WO2006082987A1 - 銀の粒子粉末およびその製造法 - Google Patents
銀の粒子粉末およびその製造法 Download PDFInfo
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- WO2006082987A1 WO2006082987A1 PCT/JP2006/302098 JP2006302098W WO2006082987A1 WO 2006082987 A1 WO2006082987 A1 WO 2006082987A1 JP 2006302098 W JP2006302098 W JP 2006302098W WO 2006082987 A1 WO2006082987 A1 WO 2006082987A1
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- Prior art keywords
- silver
- less
- particle powder
- dtem
- particles
- Prior art date
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- 239000004332 silver Substances 0.000 title claims abstract description 53
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 53
- 239000002245 particle Substances 0.000 title claims abstract description 51
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000000843 powder Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims description 28
- 239000013078 crystal Substances 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000009835 boiling Methods 0.000 claims abstract description 10
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 8
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000002296 dynamic light scattering Methods 0.000 claims description 3
- 241000404146 Minois Species 0.000 claims 1
- 239000002105 nanoparticle Substances 0.000 abstract description 23
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011814 protection agent Substances 0.000 abstract 2
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 11
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 5
- -1 silver ions Chemical class 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005576 amination reaction Methods 0.000 description 3
- 239000011362 coarse particle Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000004071 soot Substances 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003378 silver Chemical class 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 241000239290 Araneae Species 0.000 description 1
- 241000209761 Avena Species 0.000 description 1
- 235000007319 Avena orientalis Nutrition 0.000 description 1
- 244000062175 Fittonia argyroneura Species 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 101001096065 Homo sapiens Plexin domain-containing protein 1 Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
- 102100037891 Plexin domain-containing protein 1 Human genes 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 241001648319 Toronia toru Species 0.000 description 1
- 241000609666 Tuber aestivum Species 0.000 description 1
- 241000219995 Wisteria Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000002438 flame photometric detection Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003463 sulfur Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/288—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
Definitions
- the present invention relates to the ⁇ t method using silver particle powder 3 ⁇ 43 ⁇ 4.
- the silver grains of the present invention the end of which is the tempering and development of FPDs (Flat Panels, Isprays), and trenches, via holes and contact holes ⁇ ⁇ 3 ⁇ 4 ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ⁇ ' ⁇ Diagnosis It can also be applied to carriers that adsorb lees and biochemicals. Obedience
- the eye method and the liquid phase method are known.
- the eye method is vapor deposition in gas!
- Reference 1 there is a method for recognizing a spider in a 0.5 Torr key in a helium atmosphere.
- the micro method Disclosed is a method for obtaining silver colloid by reducing silver ions with ammine in the aqueous phase and moving the resulting precipitated silver phase (a high amount of m agent).
- ⁇ The silver particles obtained by the «1 grid method have a difficulty of 10 nm or less, and ⁇ 3 ⁇ 41 life in a cage is a child. However, this sickle requires special equipment. For this reason, there are s to merge ⁇ ffl silver nanoparticles into ⁇ 4.
- the liquid phase method is a male suitable for large-scale synthesis at 3 ⁇ 4 ⁇ 6 ⁇ , but ⁇ s nanoparticle is extremely key in the liquid and has the problem of rinsing a single nanoparticle powder. .
- cenoic acid as an agent in order to use ⁇ nanoparticles
- Low force S is normal, and this is a bottleneck in the application of.
- «» 2 is synthesized by synthesizing silver nanoparticles that are stable with a high ratio of more than 0.
- a high-priced glaze with a number average of tens of thousands is used.
- a high amount of ⁇ 3 ⁇ 4 agent is used.
- the present invention solves such a problem and has a fine arrangement! ! ⁇ Silver nanoparticle powder suitable for shattering and its ⁇ 13 ⁇ 4 night ⁇ (face and ⁇ ct is to be obtained. Also, 3 ⁇ 43 ⁇ 4 ⁇ aligned ⁇ F silver nano From the fact that the particles are separated into the particles, the force of the particles is obtained. Means to solve
- ⁇ ⁇ ⁇ measured by ⁇ ⁇ (DTE ⁇ O is less than 30 nm, aspect ratio is less than 1.5, X-ray crystal grain size (D x) Is less than 30 nm, single crystal ⁇ .
- this silver particle powder is made of a silver particle made by a shelf male and is a dynamic light diffuser.
- (D 5 0) is less than 1 OO nm and ⁇ (D 5 0) / (DTE ⁇ is less than 5.0.
- FIG. 1 is an electron microscope ( ⁇ ) of silver nanoparticle powder of the invention of a bowl.
