WO2014104805A1 - 담체에 담지된 중공 금속 나노입자 - Google Patents
담체에 담지된 중공 금속 나노입자 Download PDFInfo
- Publication number
- WO2014104805A1 WO2014104805A1 PCT/KR2013/012287 KR2013012287W WO2014104805A1 WO 2014104805 A1 WO2014104805 A1 WO 2014104805A1 KR 2013012287 W KR2013012287 W KR 2013012287W WO 2014104805 A1 WO2014104805 A1 WO 2014104805A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- metal nanoparticles
- carrier
- metal
- hollow
- hollow metal
- Prior art date
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- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 212
- 229910052751 metal Inorganic materials 0.000 claims description 251
- 239000002184 metal Substances 0.000 claims description 251
- 150000003839 salts Chemical class 0.000 claims description 78
- 239000002245 particle Substances 0.000 claims description 75
- 239000004094 surface-active agent Substances 0.000 claims description 63
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 46
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 45
- 238000000034 method Methods 0.000 claims description 43
- 239000000693 micelle Substances 0.000 claims description 41
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 40
- -1 lanthanum group metals Chemical class 0.000 claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 28
- 239000003638 chemical reducing agent Substances 0.000 claims description 23
- 239000010949 copper Substances 0.000 claims description 23
- 239000006185 dispersion Substances 0.000 claims description 22
- 238000004519 manufacturing process Methods 0.000 claims description 22
- 239000002105 nanoparticle Substances 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000010931 gold Substances 0.000 claims description 20
- 239000010948 rhodium Substances 0.000 claims description 20
- 239000011669 selenium Substances 0.000 claims description 20
- 239000010936 titanium Substances 0.000 claims description 20
- 229910052759 nickel Inorganic materials 0.000 claims description 16
- 229910052763 palladium Inorganic materials 0.000 claims description 16
- 229910052709 silver Inorganic materials 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 239000011651 chromium Substances 0.000 claims description 15
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 14
- 229910052697 platinum Inorganic materials 0.000 claims description 14
- 239000004332 silver Substances 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 238000000921 elemental analysis Methods 0.000 claims description 12
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052737 gold Inorganic materials 0.000 claims description 11
- 229910052684 Cerium Inorganic materials 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 10
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 10
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 10
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 239000003945 anionic surfactant Substances 0.000 claims description 10
- 229910052797 bismuth Inorganic materials 0.000 claims description 10
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 10
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 10
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 10
- 229910052741 iridium Inorganic materials 0.000 claims description 10
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims description 10
- 239000011733 molybdenum Substances 0.000 claims description 10
- 229910052762 osmium Inorganic materials 0.000 claims description 10
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 10
- 229910052702 rhenium Inorganic materials 0.000 claims description 10
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 10
- 229910052703 rhodium Inorganic materials 0.000 claims description 10
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 10
- 229910052707 ruthenium Inorganic materials 0.000 claims description 10
- 229910052711 selenium Inorganic materials 0.000 claims description 10
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- 239000003093 cationic surfactant Substances 0.000 claims description 9
- 239000006229 carbon black Substances 0.000 claims description 7
- 229910017052 cobalt Inorganic materials 0.000 claims description 7
- 239000010941 cobalt Substances 0.000 claims description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
- 239000010937 tungsten Substances 0.000 claims description 7
- 150000002739 metals Chemical class 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 229910052752 metalloid Inorganic materials 0.000 claims description 5
- 150000002738 metalloids Chemical class 0.000 claims description 5
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- JPNWDVUTVSTKMV-UHFFFAOYSA-N cobalt tungsten Chemical compound [Co].[W] JPNWDVUTVSTKMV-UHFFFAOYSA-N 0.000 claims description 3
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- 238000001179 sorption measurement Methods 0.000 description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 5
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- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
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- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
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- ITFGZZGYXVHOOU-UHFFFAOYSA-N n,n-dimethylmethanamine;methyl hydrogen sulfate Chemical compound C[NH+](C)C.COS([O-])(=O)=O ITFGZZGYXVHOOU-UHFFFAOYSA-N 0.000 description 1
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- 230000007935 neutral effect Effects 0.000 description 1
- ZHALDANPYXAMJF-UHFFFAOYSA-N octadecanoate;tris(2-hydroxyethyl)azanium Chemical compound OCC[NH+](CCO)CCO.CCCCCCCCCCCCCCCCCC([O-])=O ZHALDANPYXAMJF-UHFFFAOYSA-N 0.000 description 1
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- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
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- RTVVXRKGQRRXFJ-UHFFFAOYSA-N sodium;2-sulfobutanedioic acid Chemical class [Na].OC(=O)CC(C(O)=O)S(O)(=O)=O RTVVXRKGQRRXFJ-UHFFFAOYSA-N 0.000 description 1
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- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- WBWWGRHZICKQGZ-GIHLXUJPSA-N taurocholic acid Chemical compound C([C@@H]1C[C@H]2O)[C@@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@@H]([C@@H](CCC(=O)NCCS(O)(=O)=O)C)[C@@]2(C)[C@H](O)C1 WBWWGRHZICKQGZ-GIHLXUJPSA-N 0.000 description 1
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/892—Nickel and noble metals
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Definitions
- the present specification relates to hollow metal nanoparticles supported on a carrier.
- Nanoparticles are particles with nanoscale particle sizes, which are completely different from bulk materials due to their large specific surface area and quantum confinement effect, in which the energy required for electron transfer varies with the size of the material. Other optical, electrical, and magnetic properties are exhibited. Therefore, due to these properties, much attention has been paid to its application in the field of catalysts, electromagnetism, optics, and medicine. Nanoparticles are intermediates between bulk and molecules, and the synthesis of nanoparticles is possible in terms of a two-way approach, a "top-down” approach and a “bottom-up” approach. ⁇
- Synthesis methods of metal nanoparticles include gamma rays and electrochemical methods.
- existing methods are difficult to synthesize nanoparticles having a uniform size and shape, or environmental pollution and high cost by using organic solvents. For these reasons, economical mass production of high quality nanoparticles was difficult.
