WO2023214559A1 - Procédé de fabrication de microparticules, et solution colloïdale - Google Patents
Procédé de fabrication de microparticules, et solution colloïdale Download PDFInfo
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- WO2023214559A1 WO2023214559A1 PCT/JP2023/017012 JP2023017012W WO2023214559A1 WO 2023214559 A1 WO2023214559 A1 WO 2023214559A1 JP 2023017012 W JP2023017012 W JP 2023017012W WO 2023214559 A1 WO2023214559 A1 WO 2023214559A1
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- fine particles
- powder material
- metal atoms
- metal
- metal atom
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 42
- 239000011859 microparticle Substances 0.000 title abstract 7
- 239000000463 material Substances 0.000 claims abstract description 133
- 229910052751 metal Inorganic materials 0.000 claims abstract description 99
- 239000002184 metal Substances 0.000 claims abstract description 99
- 239000002904 solvent Substances 0.000 claims abstract description 34
- 239000000956 alloy Substances 0.000 claims abstract description 18
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 14
- 230000001678 irradiating effect Effects 0.000 claims abstract description 9
- 239000010419 fine particle Substances 0.000 claims description 179
- 239000000843 powder Substances 0.000 claims description 119
- 239000000243 solution Substances 0.000 claims description 26
- 238000002844 melting Methods 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 16
- 239000006104 solid solution Substances 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 22
- 239000002245 particle Substances 0.000 description 18
- 239000000203 mixture Substances 0.000 description 12
- 229910052759 nickel Inorganic materials 0.000 description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 229910021645 metal ion Inorganic materials 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 239000013078 crystal Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 6
- 239000002082 metal nanoparticle Substances 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 4
- 230000005496 eutectics Effects 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910052755 nonmetal Chemical group 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000013076 target substance Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- FFQALBCXGPYQGT-UHFFFAOYSA-N 2,4-difluoro-5-(trifluoromethyl)aniline Chemical compound NC1=CC(C(F)(F)F)=C(F)C=C1F FFQALBCXGPYQGT-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- WEUCVIBPSSMHJG-UHFFFAOYSA-N calcium titanate Chemical compound [O-2].[O-2].[O-2].[Ca+2].[Ti+4] WEUCVIBPSSMHJG-UHFFFAOYSA-N 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 for example Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
-
- 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
- B22F1/052—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
-
- 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
-
- 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
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
Definitions
- the present invention relates to a method for producing fine particles and a colloidal solution.
- Patent Document 1 Conventionally, as a method for producing fine particles using a laser, a method for producing fine particles as disclosed in Patent Document 1, for example, has been proposed.
- Patent Document 1 discloses a method of generating metal nanoparticles by irradiating a basic solvent in which one or more types of metal ions are dissolved with a femtosecond pulse laser.
- Patent Document 1 a basic solvent in which metal ions are dissolved is irradiated with a femtosecond pulse laser, and the metal ions are reduced by radicals (for example, hydrogen radicals) generated by decomposing water molecules in the basic solvent.
- a method of producing metal nanoparticles is disclosed. According to this production method, during the reduction reaction of metal ions, in addition to the metal nanoparticles that are the target substance, for example, chloride ions that have been bonded to the metal ions are oxidized, and impurities other than the target substance are generated. there is a possibility. For this reason, there is a possibility that the generated impurities may have an effect such as adhesion to the metal nanoparticles, and there is a concern that the quality of the metal nanoparticles may be deteriorated.
- radicals for example, hydrogen radicals
- the present invention was devised in view of the above-mentioned problems, and its purpose is to provide a method for producing fine particles and a colloidal solution that can suppress deterioration in the quality of fine particles. It is in.
- the fine particles are produced using a femtosecond pulsed laser, the method comprising: irradiating a powder material in a solvent with the femtosecond pulsed laser to produce particles containing metal atoms; the powder material has a larger median diameter than the fine particles and contains metal atoms.