- Fig. 2 shows the electronic fineness ( ⁇ ) of the silver nanoparticle powder of the present invention, which is different from the one shown in Fig. 1.
- the present inventor has repeatedly made it difficult to form silver nanoparticles and powders by the liquid phase method.
- the alcohol having a boiling point of 85 ° to 15 ° C., 85% to 15 ° 0. It was found that the silver nanoparticle powder in the form of soot can be obtained if it is returned to C (while the alcohol is flowing in liquid) and the amount is 100-400. did.
- This silver nano-particle powder is attached to the surface of tfJlH, which can be applied to the agent, so that it can be used to form fine circuit patterns.
- tfJlH which can be applied to the agent, so that it can be used to form fine circuit patterns.
- the silver powder paste of the present invention will be individually described below.
- Silver particles according to the present invention have a (DTEM) of 30 nm or less as measured by TEM G3 ⁇ 4l electron microscopic observation.
- TEM ⁇ measures the diameter of 300 independent particles that do not overlap from the image magnified 600,000 times, and finds the diameter of Pinghu. The aspect ratio and CV value are also obtained from the results.
- the aspect ratio (ratio of major axis / minor axis) of the IS body of the present invention is less than 1.5, preferably 1.2 or less, more preferably 1.1 or less.
- the photograph in Fig. 1 is almost bound, and its aspect ratio (Platinum is 1.05 or less. For this reason, it is in the process of 3 springs. To have an aspect ratio exceeding 1.5
- Tachiko's 3 ⁇ 4t worsens, and when they are drowned, pore force S is generated and disgust is high, and disconnection may occur depending on the age.
- CV value 1 0 0 Expressed by X standard difference ⁇ / number flat male.
- the CV value of the silver grains of the present invention is less than 40%, preferably less than 25%, more preferably less than 15%.
- Silver nanoparticle powders with a CV value of less than 40% are particularly suitable for spring applications. If the CV value is 40% or more, it is the same as Xieji; ⁇ Tachiko's formality is poor and there is a possibility of high-ranking or disconnection due to the occurrence of pores during drought.
- the silver nanoparticles of the present invention have a particle size of 30 nm or less.
- the crystal particle diameter of the silver particle powder can be obtained from the X-ray diffraction results using the Scherrer equation. For this reason, the crystal grain size specification # ⁇ is called X-ray crystal habit (D x), and the method for obtaining it is as follows.
- K Scherrer
- D crystal ⁇ && diameter
- ⁇ measured X-ray wavelength
- ⁇ ⁇ iffi width of peak obtained by X-ray diffraction
- ⁇ Bragg angle of diffraction line
- Single crystal! ⁇ Is expressed as the ratio of TEM3 ⁇ 4 / X ⁇ ⁇ (DT E ⁇ / (D x).
- the number of crystals covered in one particle is a leak. It can be said that the larger the temperature of a single crystal, the more the particles are made of polycrystals.
- the single crystal of the silver particles of the present invention [ ⁇ is 5.0 or less, preferably 3.0 or less, and more preferably 1.0 or less. For this reason, there are few crystal grain boundaries in a grain. The higher the boundary, the higher the loading resistance. However, the silver grains of the present invention are used for conjugation where the male is low because the single crystal is low.
- the flat light (D 5 0) by dynamic light scattering method is less than 60 nm, and ⁇
- 3 ⁇ 4 (D 5 0 ) / (DTEPvf) force 5.0 or less.
- the silver particles of the present invention can be easily fined into a shelf m and in a stable state.
- the dispersion state of! ⁇ Tachi can be calculated by the dynamic scattering method, and Hirao can also be calculated.
- the request is as follows. Particles with ⁇ in the range of about 1 nm to 5 in the liquid ⁇ ⁇ Circulation groove Brown »C ⁇ the force that changes the position and orientation from moment to moment and irradiates these particles with laser light
- the fluctuation shelf of 3 ⁇ 4g ⁇ ⁇ depending on Brown » By observing the time fluctuation of the scattered light bow, the brown wisteria boat of particles (the dispersion force can be obtained and the size of the ⁇ riko can be obtained.
- the average value of the measured female is measured, and the measured value is close to the average if ⁇ obtained by observation.
- the particles in the liquid are individual (the particles are old or wrinkled). In other words, each particle ⁇ 2 is carried at a distance in the cage so that it can move independently for each job.
- the average wrinkle by dynamic light scattering performed on the silver nanoparticle powder in watch is not so different from the average male by TEM observation, ie, measured at night according to the present invention.
