 100% by weight of the previously produced acid mixture.
  • the acid solution was then added to the water-surfactant mixture and homogenized while stirring.
  • the immersion of a pH electrode allowed the monitoring of the pH for the following synthesis.
  • 25% hydrazine hydrate solution 70 . . . 80% of the mass of the platinum used
  • the pH fell from 7 back to a pH of 1 to 2.
  • the pH was stabilized at pH 7 by further metering in of NaOH. No further pH change occurred after a further 5 to 10 minutes.
  • the pH was thereupon increased to a pH of 9 by a further addition of NaOH and stabilized there.
  • Platinum nanoparticles are precipitated in the solution during the increase in the pH. Coarser particle sizes were separated by using a centrifuge with 2000 r.p.m. (800 times the force of gravity g) for 10 min. The remaining liquid was centrifuged out at a speed of 4600 r.p.m. A fine sediment was obtained which can be washed and processed into a printable ink. The remaining platinum particle sludge was washed with water to reduce the sodium content in the solution.
  • This solution was likewise filtered by means of a hard paper filter.
  • the pH was influenced by titrating 3-5 mol NaOH.
  • a pH of 10 was reached after a very short time and platinum particles were precipitated.
  • Nanoparticles in the desired particle size range were able to be separated from the sediment by centrifuging, as explained in Example 3.
  • a volume of at least 5 liters must be provided for the described reaction due to the strong gas development in the reaction.
  • the reaction comes to a stop after approx. 30 s. In this time, the temperature in the solution increases to around 40° C.
  • the reaction vessel is cooled to room temperature while stirring continuously and is subsequently centrifuged. A separation of coarse particles larger than 300 nm at an acceleration of 800 g for 10 min. is suitable for the described reaction conditions. Subsequently, centrifuging takes place for 2 hours at a maximum acceleration of the centrifuge, e.g. at 4600 g. A yield of 65-75% of the silver mass used in nanoparticles is thus possible.
  • the particles which are too coarse for the application can furthermore be liberated from the adhering organic dispersant by burning out and can subsequently again be supplied to the process as pure silver.
  • the particles produced from the above-described synthesis are further processed to a silver particle ink.
  • the centrifuge sediment is for this purpose, after centrifuging at 4600 g for 2 hours, charged with as little water as possible and dispersed in a ball mill for 0.5 hours.
  • Additives such as 10% by weight PEG (polyethylene glycol) and 0.05% by weight Disperbyk (figures with respect to the mass of the sediment) can be added to improve the printability.
  • PEG polyethylene glycol
  • Disperbyk figures with respect to the mass of the sediment
  • the viscosity of the ink amounts to 18 mPas at a shear rate of 100/s and at 25° C. in the cylinder beaker system (TA Instruments, DA100).
  • the solid content of the ink was calculated using a density measurement and amounted to 75% by weight at a density of 3.30 g/cm 3 .
  • An FESEM shot of the Ag particles of this ink on polished Al is shown in FIG. 3 .
  • This ink was deposited on silicon with the aid of a Dimatix SQ128 printhead.
  • the layer thickness in a single print amounted to 3.2 ⁇ m, with a line width of 50 ⁇ m.
  • layer thicknesses of 16 ⁇ m are reached, with line widths of 60 ⁇ m.
  • An FESEM shot of these printed layers is shown in FIG. 4 .
  • the printed structures were burnt in a tube furnace at a heating rate of 10 K/min up to a temperature of 1000° C. In this respect, the electrical resistance of the printed structure was determined using a 4-point measurement.
  • the curve in dependence on the temperature is shown in FIG. 5 .
  • the printed layer already becomes conductive at temperature above 275° C.
  • Example 1 Unlike Example 1, a “coarser” ink with an extremely high solid content can be produced using the silver particles obtained in accordance with Example 6. This achievable solid fraction in printable inks of up to 75% by weight greatly surpasses that of conventional printable inks with silver nanoparticles. A solid fraction of a maximum of 40% by weight is known from them.
  • the temperature in the solution increases to around 40° C.
  • the reaction vessel is cooled to room temperature while being stirred continuously and is subsequently centrifuged.
  • a separation of coarse particles larger than 300 nm at an acceleration of 800 g over a period of 10 min. is suitable for the described reaction conditions.
  • centrifuging takes place for 2 hours at a maximum acceleration of the centrifuge, e.g. at 4600 g.
  • a yield of 65-75% of the silver mass used in nanoparticles is thus possible.
  • the particles which are too coarse for the application can furthermore be liberated from the adhering organic dispersant by burning out and can subsequently again be supplied to the process as pure silver.
  • the particles produced from the above-described synthesis are further processed to a silver particle ink.
  • the centrifuge sediment is for this purpose, after centrifuging at 4600 g for 2 hours, charged with as little water as possible and dispersed in a ball mill for 0.5 hours.
  • Additives such as 10% by weight PEG (polyethylene glycol) and 0.05% by weight Disperbyk (figures with respect to the mass of the sediment) can be added to improve the printability.
  • PEG polyethylene glycol
  • Disperbyk figures with respect to the mass of the sediment
  • the viscosity of the ink amounts to 20 mPas at a shear rate of 100/s and at 25° C. in the cylinder beaker system (TA Instruments, DA100).
  • the solid content of the ink is calculated using a density measurement and amounted to 74% by weight at a density of 3.29 g/cm 3 .

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US13/813,566 2010-08-03 2011-07-29 Method for producing nanoparticles from a noble metal and use of the nanoparticles thus produced Abandoned US20130205950A1 (en)

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DE102010033924A DE102010033924A1 (de) 2010-08-03 2010-08-03 Verfahren zur Herstellung von Nanopartikeln aus einem Edelmetall und die Verwendung der so hergestellten Nanopartikel
DE102010033924.5 2010-08-03
PCT/DE2011/001551 WO2012016565A2 (de) 2010-08-03 2011-07-29 Verfahren zur herstellung von nanopartikeln aus einem edelmetall und die verwendung der so hergestellten nanopartikel

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