- the powder material contains a first powder material containing a first metal atom and a second metal atom different from the first metal atom. and a second powder material containing the fine particles, and the fine particles are an alloy containing the first metal atoms and the second metal atoms.
- the melting point of the second powder material is higher than the melting point of the first powder material.
- the fine particles are a solid solution in which the first metal atoms and the second metal atoms are combined.
- a colloidal solution in a fifth invention is characterized by comprising the fine particles produced by the method for producing fine particles according to any one of the first to third inventions, and a solvent in which the fine particles are dispersed. do.
- the powder material includes a first powder material containing a first metal atom and a second powder material containing a second metal atom different from the first metal atom.
- the fine particles are an alloy containing first metal atoms and second metal atoms. Therefore, the ratio between the first powder material and the second powder material can be adjusted, making it easier to control the composition ratio of each metal atom contained in the fine particles. This makes it possible to suppress variations in the composition ratio of each metal atom contained in the fine particles.
- the melting point of the second powder material is higher than the melting point of the first powder material. That is, fine particles are produced that have the characteristics of the first powder material and a melting point higher than that of the first powder material. Therefore, compared to the case where fine particles are manufactured without using the second powder material, the temperature range in which the fine particles are stable can be expanded. This makes it possible to improve the stability of the generated fine particles.
- the fine particles are a solid solution that is a combination of first metal atoms and second metal atoms. Therefore, compared to fine particles that are not solid solutions, local state changes and chemical changes in the fine particles are less likely to occur. This makes it possible to further improve the stability of the generated fine particles.
- the colloidal solution includes a solvent in which fine particles are dispersed. For this reason, aggregation of fine particles can be more easily suppressed than when fine particles are stored without using a solvent. This makes it possible to provide fine particles with maintained quality.
- FIG. 1 is a schematic perspective view showing an example of a manufacturing apparatus used in the method for manufacturing fine particles in this embodiment.
- the fine particles in this embodiment are used not only in electronic devices such as power generation elements, but also in fields such as medicine and food.
- the fine particles include not only metal fine particles but also fine particles containing metal atoms and non-metal atoms.
- Fine particles can be used, for example, in the energy field, such as power generation elements, and in the electronic device field, such as conductive parts.
- fine particles can be used, for example, in the medical field as pharmaceuticals or cosmetics, the material field as part of composite materials, and the food field.
- fine particles having additional functions can be produced, which is expected to be used in a variety of applications.
- the fine particles include a plurality of particles having a particle diameter of, for example, 1 nm or more and 100 nm or less.
- the fine particles may include, for example, particles having a median diameter (median diameter: D50) of 1 nm or more and 10 nm or less, and may also include, for example, particles having an average particle diameter of 1 nm or more and 10 nm or less.
- the median diameter or average particle diameter can be measured, for example, using a particle size distribution meter.
- a particle size distribution measuring device using a dynamic light scattering method for example, Zetasizer Ultra manufactured by Malvern Panalytical, etc.
- fine particles refers not only to a group of particles generated by a single metal, but also to a group of particles generated by, for example, multiple types of metal particles. Fine particles may refer to particles produced by an alloy, for example.
- the colloidal solution in this embodiment is used in the same field as fine particles.
- a colloidal solution refers to a state in which two or more types of substances including, for example, fine particles are mixed.
- the colloidal solution includes, for example, a solvent 6 in which fine particles are dispersed.
- the colloidal solution includes a solvent 6 in which fine particles are dispersed.
- aggregation of the particles can be more easily suppressed than when the particles are stored without using the solvent 6. This makes it possible to provide fine particles with maintained quality.
- fine particles examples include known metal atoms such as nickel, platinum, gold, and titanium.
- the fine particles may include, for example, pure metals, alloys containing no non-metals, or metal oxides. Note that when producing a colloidal solution in which fine particles of an alloy containing no pure metal or non-metal are dispersed, by using alcohol as the solvent 6, factors that promote oxidation of the fine particles can be reduced. This makes it possible to provide fine particles with better quality.