- the flatness by dynamic light t3 ⁇ 4L method; ⁇ 1 ⁇ 2 is 60 nm or less, preferably 30 nm or less, more preferably 20 nm or less, which is not much different from that of TEM observation. ,. Therefore, the monodispersed state is SS, and according to the present invention, the silver nanoparticle powder is independent.
- the particles are simply ⁇ : in the cage, there is an age at which the vertical diameter and crease of the crane are produced by measurement.
- the night of the temple is necessary to be suitable for the 4th birthday of the instrument, and the amount of light is constrained by the error. Will occur.
- the dust of ⁇ comes out strongly and causes errors, so pay attention to the cleanliness of the previous key rule of the sample ⁇ . It is necessary to attach.
- Nano For particle measurement a laser source with a crane output of 10 O mW or more is suitable for earning a detached bow.
- the particle ⁇ is adsorbed, Russia also delta Me of such a suction layer, a two-: ⁇ also be 3 ⁇ 4 Personal Protection for First Aid or Rescue Personnel St is known larger that force s. Especially when ⁇ is 1 O nm; ⁇ becomes ⁇ .
- the silver particles of the present invention should be converted into salt in alcohol with a boiling point of 85-: 15 ° C under orchid U *, at 85-: 1550 ° C. You can ⁇ g.
- the alcohol as the ⁇ 1 base agent used in the present invention is not particularly limited as long as it has a boiling point of 85 ° C to 150 ° C. If the boiling point is less than 85 ° C, it is difficult to raise the reaction temperature to 85 ° C or higher unless it is nourish like a truffle.
- preferred alcohols include isobutanol, a-butanol, s-butanol or t-butanol, and f3 ⁇ 4 or 1 or 23 ⁇ 4 ⁇ .
- As the silver salt shelves silver salt that transforms into alcohol. U is preferred from a practical point of view.
- fatty acids and the like have a problem such as losing the moon and the isonitrileization ⁇ ) is a bridge, etc.
- the molecular weight is 10 0 to 4 0 0 Ami As you do.
- primary amines are preferred.
- Second-class amines or ⁇ ⁇ third-class amines themselves act as agents, so alcohol is already used as an IJ: ⁇ may become 2 ⁇ agents and ⁇ Sig ⁇ 's chest may be difficult .
- 3 ⁇ 43 ⁇ 43 ⁇ 4 is less than 85 ° C, the yield of good nanoparticle powder is low, and even if ittl is higher than 50 ° C, the yield is not improved. This is preferable because it becomes prominent. Therefore, 85 ⁇ : I 50 ⁇ C of silver ions by alcohol is applied to 3 ⁇ 4 °; 3 ⁇ 4T, but it is difficult to return the collected alcohol to the liquid phase using this device. It is good. Silver salt lakes should be 5 Ommo 1 km, and costs below this would be costly and not industrially dredging.
- the key is despised, re-tanol is added, and it is thorough with ultrasound ⁇ «.
- the silver nanoparticle powder of the present invention is obtained, and the silver nanoparticle powder of the present invention is reconstituted (for example, hexane, toluene, kerosene, decane, dodecane, tetradecane, etc.).
- Sffi Difficult or extreme [ ⁇ Raw is small and can be reversible.
- the obtained ⁇ « is then subjected to centrifugal separation for the purpose of removing coarse particles and then only the supernatant.
- the collected supernatant is used as a sample for various rules such as soot, X-rays, soot distribution, etc.