- the problem to be solved by the present application is to provide hollow metal nanoparticles having a uniform size of high quality supported on a carrier.
- One embodiment of the present specification includes a hollow core part; And hollow metal nanoparticles including a shell portion including a first metal and a second metal on a carrier, and the average particle diameter of the expanded metal nanoparticles is 30 nm or less. To provide.
- the hollow metal nanoparticles supported on the carrier may include forming a solution by adding a first metal salt, a second metal salt, and a surfactant to a solvent; Adding and dispersing a carrier to the solution; And adding a reducing agent to the solution to form hollow metal nanoparticles supported on a carrier, wherein the forming of the solution includes forming a micelle in which the surfactant forms a micelle, and the outside of the micelle.
- the hollow metal nanoparticles are provided with a hollow metal nanoparticles supported on a carrier, characterized in that the micelle region comprises a hollow.
- hollow metal nanoparticles of uniform size to a few nanometers, there is an advantage that can be used in various fields because of excellent adhesion or dispersion between the carrier and the hollow metal nanoparticles.
- Figure 1 shows a model of the hollow metal nanoparticles containing a surfactant in the hollow metal nanoparticles supported on the carrier prepared according to Example 1.
- FIG. 2 shows a model of hollow metal nanoparticles in which a surfactant is removed from hollow metal nanoparticles supported on a carrier prepared according to Example 1.
- Figure 3 shows a model of the hollow metal nanoparticles containing a surfactant among the hollow metal nanoparticles supported on the carrier prepared according to Example 2.
- FIG. 4 shows a model of a surfactant-free state and hollow metal nanoparticles among hollow metal nanoparticles supported on a carrier prepared according to Example 2.
- Figure 5 shows a cross-section of the hollow metal nanoparticles prepared according to Examples 1 to 4 supported on the carrier.
- FIG. 6 shows that a general carrier-supporting nanoparticle is agglomerated on a carrier W 201
- FIG. 7 shows a transmission electron microscope (TEM) image of hollow metal nanoparticles supported on a carrier prepared according to Example 1.
- TEM transmission electron microscope
- FIG. 8 shows a transmission electron microscope (TEM) image of hollow metal nanoparticles supported on a carrier prepared according to Example 1.
- FIG. ' shows a transmission electron microscope (TEM) image of hollow metal nanoparticles supported on a carrier prepared according to Example 1.
- FIG. ' shows a transmission electron microscope (TEM) image of hollow metal nanoparticles supported on a carrier prepared according to Example 1.
- FIG. ' shows a transmission electron microscope (TEM) image of hollow metal nanoparticles supported on a carrier prepared according to Example 1.
- FIG. 9 shows a transmission electron microscope (TEM) image of hollow metal nanoparticles supported on a carrier prepared according to Example 3.
- TEM transmission electron microscope
- FIG. 10 shows a transmission electron microscope (TEM) image of hollow metal nanoparticles supported on a carrier prepared according to Example 4.
- TEM transmission electron microscope
- FIG. 11 shows a transmission electron microscope (TEM) image of vaporized metal nanoparticles supported on a carrier prepared according to Example 2.
- TEM transmission electron microscope
- the hollow means that the core portion of the hollow metal nanoparticle is empty.
- the hollow may be used as the same meaning as the hollow core.
- the hollow includes the terms hollow, hole, void, porous.
- the hollow may comprise a space in which no internal material is present at least 50% by volume, specifically at least 70% by volume, more specifically at least 80% by volume.
- at least 50% by volume, in particular at least 70% by volume, more specifically at least 80% by volume may include a void space.
- One embodiment of the present application is a hollow core (core) portion; And hollow metal nanoparticles including a shell portion including a first metal and a second metal on a carrier, and the average particle diameter of the hollow metal nanoparticles is 30 ⁇ or less. to provide.
- the average particle diameter of the hollow metal nanoparticles may be 30 nm or less, more specifically 20 nm or less, or 10 nm or less. Alternatively, the average particle diameter of the hollow metal nanoparticles may be 6 nm or less. The average particle diameter of the hollow metal nanoparticles may be 1 nm or more. When the particle diameter of the hollow metal nanoparticles is 30 nm or less, there is a great advantage that the nanoparticles can be used in various fields. Moreover, when the particle diameter of a hollow metal nanoparticle is 20 nm or less, it is more preferable.
- the particle diameter of the hollow metal nanoparticles is 10 ⁇ or less, or 6 nm or less, the surface area of the particles As it becomes wider, there is an advantage in that the possibility of use in various fields becomes larger.
- the efficiency can be significantly increased.
- the average particle diameter of the hollow metal nanoparticles is measured for 200 or more hollow metal nanoparticles using graphic software (MAC-View), and the average particle diameter is measured through the obtained statistical distribution.
- MAC-View graphic software
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 30 nm or less.
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 20 nm or less.
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 15 nm or less.
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 12 nm or less.
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 10 nm or less.
- the average particle diameter of the hollow metal nanoparticles may be 1 nm or more and 6 nm or less.
- the degree of dispersion of the hollow metal nanoparticles may be 20% or more and 50% or less, or 20% or more and 40% or less. Specifically, according to one embodiment of the present application, the degree of dispersion of the hollow metal nanoparticles may be 25% or more and 40% or less, or 25% or more and 35% or less.
- the equipment is used to measure the dispersion degree, and after pretreatment of the sample at 400 ° C., pulse dosing using CO as adsorption gas to saturate the CO and stop dosing and stop the C0 The amount of adsorption of was calculated.
- the degree of dispersion of the hollow metal nanoparticles may be calculated as follows.
- the degree of dispersion represents the proportion of hollow metal nanoparticles revealed on the surface of the carrier. As this value is high, the ratio of the hollow metal nanoparticles revealed on the surface of the carrier is high. That is, the higher the value of the degree of dispersion, it may mean that the distribution of the hollow metal nanoparticles supported on the carrier is evenly distributed.