- the fine particles exhibit, for example, a perovskite structure.
- the fine particles include, for example, barium titanate (BaTiO 3 ), strontium titanate (SrTiO 3 ), calcium titanate (CaTiO 3 ), lead titanate (PbTiO 3 ), tin titanate (SnTiO 3 ), and cadmium titanate (CdTiO 3 ) . ), and strontium zirconate (SrZrO 3 ).
- the fine particles are generated using, for example, a first powder material and a second powder material.
- the first powder material contains a first metal atom (first metal atom)
- the second powder material contains a second metal atom (second metal atom).
- the fine particles are, for example, an alloy containing first metal atoms and second metal atoms.
- the fine particles contain, for example, a second powder material (second powder material) having a melting point higher than that of the first powder material (first powder material). That is, fine particles are produced that have the characteristics of the first powder material and have a higher melting point than the first powder material.
- the temperature range in which the fine particles are stable can be expanded. This makes it possible to improve the stability of the fine particles.
- the fine particles may be an alloy containing two different metal atoms, or an alloy containing three or more different metal atoms.
- the fine particles are, for example, a solid solution of a first metal atom and a second metal atom.
- the fine particles are, for example, a solid solution of a first metal atom and a second metal atom.
- the solid solution fine particles may contain three or more types of metal atoms.
- a combination of metal atoms whose mixing enthalpy is 0 or less may be selected.
- the fine particles are, for example, a eutectic that is a combination of a first metal atom and a second metal atom.
- the stability of the fine particles can be improved compared to fine particles that are not eutectic.
- the fine particles include, for example, two or more types of materials exhibiting the same crystal structure.
- the crystal structure tends to be the same throughout the fine particles of the alloy. This makes it possible to improve the stability of the generated fine particles.
- FIG. 1 is a schematic perspective view showing an example of a manufacturing apparatus 100 in this embodiment.
- the manufacturing apparatus 100 includes, for example, a laser device 1, a lens 2, a container 3, and a solution 4, as shown in FIG.
- the manufacturing apparatus 100 may include a plurality of containers 3 and solutions 4 for one laser device 1, for example.
- the laser device 1 emits a pulsed laser having a time width of, for example, about 10 ⁇ 15 seconds.
- a femtosecond pulse laser such as Astrella manufactured by COHERENT, which exhibits the following characteristics, can be used.
- Laser wavelength 800nm ⁇ 20nm
- Pulse width 100fs Energy: 5-9mJ
- Repetition frequency 100Hz (output 0.5-0.9W)
- the laser device 1 may be, for example, Spitfire Pro manufactured by Spectra Physics, and can be arbitrarily selected depending on the application. Note that the laser emitted from the laser device 1 has an energy of about several mJ, and it is difficult to efficiently generate fine particles with energy of about several ⁇ J, which is used for example in laser processing.
- the lens 2 condenses the laser emitted from the laser device 1.
- the light intensity can be increased in a specific area.
- the laser can be focused inside the solution 4 rather than at the interface of the solution 4.
- a known lens such as a condenser lens is used.
- the position of the lens 2 at which the laser is focused inside the solution 4 may be adjusted by adjusting the shape of the lens 2, the distance from the solution 4, etc., for example.
- the lens 2 may be a variable focus lens, for example, and the position at which the laser is focused inside the solution 4 may be adjusted while the position of the lens 2 is fixed.
- Container 3 contains solution 4.
- a transparent material is used as the container 3, for example a quartz cuvette.
- a material having a lower absorption rate at a wavelength around 800 nm than around 400 nm is used as the container 3. In this case, when irradiating the laser through the container 3, it is possible to suppress a decrease in the production efficiency of fine particles.
- Solution 4 includes powder material 5 and solvent 6.