- the resulting nanoparticle powder is true. 3 ⁇ 4t dry (for example, 12 hours at 20 ° C) and measure the desiccant in a dish ⁇ m, HC ⁇ 3 ⁇ 43 ⁇ 4salted salt! Silver «
- Fig. 1 and Fig. 2 are ⁇ EM ⁇ (photos of ⁇ ⁇ - etc.) of the silver nanoparticle powder in the ⁇ forest example. As can be seen in these photographs, it can be seen that the silver nanoparticles of are wrinkled at predetermined intervals. 3 ⁇ 4 ⁇ It is a force type, but -i (OTE, aspect ratio, CV value is measured for particles that are slightly
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CN2006800039081A CN101111335B (zh) | 2005-02-02 | 2006-02-01 | 银粒子粉末、银粒子的分散液、及银粒子粉末的制造方法 |
EP06713241A EP1844884B1 (en) | 2005-02-02 | 2006-02-01 | Silver particle powder and process for producing the same |
KR1020077017518A KR101236260B1 (ko) | 2005-02-02 | 2006-02-01 | 은 입자 분말 및 이의 제조방법 |
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JP2005026805A JP4284283B2 (ja) | 2005-02-02 | 2005-02-02 | 銀の粒子粉末の製造法 |
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US (1) | US7776442B2 (ja) |
EP (1) | EP1844884B1 (ja) |
JP (1) | JP4284283B2 (ja) |
KR (1) | KR101236260B1 (ja) |
CN (1) | CN101111335B (ja) |
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Cited By (4)
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EP2067550A1 (en) * | 2006-09-26 | 2009-06-10 | DOWA Electronics Materials Co., Ltd. | Silver microparticle powder and method for production thereof |
US7981326B2 (en) * | 2007-01-09 | 2011-07-19 | Dowa Electronics Materials Co., Ltd. | Silver fine powder, process for producing the same, and ink |
US8003019B2 (en) * | 2007-01-09 | 2011-08-23 | Dowa Electronics Materials Co., Ltd. | Silver particle dispersion ink |
CN104801710B (zh) * | 2008-12-26 | 2017-05-03 | 同和电子科技有限公司 | 微小银粒子粉末及其制造方法以及使用该粉末的银糊料及其使用方法 |
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WO2007065154A2 (en) * | 2005-12-02 | 2007-06-07 | Nanodynamics Inc. | Method of manufacturing silver platelets |
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JP4986745B2 (ja) * | 2007-07-05 | 2012-07-25 | Dowaエレクトロニクス株式会社 | 銀ペースト |
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KR101239816B1 (ko) * | 2008-06-26 | 2013-03-06 | 디아이씨 가부시끼가이샤 | 은 함유 분체의 제조 방법, 은 함유 분체, 도전성 페이스트 및 플라스틱 기판 |
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US9034075B2 (en) * | 2012-04-30 | 2015-05-19 | Dow Global Technologies Llc | Methods of manufacturing high aspect ratio silver nanowires |
WO2014017443A1 (ja) * | 2012-07-24 | 2014-01-30 | Dic株式会社 | 金属ナノ粒子複合体、金属コロイド溶液及びそれらの製造方法 |
JP2013151753A (ja) * | 2013-03-04 | 2013-08-08 | Dowa Electronics Materials Co Ltd | 極性媒体との親和性に優れた銀微粉および銀インク |
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JP6912692B2 (ja) * | 2017-08-18 | 2021-08-04 | 御国色素株式会社 | 広分布な粒度分布を持つ銀ナノ粒子の製造方法及び銀ナノ粒子 |
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- 2006-02-01 WO PCT/JP2006/302098 patent/WO2006082987A1/ja active Application Filing
- 2006-02-01 US US11/883,344 patent/US7776442B2/en active Active
- 2006-02-01 KR KR1020077017518A patent/KR101236260B1/ko active IP Right Grant
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2067550A1 (en) * | 2006-09-26 | 2009-06-10 | DOWA Electronics Materials Co., Ltd. | Silver microparticle powder and method for production thereof |
EP2067550A4 (en) * | 2006-09-26 | 2012-07-25 | Dowa Electronics Materials Co | SILVER MICROTEIL POWDER AND MANUFACTURING METHOD THEREFOR |
US7981326B2 (en) * | 2007-01-09 | 2011-07-19 | Dowa Electronics Materials Co., Ltd. | Silver fine powder, process for producing the same, and ink |
US8003019B2 (en) * | 2007-01-09 | 2011-08-23 | Dowa Electronics Materials Co., Ltd. | Silver particle dispersion ink |
CN101584010B (zh) * | 2007-01-09 | 2012-08-29 | 同和电子科技有限公司 | 银粒子分散液及其制造方法 |
CN104801710B (zh) * | 2008-12-26 | 2017-05-03 | 同和电子科技有限公司 | 微小银粒子粉末及其制造方法以及使用该粉末的银糊料及其使用方法 |
US9721694B2 (en) | 2008-12-26 | 2017-08-01 | Dowa Electronics Materials Co., Ltd. | Fine silver particle powder, method for manufacturing the same, silver paste using the powder and method of use of the paste |
Also Published As
Publication number | Publication date |
---|---|
EP1844884A4 (en) | 2009-08-12 |
TW200633799A (en) | 2006-10-01 |
CN101111335A (zh) | 2008-01-23 |
EP1844884A1 (en) | 2007-10-17 |
US20080152912A1 (en) | 2008-06-26 |
KR20070099631A (ko) | 2007-10-09 |
KR101236260B1 (ko) | 2013-02-22 |
US7776442B2 (en) | 2010-08-17 |
JP2006213955A (ja) | 2006-08-17 |
CN101111335B (zh) | 2010-05-19 |
EP1844884B1 (en) | 2012-12-26 |
JP4284283B2 (ja) | 2009-06-24 |
TWI272983B (en) | 2007-02-11 |
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