- the hollow metal nanoparticle is a hollow core
- the shell part may include at least one first shell including a first metal; And at least one second shell comprising a second metal.
- the second shell may be present in at least one region of the outer surface of the first shell, and may exist in a form surrounding the front surface of the outer surface of the first shell. If the second shell is present in some region of the outer surface of the first shell it may be present in the form of discontinuous faces.
- the shell part may include at least one shell including the first metal and the second metal.
- the hollow metal nanoparticles may include a hollow core; And at least one shell comprising a crab 1 metal and a crab 2 metal.
- the thickness of the shell portion may be more than Onm 5 nm or less, more specifically, more than Onm 3 nm or less. In addition, in one embodiment of the present application, the thickness of the shell portion may be greater than 1 nm and 2 nm or less.
- the average bib diameter of the hollow metal nanoparticles is 30i or less
- the thickness of the shell portion may be more than Onm 5nm or less, more specifically, the average particle diameter of the hollow metal nanoparticles is 20nm or less or 10nm or less
- the thickness of the shell portion May be greater than Onm and no greater than 3 nm.
- the hollow particle diameter of the hollow metal nanoparticles may be lnm or more and ⁇ or less, specifically lnm or more and 4 ⁇ or less.
- the thickness of each shell may be 0.25 nm or more and 5 nm or less, specifically 0.25 nm or more and 3 mm 3 or less.
- the shell portion may be a shell formed by mixing a first metal and a second metal, or may be a plurality of shells including a first shell and a crab 2 shell separately formed with different mixing ratios of the first metal and the second metal. Or a plurality of shells comprising a first shell comprising only crab 1 metal and a second shell comprising only crab 2 metal.
- the hollow volume of the hollow metal nanoparticles may be 50 vol% or more, specifically 70 vol 3 ⁇ 4 or more, and more specifically 80 vol or more of the total volume of the hollow metal nanoparticles.
- the hollow metal nanoparticles supported on the carrier prepared by the method of the present application generally replace the existing nanoparticles in the field where nanoparticles can be used. Can be used by Since the hollow metal nanoparticles supported on the carrier of the present application are very small in size and have a larger specific surface area than those of the conventional nanoparticles, the hollow metal nanoparticles may exhibit excellent activity as compared to the conventional nanoparticles. Specifically, the hollow metal nanoparticles supported on the carrier of the present application may be used in various fields such as a catalyst, a drug delivery, a gas sensor, and the like.
- the vaporized metal nanoparticles supported on the carrier may be used as an active substance formulation in cosmetics, insecticides, animal nutrition or food supplements as catalysts, or may be used as pigments in electronic products, optical articles or polymers.
- at least two major peaks representing the atomic percentage of at least one of the first metal and the second metal may exist in the elemental analysis data of the hollow metal nanoparticles.
- the peak refers to the point where the shape of the graph is sharp as the slope of the graph changes from a positive value to a negative value.
- the major peak refers to a peak located at the apex of each of the peaks of the connecting line connecting peaks among the peaks representing the atomic percentage contained in the particle in the elemental analysis data of the particle.
- the peak located at the peak of each peak may be one, but may be two or more having the same atomic percentage value.
- the major peak is a peak having a height higher than the average value of the peaks of the connecting line connecting the peaks among the peaks representing the atomic percentage contained in the particle in the elemental analysis data of the particles It means a peak located at each vertex.
- the average value of the peaks means the average value of all the peaks representing the atomic percentage.
- the major peak is the 1st or 2nd highest height ratio among the peaks of the connecting line connecting peaks among the peaks representing the atomic percentage contained in the particle in the elemental analysis data of the particle. It means the peak located at the peak of the peak having.
- the particle diameter of the hollow metal nanoparticle when the particle diameter of the hollow metal nanoparticle is 10OT, at least one major peak representing an atomic percentage of the first metal is present in an area of 0% to 30% from one end point of the particle diameter. And at least one other major peak representing the atomic percentage of the first metal in the region of 0% to 30% from the other end point of the particle diameter.
- the particle diameter of the hollow metal nanoparticle when the particle diameter of the hollow metal nanoparticle is 10, at least one major peak indicating an atomic percentage of the second metal is present in an area of 0% to 30% from one end point of the particle diameter. And at least one other major peak representing the atomic percentage of the second metal in the region of 0% to 30% from the other end point of the particle diameter.
- the particle diameter of the hollow metal nanoparticle means a starting point or one end point of the graph to which the peak of the first metal is connected, and the starting point or the end point is a point at which the graph of the peak of the crab 1 metal is started; Alternatively, it means a point where the vertical value of the graph in which the peak of the first metal is connected becomes zero.
- at least one major peak representing the atomic percentage of the second metal is present in an area of 0% to 30% from one end point of the particle diameter, and the other
- the particle diameter of the hollow metal nanoparticles means a starting point or one end point of the graph to which the peak of the second metal is connected, and the starting point or the end point is a point where the graph to which the peak of the second metal is connected or the second metal is started. It means the point where the vertical value of graph is connected to the peak of.
- the hollow metal nanoparticles are hollow cores; And a shell portion including the first metal and the second metal, wherein at least two major peaks representing the atomic percentage of the first metal in the particle and elemental analysis data are present, and the atomic percentage of the second metal is determined. Plural peaks may be present in all regions of the particle diameter.
- the hollow metal nanoparticles are hollow core (core) portion; And a shell portion including the first metal and the crab metal, wherein at least two major peaks representing the atomic percentage of the second metal in the elemental analysis data of the particle are present, and the atomic percentage of the first metal is determined. Plural peaks may be present in all regions of the particle diameter.
- the hollow metal nanoparticles are hollow core (core) portion; And At least two major peaks representing the atomic percentage of the first metal in the elemental analysis data of the particle, the shell portion including the first metal and the crab second metal, and representing the atomic percentage of the second metal. There may be at least two major peaks.
- the cross-sectional elemental analysis data of the particles may be obtained by using an energy dispersive spectrometer (EDS).