- the solvent 6 suspends the powder material 5.
- the fine particles in this embodiment are generated by irradiating the powder material 5 suspended in the solvent 6 with a laser emitted from the laser device 1 .
- the powder material 5 has, for example, a larger median diameter than the fine particles.
- the powder material 5 includes a plurality of particles having a finite particle diameter of, for example, 500 ⁇ m or less.
- the powder material 5 includes particles having a median diameter of, for example, 50 nm or more and 100 ⁇ m or less.
- the powder material 5 Since the powder material 5 is directly reflected in the composition of the fine particles to be generated, it can be arbitrarily set depending on the type of fine particles to be generated. For example, when gold is used as the powder material 5, the generated fine particles contain gold. In this case, compared to, for example, a method for producing fine particles in which chloroauric (III) acid hydrate is reduced, the generation of impurities that may adhere to the fine particles can be suppressed. This makes it possible to suppress deterioration in quality of the generated fine particles.
- the powder material 5 includes, for example, one or more types of materials. For example, when the powder material 5 contains two or more kinds of materials, fine particles of an alloy containing each material can be produced.
- the powder material 5 contains known metal atoms such as nickel, platinum, gold, and titanium. As long as the powder material 5 contains metal atoms, it may contain, for example, any one of a pure metal, an alloy containing no non-metal, and a metal oxide.
- the powder material 5 includes, for example, a first powder material and a second powder material.
- the first powder material contains first metal atoms.
- the second powder material contains second metal atoms different from the first metal atoms.
- the first powder material has, for example, a different composition than the second powder material.
- the second powder material has a melting point higher than that of the first powder material, for example. That is, fine particles are produced that have the characteristics of the first powder material and a melting point higher than that of the first powder material.
- the temperature range in which the fine particles are stable can be expanded. This makes it possible to improve the stability of the generated fine particles.
- the powder material 5 may include, for example, two or more types of materials exhibiting the same crystal structure.
- the crystal structure of the entire fine particles of the produced alloy exhibits the same tendency. This makes it possible to improve the stability of the fine particles.
- the crystal structures of iron, sodium, and potassium exhibit a body-centered cubic lattice. Therefore, by including a material containing at least two of iron, sodium, and potassium as the powder material 5, the crystal structure of the entire fine particles of the produced alloy tends to be the same.
- the crystal structures of nickel, aluminum, and calcium exhibit face-centered cubic lattices. Therefore, by including a material containing at least two types of nickel, aluminum, and calcium as the powder material 5, the crystal structure tends to be the same throughout the produced fine particles of the alloy.
- the method for producing fine particles includes, for example, an irradiation step.
- the method for producing fine particles may include at least one of a conditioning step and a stirring step.
- a femtosecond pulse laser is focused and irradiated onto the powder material 5 suspended in the solvent 6.
- a femtosecond pulse laser is emitted from the laser device 1 to irradiate the powder material 5 suspended in the solvent 6.
- the pulse width of the femtosecond pulsed laser is shorter than the time for the heat of the laser to be transmitted inside the powder material 5, the heat does not diffuse to areas other than the irradiation target. In this case, laser energy is less likely to be consumed in reactions other than the generation of fine particles. This makes it possible to improve the production efficiency of fine particles.
- the irradiation step is a process in which the femtosecond pulse laser is focused and the powder material 5 is irradiated, and for example, the solvent 6 may also be irradiated.
- radicals are generated in the solvent 6, but the method for producing fine particles in this embodiment does not require a process of chemically reacting the radicals with the powder material 5. In this case, the amount of fine particles produced is less affected by the reaction rate between radicals and the powder material 5 and the amount of radicals produced.
- the powder material 5 having a larger median diameter than the fine particles is irradiated with a femtosecond pulse laser. Therefore, compared to a method for producing fine particles that utilizes the reduction of metal ions, it is possible to suppress the generation of impurities that are generated due to the reduction reaction of metal ions and that may affect the fine particles. This makes it possible to produce fine particles whose quality is less likely to deteriorate.