- EDS energy dispersive spectrometer
- the cross-sectional elemental analysis data is to determine what elements are measured in the two-dimensional region when the particles are transmitted through the above. That is, in the case of the hollow metal nanoparticles, the shell part can be observed in the form of a major peak because the elements are distributed more densely than the region where the hollow is located. Furthermore, when the amount of the element is relatively small, it can be observed as a plurality of peaks in the entire region.
- the shell portion of the hollow metal nanoparticle may be formed of a metal including a first metal and a second metal. That is, the shell portion of the hollow metal nanoparticles of the present invention may be formed of a metal rather than a metal oxide.
- the shell portion of the present application is present in the front of the outer hollow, it may be present in a form surrounding the hollow. Specifically, according to one embodiment of the present application, the shell portion may be formed on the entire outer surface of the hollow core portion. That is, the shell portion of the present application may form the form of the hollow metal nanoparticles.
- the hollow metal nanoparticles may have a spherical shape.
- the shell portion of the present application may have a spherical shape including a hollow core.
- the spherical shape of the present application does not mean only a perfect spherical shape, but may include an approximately spherical shape.
- the hollow metal nanoparticles may not have a spherical outer surface, and the radius of curvature may not be constant in one hollow metal nanoparticle.
- the shell portion may be a shell of a single layer, or may be a shell of two or more layers.
- the shell portion may include a first shell including a first metal; And a second shell including a second shell including a second metal.
- the first metal and the crab 2 metal may be present in a mixed form. At this time, they may be uniformly or nonuniformly mixed.
- the atomic bag of the first metal and the crab 2 metal of the shell portion The fraction ratio may be 1: 5 to 10: 1.
- the ratio of the crab metal in the shell may be present in a gradation state.
- the ratio with the second metal may be present in the shell at a constant rate, and the first metal may be present in the form of a gradient.
- the ratio of the first metal at the center may be the highest, and the ratio of the first metal may be lowered toward both ends of the shell. That is, the ratio of the first metal increases from the portion adjacent to the hollow core toward the center of the shell, and the ratio of the first metal decreases from the center of the shell toward the outer edge of the shell. At this time, a point where the ratio of the first metal is the highest may exist in the center of the shell.
- the portion of the shell in contact with the hollow core may be present in a volume of at least 50% by volume of the first metal, or at least 70 volume 3 ⁇ 4, and in the surface of the shell in contact with the outside at least of 50 volume of 3 ⁇ 4, or 70 It may be present in volume% or more.
- the shell may be a first shell or a second shell separately formed with different mixing ratios of the first metal and the second metal.
- the atomic percentage ratio of the first metal to the second metal in each shell may be 1: 5 to 10: 1.
- each shell may include only the first metal or the second metal.
- the hollow metal nanoparticles may be a vacuum core; At least one first shell comprising a crab 1 metal; And one or more second shells comprising a second metal.
- the crab shell may be present in the front of the hollow outer.
- the second shell may be present in at least one region of the outer surface of the first shell and may be in a form surrounding the front surface of the outer surface of the U shell. If the crab 2 shell is present in some area of the outer surface of the first shell it may be present in the form of discontinuous face.
- the hollow metal nanoparticle includes a hollow core, a first shell including a crab metal formed on the entire outer surface of the hollow core, and a second metal formed on the entire outer surface of the first shell. It may include a second shell comprising.
- the hollow metal nanoparticles may include a shell of a single layer including a first metal and a second metal formed on the entire outer surface of the hollow core.
- the hollow core may include a surfactant having a positive charge.
- the crab metal is in the group consisting of metal, metalloid, lanthanum group metal and actinium group metal belonging to Group 3 to 15 of the periodic table It may be selected, specifically platinum (Pt), ruthenium (Ru), rhodium (Rh), molybdenum (Mo), osmium (0s), iridium (Ir), rhenium (Re), palladium (Pd), vanadium (V ), Tungsten (W), cobalt (Co), iron (Fe), selenium (Se), nickel (Ni), bismuth (Bi), tin (Sn), crumb (Cr), titanium (Ti), gold It may be one selected from the group consisting of (Au), cerium (Ce), silver (Ag) and copper (Cu).
- the second metal may be different from the first metal.
- the second metal may be selected from the group consisting of metals, metalloids, lanthanum group metals, and actinium group metals belonging to Groups 3 to 15 of the periodic table, specifically, platinum (Pt), ruthenium (Ru), and rhodium (Rh), molybdenum (Mo), osmium (0s), iridium (Ir), rhenium (Re), palladium (Pd), vanadium (V), tungsten cobalt (Co), iron (Fe), selenium (Se), At least selected from the group consisting of nickel (Ni), bismuth (Bi), tin (Sn), crumb (Cr), titanium (Ti), gold (Au), cerium (Ce), silver (Ag) and copper (Cu) It can be either.
- the first metal may be selected from the group consisting of platinum (Pt), silver (Ag), palladium (Pd), and gold (Au), and even more specifically, platinum (Pt).
- the second metal is ruthenium (Ru), rhodium (Rh), molybdenum (Mo), osmium (0s), iridium (Ir), rhenium (Re), palladium (Pd), vanadium (V), tungsten (W) ), Cobalt (Co) ⁇ Iron (Fe), Selenium (Se), Nickel (Ni), Bismuth (Bi), Tin (Sn), Chromium (Cr), Titanium (Ti), Cerium (Ce), Silver (Ag ) And copper (Cu), and may be even more specifically nickel (Ni).
- the metal 1 is ruthenium (Ru), rhodium (Rh), molybdenum (Mo), osmium (0s), iridium (Ir), rhenium (Re), palladium (Pd), vanadium (V), tungsten ( W), cobalt (Co), iron (Fe), selenium (Se), nickel (Ni), bismuth (Bi), tin (Sn), chromium (Cr), titanium (Ti), cerium (Ce), silver (Ag) and copper (Cu) may be selected from the group 3 ⁇ 4, even more specifically nickel (NO.)