- the powder material 5 including a first powder material containing a first metal atom and a second powder material containing a first metal atom may be irradiated with a femtosecond pulse laser. good.
- fine particles of the alloy containing the first metal atoms and the second metal atoms are generated.
- the ratio of the first powder material to the second powder material can be adjusted, making it easier to control the composition ratio of each metal atom contained in the fine particles. This makes it possible to produce fine particles in which variation in the composition ratio of each metal atom contained is suppressed.
- the powder material 5 including the first powder material and the second powder material having a higher melting point than the first powder material may be irradiated with a femtosecond pulse laser. That is, fine particles are produced that have the characteristics of the first powder material and a melting point higher than that of the first powder material.
- the temperature range in which the fine particles are stable can be expanded. This makes it possible to produce highly stable fine particles.
- the powder material 5 containing the first metal atoms and the second metal atoms is irradiated with a femtosecond pulse laser to generate fine particles of a solid solution in which the first metal atoms and the second metal atoms are combined.
- a femtosecond pulse laser to generate fine particles of a solid solution in which the first metal atoms and the second metal atoms are combined.
- the powder material 5 containing the first metal atoms and the second metal atoms is irradiated with a femtosecond pulse laser to form fine particles of a eutectic in which the first metal atoms and the second metal atoms are combined. May be generated. In this case, it is possible to produce fine particles that are more stable than fine particles that are not eutectic.
- the powder material 5 contains metal atoms.
- the laser may be absorbed by the surface of the metal atoms contained in the powder material 5 before reaching the focal point, and the laser irradiated to the powder material 5 may cause fine particles. It is assumed that there may be cases where the amount of energy is not consumed efficiently for generation. That is, by adjusting the wavelength of the irradiated laser, it is possible to improve the generation efficiency of fine particles.
- the oscillation wavelength of the laser emitted from the laser device 1 is adjusted to a wavelength that avoids a wavelength range that is absorbed by metal atoms contained in the powder material 5.
- the laser energy is less likely to be absorbed by the metal atoms contained in the powder material 5, and is more likely to be efficiently consumed to generate fine particles. This makes it possible to improve the production efficiency of fine particles.
- the oscillation wavelength of the laser emitted from the laser device 1 may be adjusted using, for example, a wavelength conversion function that the laser device 1 has.
- the adjustment step may be performed during the irradiation step, at least before or after the irradiation step, or may be performed in multiple steps.
- the powder material 5 is irradiated with a laser. At this time, it is necessary to focus the laser on the powder material 5, but it is assumed that the powder material 5 will settle in the solvent 6 over time and become difficult to be irradiated with the laser. That is, by stirring the solvent 6 so that the powder material 5 passes through the focus of the laser, it is possible to improve the production efficiency of fine particles.
- the solvent 6 in which the powder material 5 is suspended is stirred.
- the solvent 6 may be stirred while performing the irradiation step. In this case, it becomes easier to uniformly irradiate the powder material 5 with the laser. This makes it possible to improve the production efficiency of fine particles.
- the solvent 6 may be stirred using a known stirrer such as a stirrer. The stirring step may be performed at least either before or after the irradiation step.
- the stirring step helps keep the powder material 5 in the solvent 6 in a dispersed state. That is, it prevents the powder material 5 in the solvent 6 from settling over time. Therefore, the powder material 5 can be easily irradiated with the laser. Thereby, it is possible to improve the generation efficiency of fine particles.
- the stirring step facilitates keeping the first powder material containing the first metal atoms and the second powder material containing the second metal atoms in the solvent 6 uniformly dispersed, for example. Therefore, the composition ratio of each metal contained in the fine particles of the solid solution containing the first metal atoms and the second metal atoms tends to be uniform. This makes it possible to produce fine particles with higher uniformity.
- the irradiation step includes irradiating the powder material 5 in the solvent 6 with a femtosecond pulse laser to generate fine particles containing metal atoms, and the powder material 5 is larger than the fine particles. It has a median diameter. Therefore, compared to a method for producing fine particles that involves reduction of metal ions, the generation of impurities that may affect the fine particles can be suppressed. This makes it possible to suppress deterioration in quality of the generated fine particles.
- the powder material 5 includes, for example, a first powder material containing a first metal atom and a second powder material containing a second metal atom different from the first metal atom.
- the fine particles are an alloy containing first metal atoms and second metal atoms. Therefore, the ratio between the first powder material and the second powder material can be adjusted, making it easier to control the composition ratio of each metal atom contained in the fine particles. This makes it possible to suppress variations in the composition ratio of each metal atom contained in the fine particles.
- the melting point of the second powder material is higher than the melting point of the first powder material. That is, fine particles are produced that have the characteristics of the first powder material and a melting point higher than that of the first powder material. Therefore, compared to the case where fine particles are manufactured without using the second powder material, the temperature range in which the fine particles are stable can be expanded. This makes it possible to improve the stability of the generated fine particles.
- the fine particles are a solid solution that is a combination of first metal atoms and second metal atoms. Therefore, compared to fine particles that are not solid solutions, local state changes and chemical changes in the fine particles are less likely to occur. This makes it possible to further improve the stability of the generated fine particles.
- the colloidal solution includes a solvent 6 in which fine particles are dispersed. Therefore, compared to the case where the fine particles are stored without using the solvent 6, aggregation of the fine particles can be more easily suppressed. This makes it possible to provide fine particles with maintained quality.
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Abstract
L'invention fournit un procédé de fabrication de microparticules permettant d'améliorer la pureté de microparticules, et une solution colloïdale. Plus précisément, l'invention concerne un procédé qui est destiné à produire des microparticules à l'aide d'un laser à impulsion femtoseconde, et qui est caractéristique en ce qu'il comporte une étape d'irradiation au cours de laquelle le laser à impulsion femtoseconde irradie un matériau de poudre (5) dans un solvant (6), et des microparticules comprenant des atomes métalliques sont générées. En outre, le matériau de poudre (5) présente un diamètre à mi-hauteur supérieur à celui des microparticules, et comprend des atomes métalliques. Par exemple, le matériau de poudre (5) inclut un premier matériau de poudre comprenant un premier atome métallique, et un second matériau de poudre comprenant un second atome métallique différent du premier atome métallique, et les microparticules consistent en un alliage comprenant le premier et le second atome métallique.
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JP2022-075928 | 2022-05-02 | ||
JP2022075928A JP7185969B1 (ja) | 2022-05-02 | 2022-05-02 | 微粒子の製造方法 |
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WO2023214559A1 true WO2023214559A1 (fr) | 2023-11-09 |
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JP (1) | JP7185969B1 (fr) |
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JP2008006513A (ja) * | 2006-06-27 | 2008-01-17 | Kyoto Univ | ナノサイズワイヤーの製造方法およびナノサイズワイヤー |
JP2012046778A (ja) * | 2010-08-25 | 2012-03-08 | Toyota Central R&D Labs Inc | 化合物ナノ粒子の製造方法 |
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US8802234B2 (en) | 2011-01-03 | 2014-08-12 | Imra America, Inc. | Composite nanoparticles and methods for making the same |
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JP2008006513A (ja) * | 2006-06-27 | 2008-01-17 | Kyoto Univ | ナノサイズワイヤーの製造方法およびナノサイズワイヤー |
JP2012046778A (ja) * | 2010-08-25 | 2012-03-08 | Toyota Central R&D Labs Inc | 化合物ナノ粒子の製造方法 |
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TW202408685A (zh) | 2024-03-01 |
JP2023165185A (ja) | 2023-11-15 |
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