- the second metal is platinum (Pt), silver (Ag), palladium (Pd) and gold It may be selected from the group consisting of (Au), may be even more specifically platinum (Pt).
- One embodiment of the present application is a hollow core; At least one first shell comprising a first metal; And / or at least one second shell comprising a second metal.
- One embodiment of the present application is a hollow core; And it may provide a hollow metal nanoparticle comprising at least one shell comprising a crab 1 metal and a second metal.
- the shell may be a single layer or two or more layers. have.
- the crab 1 metal and the second metal may be present in a mixed form. At this time, they may be mixed uniformly or non-uniformly.
- an atomic percentage ratio of the first metal and the second metal may be 1: 5 to 10: 1.
- the first metal and the second metal in the shell may be present in a gradient state, the portion of the shell in contact with the hollow core 50% by volume or more, Or at least 70% by volume, and at least 50% by volume of the second metal, or at least 70% by volume, may be present on the surface portion of the shell that is in contact with the outside.
- the shell when the shell is a single layer, it may include only the first metal or the second metal.
- Particle diameters of the plurality of hollow metal nanoparticles formed in one embodiment of the present application may be within the range of 80% to 120% of the average particle diameter of the hollow metal nanoparticles.
- the particle diameter of the hollow metal nanoparticles may be in the range of 90% to 110% of the average particle diameter of the hollow metal nanoparticles. If it is out of the above range, since the size of the hollow metal nanoparticles becomes entirely non-uniform, it may be difficult to ensure the specific properties required by the vaporized metal nanoparticles. For example, when the hollow metal nanoparticles outside the range of 80% to 120% of the average particle diameter of the hollow metal nanoparticles are used as a catalyst, the activity of the catalyst may be somewhat insufficient.
- the hollow nanoparticles may include an anionic surfactant or cationic surfactant inside the hollow core.
- the carrier may use a carbon-based material or inorganic fine particles.
- Carbon based materials include carbon black, carbon nanotubes (CNT), graphite, graphene, activated carbon, porous carbon, mesoporous carbon, carbon fiber and carbon nano wire
- One selected from the group consisting of may be used, and the carbon blocks include denka black, ketjen blocks, or acetylene black.
- the inorganic fine particles may be selected from the group consisting of alumina, silica, titania, and zirconia.
- One embodiment of the present application comprises the steps of adding a first metal salt, a second metal salt and a surfactant to the solvent to form a solution; Hollow metal nanoparticles by adding a reducing agent to the solution Forming a; And and comprising the step of supporting the hollow metallic nanoparticles on a support,) '
- Forming the solution may include the surfactant forming a micelle, and the first metal salt and the second metal salt surround the outside of the micelle,
- Forming the hollow metal nanoparticles provides a method for producing hollow metal nanoparticles supported on a carrier that includes forming the micelle region in a hollow form.
- the supporting of the hollow metal nanoparticles may be adding a carrier after the forming of the hollow metal nanoparticles.
- One embodiment of the present application comprises the steps of adding a carrier, a crab 1 metal salt, a second metal salt and a surfactant to a solvent to form a composition; And adding a reducing agent to the composition to form hollow metal nanoparticles supported on a carrier.
- Forming the solution may include the surfactant forming a micelle, wherein the first metal salt and the crab dimetal salt surround the outside of the micelle,
- the vaporized metal nanoparticles provide a method for producing hollow metal nanoparticles supported on a carrier, wherein the micelle region is formed to be hollow.
- the forming of the composition may include mixing the carrier and the solution formed by adding the first metal salt, the metal salt 12 and the surfactant to a solvent.
- the forming of the composition may be performed by adding the carrier to a solution formed by adding the first metal salt, the second metal salt, and a surfactant to a solvent.
- the carrier may be a solution in which the carrier is dispersed in a solvent.
- the hollow metal nanoparticles may be prepared on a carrier.
- the carrier is added in the intermediate step of the manufacturing method, the adhesion between the carrier and the manufactured hollow metal nanoparticles is improved, so that the stability of the hollow metal nanoparticles is excellent.
- the dispersion degree of the hollow metal nanoparticles on the carrier is excellent. The better the dispersion degree, the more active points that can participate in reaction, so the reactivity is improved.
- the durability ' can be improved.
- the reduction potential since the reduction potential is not used, there is an advantage in that the reduction potential between the first metal and the second metal is not considered. Because of the use of charge (charge) between metal ions, there is an advantage that the method is simple compared to the conventional manufacturing method, the mass production is easy.
- Forming the solution may further add a stabilizer.
- the stabilizer may include one or two or more selected from the group consisting of disodium phosphate, dipotassium phosphate, disodium citrate and trisodium citrate.
- the first metal salt is not particularly limited as long as it can be ionized in a solution to provide metal ions in the first metal.
- the first metal salt may comprise the first metal.
- the first metal may be different from the second metal.
- the crab metal of the first metal salt may be selected from the group consisting of metals, metalloids, lanthanum group metals, and actinium group metals belonging to groups 3 to 15 of the periodic table.
- platinum Pt
- ruthenium Ru
- rhodium Rh
- molybdenum Mo
- osmium 0s
- iridium Ir
- rhenium Re
- palladium Pd
- vanadium V
- tungsten cobalt Co
- iron Fe
- selenium Se
- Ni nickel
- bismuth Bi
- tin Sn
- chromium Cr
- titanium Ti
- gold Au
- Ce cerium
- silver At least one selected from the group consisting of (Ag) and copper (Cu).
- ruthenium ruthenium
- Rh rhodium
- Mo molybdenum
- Mo molybdenum
- Ir iridium
- Rh rhenium
- Re palladium
- V vanadium
- tungsten cobalt
- Iron Iron
- Se selenium
- Ni nickel
- Bi bismuth
- tin Sn
- Cr chromium
- Ti titanium
- Ce cerium
- Ag silver
- Cu copper
- It may be selected from the group consisting of), and may be even more specifically nickel (Ni).
- the second metal salt is not particularly limited as long as it can be ionized in a solution to provide metal ions in the second metal.
- the second metal salt may comprise a second metal.
- the second metal may be different from the first metal. All.
- the second metal of the second metal salt may be selected from the group consisting of metals, metalloids, lanthanum group metals, and actinium group metals belonging to Groups 3 to 15 of the periodic table.
- platinum Pt
- ruthenium Ru
- rhodium Rh
- molybdenum Mo
- osmium (0s)
- iridium Ir
- rhenium Re
- palladium Pd
- Cobalt Co Iron (Fe), Selenium (Se), Nickel (Ni), Bismuth (Bi), Tin (Sn), Crum (Cr), Titanium (Ti), Gold (Au), Cerium (Ce)
- It may be one selected from the group consisting of silver (Ag) and copper (Cu) More specifically, it may be selected from the group consisting of platinum (Pt), palladium (Pd) and gold (Au), even more It may be particularly platinum (P
- the first metal and the second metal salt is a metal and each of the first I] nitroxide (nitrate, ⁇ 0 3 ") of the second metal in the embodiment of the present application, Cargo (Chloride, Cl "), beureum cargo (Bomide,
- the first metal and the second metal may form the hollow metal nanoparticles.
- the first metal and the second metal may form a shell portion of the hollow metal nanoparticles, and the shell portion may include a first shell and a second shell.
- the shell part may be formed of a first shell including a first metal and a second shell including a second metal.
- the first shell and the crab 2 shell may include metals different from each other.
- the shell part of the present specification may include one shell including the first metal and the second metal.
- the crab dimetal salt may form the form of a second shell, or may be combined with the first metal salt to form the form of the first shell together.
- the first metal salt may have a form surrounding the outer surface of the surfactant forming the micelle.
- the second metal salt may have a form surrounding the first metal salt.
- the first metal salt and the second metal salt may form a shell part including a first metal and a second metal, respectively, based on a reducing agent.
- the molar ratio of the first metal salt and the second metal salt may be 1: 5 to 10: 1, specifically 2: 1 to 5: 1. Moles of First Metal Salts Moles of Second Metal Salts If less than the number, it is difficult for the first metal to contain the hollow to form the first shell. In addition, when the number of moles of the first metal salt exceeds 10 times the number of moles of the second metal salt, it is difficult for the second metal salt to form the second shell surrounding the first shell.
- the solvent may be a solvent including water.
- the solvent dissolves a crab 1 metal salt and a second metal salt, and may be water or a mixture of water and an alcohol of (: ⁇ (: 6) , and specifically, may be water. Since the present application does not use an organic solvent as a solvent, there is no need for a post-treatment process for treating an organic solvent in a manufacturing process, and thus there is a cost saving effect and an environmental pollution prevention effect.
- the surfactant may form a micelle in the solution.
- the charge of the surfactant may be classified according to the kind of the charge on the outer surface of the micelle. That is, when the charge on the outer surface of the micelle is anionic, the surfactant forming the micelle may be an anionic surfactant. In addition, when the charge on the outer surface of the micelle is cationic, the surfactant forming the micelle may be a cationic surfactant.
- the surfactant may be an anionic surfactant.
- the surfactant is anionic surfactant
- the outer surface of the surfactant forming the micelle since the outer surface of the surfactant forming the micelle is anionic, it may be surrounded by a cationic first metal salt.
- the first metal salt may be surrounded by a second metal salt having an anion.
- the region in which the anionic surfactant forms the micelle is such that the first metal salt having the cation and the second metal salt having the anion do not exist, and form a hollow.
- the crab 2 metal salt is formed of a shell portion including the first metal and the second metal, the region forming the micelle may be a hollow core that does not contain a metal.
- the surfactant may be a cationic surfactant.
- the outer surface of the surfactant forming the micelle may be cationic and may be surrounded by a first metal salt having an anion. Furthermore, the first metal salt may be surrounded by a cation based metal salt. According to the exemplary embodiment of the present application, the region in which the cationic surfactant forms the micelle is such that the first metal salt bearing the anion and the second metal salt bearing the cation do not exist, thereby forming a hollow. Can be. That is, when the first metal salt and the second metal salt are formed by the shell portion including the crab 1 metal and the second metal by a reducing agent, the light and shade region forming the micelle may be a hollow core not containing metal.
- the forming of the solution may further include adding a non-neutral surfactant.
- the nonionic surfactant is specifically polyoxyethylene fatty alcohol ether, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene fatty acid ester, polyoxyethylene alkyl ether, polyoxyethylene castor Free derivative, sorbitan ester, glyceryl ester, glycerol monostearate, polyethylene glycol, polypropylene glycol, polypropylene glycol ester, cetyl alcohol, cetostearyl alcohol, stearyl alcohol, aryl alkyl polyether alcohol, poly Oxyethylene polyoxypropylene copolymer, poloxamer, poloxamine, methyl cellulose, hydroxy salose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxy propylcelrose, hydroxy propylmethyl salose, With hydroxypropylmethylsal Phthalate, noncrystalline saelreul Rose, polysaccharides, starch, starch derivatives, hydroxyethyl starch,
- the nonionic surfactant is adsorbed on the surface of the shell, and serves to uniformly disperse the enhanced metal nanoparticles formed in the solution.
- the hollow metal particles are prevented from agglomeration or coagulation, and the vaporized metal nanoparticles can be formed in a uniform size.
- the concentration of the surfactant in the solution may be 0.2 times or more and 5 times or less of the critical micelle concentration (CMC) for the solvent. For example, it may be 1 times.
- CMC critical micelle concentration
- the concentration of the surfactant in the solution may be 0.2 times or more and 5 times or less of the critical micelle concentration (CMC) for water.
- CMC critical micelle concentration
- the concentration of the surfactant is less than 0.2 times the critical micelle concentration, the surfactant may not form micelles and thus may not form hollow particles.
- the concentration of the surfactant exceeds 5 times the critical micelle concentration, a non-spherical rod or plate may be formed, it may not be able to form hollow metal nanoparticles.
- the size of the hollow metal nanoparticles may be adjusted by controlling the first and second metal salts surrounding the surfactant and / or micelle forming the micelle.
- the size of the hollow metal nanoparticles may be controlled by the chain length of the surfactant forming the micelle. Specifically, if the chain length of the surfactant is short, the size of the micelle is reduced, the hollow size is also reduced, and thus the size of the hollow metal nanoparticles can be reduced.
- the carbon number of the chain of the surfactant may be 15 or less. Specifically, the carbon number of the chain may be 8 or more and 15 or less. Alternatively, the carbon number of the chain may be 10 or more and 12 or less.
- the size of the hollow metal nanoparticles may be adjusted by adjusting the type of counter ions of the surfactant forming the micelle. Specifically, the larger the size of the counter ion of the surfactant, the weaker the bonding force with the head portion of the outer end of the surfactant may be a larger size of the hollow, thereby increasing the size of the hollow 3 ⁇ 4-speed nanoparticles.
- the surfactant is an anionic surfactant
- the surfactant may include NH 4 , K, Na or Li as a counter ion.
- the counter ion of the surfactant is NH 4 +
- the counter ion of the surfactant is K +
- the counter ion of the surfactant is Na +
- the counter ion of the surfactant is Li +
- the size of the hollow nanoparticles can be reduced. This can be confirmed by the following examples.
- the surfactant when the surfactant is a cationic surfactant, the surfactant may include ⁇ , Br “ or CI— as a counter ion.
- the size of the hollow nanoparticles may be reduced in the order of the counter ion of the surfactant is Cf.
- the size of the hollow metal nanoparticles may be adjusted by adjusting the size of the head of the outer end of the surfactant forming the micelle. Furthermore, in the case of increasing the size of the head of the surfactant formed on the outer surface of the micelle, the repulsive force between the head of the surfactant is increased, the hollow can be increased, thereby increasing the size of the hollow metal nanoparticles Can be.
- the size of the hollow metal nanoparticles may be determined by the combination of the above-described elements.
- the manufacturing method may be performed at room temperature. That is, each step of the manufacturing method may be performed at room temperature. Specifically, the temperature in the range of 4 ° C or more and 35 ° C or less, more specifically 15 ° C or more can be carried out at 28 or less.
- Forming the solution in one embodiment of the present application may be carried out at room temperature, specifically 4 ° C or more and 35 ° C or less, more specifically 15 ° C or more and 28 " C or less. If the organic solvent is used, there is a problem to be prepared at a high temperature of more than 100 ° C. Since the present application can be prepared at room temperature, the manufacturing method is simple, there is a process advantage and a large cost reduction effect.
- to form the solution is 5 minutes to 120 minutes Or, more specifically, for 10 minutes to 90 minutes, and even more specifically for 20 minutes to 60 minutes.
- the supporting of the hollow metal nanoparticles may be performed by preparing the hollow metal nanoparticles and then dropping the dispersion of the hollow metal nanoparticles into the dispersion of the carrier and then stirring the hollow metal nanoparticles. .
- the step of supporting the hollow metal nanoparticles on a carrier may be performed at room temperature. Specifically, 4 ° C or more in the range of 35 ° C or less, more specifically 15 ° C or more can be carried out at 28 ° C or less.
- Dispersing by adding the carrier in one embodiment of the present application may be carried out at room temperature, specifically in the range and temperature of 4 to 35 ° C. Since the present application can be manufactured at room temperature, the manufacturing method is simple, there is a process advantage, and the cost reduction effect is large.
- the step of dispersing may be performed by stirring for 5 minutes to 120 minutes, more specifically 10 minutes to 90 minutes, even more specifically 20 minutes to 60 minutes.
- the manufacturing method according to the embodiment of the present application has the advantage that the metal salts are evenly dispersed since the first metal salt and the second metal salt are dispersed in the carrier before the hollow metal nanoparticles are formed. Thus, when hollow metal nanoparticles are formed, less coarsening of the particles is generated. In addition, there is an advantage that the adhesion or bonding force between the hollow metal nanoparticles and the carrier is improved.
- a reducing agent to the solution; And adding a reducing agent to the solution to form hollow metal nanoparticles supported on the carrier at room temperature, specifically 4 ° C or more and 35 ° C or less, more specifically 15 ° C or more and 28 ° C or less. This can be done at Since the present application can be manufactured at room temperature, the manufacturing method is simple, there is a process advantage, and the cost reduction effect is large.
- the forming of the hollow metal nanoparticles may include reacting the solution and the reducing agent for a predetermined time, specifically, for 5 minutes to 120 minutes, more specifically for 10 minutes to 90 minutes, and more specifically for 20 minutes to 60 minutes. Can be done.
- the reducing agent is a standard reducing -0.23V or less, specifically, -4V or more -0.23V or less strong reducing agent, reducing the metal ions to reduce the reducing power to precipitate as metal particles It will not specifically limit, if it has.
- a reducing agent may be, for example, at least one selected from the group consisting of NaBH 4 , NH 2 NH 2) L1AIH 4 and LiBEt3H.
- a weak reducing agent it may be difficult to carry out continuous process such as a slow reaction rate and subsequent heating of the solution, which may cause a problem in mass production.
- a weak reducing agent ethylene glycol
- the method may further include removing a surfactant inside the hollow after forming the hollow metal nanoparticles.
- the removal method is not particularly limited and may be, for example, a method of washing with water.
- the surfactant may be an anionic surfactant or a cationic surfactant.
- a manufacturing method adding a carrier, a first metal salt, a second metal salt and a surfactant to a solvent to form a composition; And adding a reducing agent to the composition to form hollow metal nanoparticles supported on the carrier, and then performing a filtration process using a filter after centrifugation or washing after washing.
- adding a first metal salt, a second metal salt and a surfactant to a solvent to form a solution Adding a reducing agent to the solution to form hollow metal nanoparticles; And adding a carrier to the solution to support the hollow metal nanoparticles on the carrier, and then performing a filtration process using a filter after centrifugation or washing after washing.
- CMC critical micelle concentration for water
- Example 1 shows a model of the hollow metal nanoparticles including the surfactant among the hollow metal nanoparticles supported on the herbicide carrier according to Example 1, and shows a model of the hollow metal nanoparticles with the surfactant removed. 2 is shown.
- FIG. 7 and 8 show transmission electron microscope (TEM) images of hollow metal nanoparticles supported on a carrier prepared according to Example 1.
- TEM transmission electron microscope
- the particle diameters of the hollow metal nanoparticles were 9.3 nm, 15.3 nm, 17.1 nm, 19.5 nm, and 19.7 nm. there was.
- the particle diameters of the formed hollow metal nanoparticles were measured for 200 or more hollow metal nanoparticles using graphic software (MAC-View) based on FIG. 5, and the average particle diameter was 15 nm based on the obtained statistical distribution. Calculated as 5 ⁇ ⁇ .
- the dispersion degree of the hollow metal nanoparticles supported on the carrier prepared according to Example 1 was 35%
- CTAB cetyltrimethylammonium bromide cationic surfactant 0.02 ⁇ ol in 20ml of distilled water
- the solution was added, dissolved to form a solution, and stirred for 30 minutes.
- the molar ratio of K 2 PtCl 4 and NiCl 2 was 1: 1, wherein the calculated concentration of CTAB was approximately 1 times the critical micelle concentration (CMC) for water.
- FIG. 3 shows a model of the hollow metal nanoparticles including the surfactant among the hollow metal nanoparticles supported on the carrier prepared according to Example 2, and shows a model of the hollow metal nanoparticles with the surfactant removed. 4 is shown.
- Figure 11 shows a transmission electron microscope (TEM) image of the hollow metal nanoparticles supported on a carrier prepared according to Example 2.
- TEM transmission electron microscope
- the degree of dispersion of the hollow metal nanoparticles supported on the carrier prepared according to Example 2 was 28%.
- Ni (N0 3 ) 2 0.03 ⁇ ol as the first metal salt, K 2 PtCl 4 0.01 ⁇ as the second metal salt, Trisodium Citrate 0.12 ⁇ ol as the stabilizer, and ammonium lauryl sulfate as the negative surfactant (Ammonium Lauryl Sulfate: ALS) 0.02 kPa was added to 26 ml of distilled water, dissolved to form a solution, and stirred for 30 minutes.
- the ⁇ 0) 2 and the molar ratio of K 2 PtCl 4 is 3: 1 was, at this time, the concentration of the calculation 3 ⁇ 4 ALS is approximately twice the threshold misael concentration (CMC) in water.
- FIG. 9 shows a transmission electron microscope (TEM) image of hollow metal nanoparticles supported on a carrier prepared according to Example 3.
- TEM transmission electron microscope
- the degree of dispersion of the hollow metal nanoparticles supported on the carrier prepared according to Example 3 was 33%.
- Example 4 In order to measure the dispersion degree, Micromeritics' AutoChem ⁇ 2920 equipment was used, and adsorption gas was used for C0. Unlike Example 3, in which the hollow metal nanoparticles were prepared by adding a reducing agent after supporting the carbon black, in Example 4, the hollow metal nanoparticles were prepared by adding the reducing agent and then supported on the carbon blocks. Specifically, it is as follows.
- Ni (N0 3 ) 2 0.03 ⁇ ol as the first metal salt, K 2 PtCl 4 0.01 ⁇ ol as the second metal salt, 0.12 mmol of Tri sodium Citrate as the stabilizer, ammonium lauryl sulfide as the anionic surfactant Pate (Aonium Lauryl Sulfate: ALS) 0.02 ⁇ was added to 26 ml of distilled water, dissolved to form a solution, and stirred for 30 minutes.
- the molar ratio of ⁇ 0 3 ) 2 to K 2 PtCl 4 was 3: 1, and the concentration of ALS measured was approximately twice the critical micelle concentration (CMC) for water.
- a transmission electron microscope (TEM) image of the hollow metal nanoparticles supported on the carrier prepared according to Example 4 is shown in FIG. 10. At this time, the particle size was 20 nm.
- the dispersion degree of the hollow metal nanoparticles supported on the carrier prepared according to Example 4 was 24%.
- Figure 5 shows a cross-section of the hollow metal nanoparticles prepared according to Examples 1 to 4 supported on the carrier.
- Figure 6 shows that the general carrier-carried nanoparticles appear to be agglomerated on the carrier.
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Abstract
Description
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CN201380068898.XA CN104884194A (zh) | 2012-12-27 | 2013-12-27 | 负载在载体上的中空金属纳米粒子 |
JP2015546402A JP6350883B2 (ja) | 2012-12-27 | 2013-12-27 | 担体に担持された中空金属ナノ粒子を含む触媒 |
EP13866555.9A EP2913123B1 (en) | 2012-12-27 | 2013-12-27 | Hollow metal nano particles supported on carrier |
US14/649,846 US9517450B2 (en) | 2012-12-27 | 2013-12-27 | Hollow metal nano particles supported on carrier |
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US10814313B2 (en) * | 2015-10-27 | 2020-10-27 | Fondazione lstituto Italiano Di Tecnologia | Method for the preparation of metal oxide hollow nanoparticles |
JP2019104989A (ja) * | 2019-01-15 | 2019-06-27 | 株式会社新光化学工業所 | コアシェル型金属ナノ粒子及びコアシェル型金属ナノ粒子の製造方法 |
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KR20140085368A (ko) | 2014-07-07 |
JP6350883B2 (ja) | 2018-07-04 |
KR101557561B1 (ko) | 2015-10-07 |
CN104884194A (zh) | 2015-09-02 |
US20150314275A1 (en) | 2015-11-05 |
US9517450B2 (en) | 2016-12-13 |
EP2913123A1 (en) | 2015-09-02 |
EP2913123A4 (en) | 2016-07-20 |
EP2913123B1 (en) | 2023-02-01 |
JP2016507356A (ja) | 2016-03-10 |
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