JP2006213955A - 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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- 239000002245 particle Substances 0.000 title claims abstract description 105
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 69
- 239000004332 silver Substances 0.000 title claims abstract description 69
- 239000000843 powder Substances 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003223 protective agent Substances 0.000 claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 238000009835 boiling Methods 0.000 claims abstract description 10
- 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 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims description 27
- -1 amino compound Chemical class 0.000 claims description 12
- 238000002296 dynamic light scattering Methods 0.000 claims description 8
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 11
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- 238000006243 chemical reaction Methods 0.000 description 13
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 12
- 239000002612 dispersion medium Substances 0.000 description 11
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 238000005259 measurement Methods 0.000 description 10
- 239000002244 precipitate Substances 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000003638 chemical reducing agent Substances 0.000 description 8
- 239000002270 dispersing agent Substances 0.000 description 8
- 125000002924 primary amino group Chemical class [H]N([H])* 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 238000010304 firing Methods 0.000 description 6
- 229910001961 silver nitrate Inorganic materials 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 5
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- 150000001875 compounds Chemical class 0.000 description 4
- 239000002082 metal nanoparticle Substances 0.000 description 4
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- 238000006722 reduction reaction Methods 0.000 description 4
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- 230000005653 Brownian motion process Effects 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000005537 brownian motion Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000011362 coarse particle Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
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- 150000004665 fatty acids Chemical class 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
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- 150000003573 thiols Chemical class 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
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- 239000011261 inert gas Substances 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
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- 150000003464 sulfur compounds Chemical class 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001704 evaporation Methods 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
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000001556 precipitation Methods 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
- 238000000790 scattering method Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 150000003463 sulfur Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- 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
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- 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
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- 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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System 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
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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- 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
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Abstract
【解決手段】 TEM観察により測定される平均粒径(DTEM ) が30nm以下,アスペクト比が1.5未満,X線結晶粒子径(Dx )が30nm以下,単結晶化度〔(DTEM )/(Dx )〕が5.0以下,およびCV値〔=100×標準偏差(σ)/個数平均粒径(DTEM 〕が40%未満の銀のナノ粒子粉末であって,粒子表面に分子量100〜400の有機保護剤が被着している銀のナノ粒子粉末である。このナノ粒子粉末は,沸点が85〜150℃のアルコール中で銀塩を有機保護剤の共存下で85〜150℃の温度で還元処理することによって得られる。
【選択図】 なし
Description
本発明に従う銀粒子は,TEM(透過電子顕微鏡)観察により測定される平均粒径(DTEM ) は30nm以下である。TEM観察では60万倍に拡大した画像から重なっていない独立した粒子300個の径を測定して平均値を求める。アスペクト比とCV値も同様の観察結果から求める。
本発明の銀粒子粉末のアスペクト比(長径/短径の比)は1.5未満,好ましくは1.2以下,さらに好ましくは1.1以下である。図1の写真のものはほぼ球形であり,そのアスペクト比(平均)は1.05以下である。このため配線形成用途に好適である。アスペクト比が1.5を超える場合には、その粒子の分散液を基板に塗布して乾燥したときに粒子の充填性が悪くなり,焼成時にポアが発生して抵抗が高くなり,場合によっては断線が起きることがある。
CV値は粒径のバラツキを示す指標であり,CV値が小さいほど粒径が揃っていることを示す。CV値=100×標準偏差σ/個数平均粒径で表される。本発明の銀粒子粉末のCV値は40%未満,好ましくは25%未満、さらに好ましくは15%未満である。CV値が40%未満の銀ナノ粒子粉末は配線用途に好適である。CV値が40%以上では前記と同様に粒子の充填性が悪く焼成時のポアの発生による高抵抗化や断線が起きる可能性がある。
本発明の銀ナノ粒子は結晶粒子径が30nm以下である。銀粒子粉末の結晶粒子径はX線回折結果から Scherrer の式を用いて求めることができる。このため、結晶粒子径は本明細書ではX線結晶粒径(Dx)と呼ぶ。その求め方は、次のとおりである。
Scherrer の式は、次の一般式で表現される。
D=K・λ/β COSθ
式中、K:Scherrer定数、D:結晶粒子径、λ:測定X線波長、β:X線回折で得られたピークの半価幅、θ:回折線のブラッグ角をそれぞれ表す。
Kは0.94の値を採用し,X線の管球はCuを用いると,前式は下式のように書き換えられる。
D=0.94×1.5405/β COSθ
単結晶化度はTEM粒径/X線結晶粒径の比(DTEM ) /(Dx )で表される。単結晶化度は1個の粒子中に存在する結晶の数に概略相当する。単結晶化度が大きいほど多結晶からなる粒子であると言える。本発明の銀粒子の単結晶化度は5.0以下,好ましくは、3.0以下,さらに好ましくは1.0以下である。このため,粒子中の結晶粒界が少ない。結晶粒界が多くなるほど電気抵抗が高くなるが,本発明の銀粒子粉末は単結晶化度が低いので抵抗が低く,導電部材に用いる場合に好適である。
銀粒子粉末と有機溶媒を混合して得られた本発明の分散液は,動的光散乱法による平均粒径(D50)が60nm以下であり,分散度=(D50)/(DTEM ) が5.0以下である。
本発明の銀粒子粉末は,沸点が85〜150℃のアルコール中で銀塩を有機保護剤の共存下で85〜150℃の温度で還元処理することによって製造することができる。
溶媒兼還元剤としてのイソブタノール(和光純薬株式会社製の特級)200mLに、オレイルアミン(和光純薬株式会社製)132.74mLと硝酸銀結晶13.727gを添加し、マグネットスターラーにより攪拌して室温で溶解した。この溶液を還流器のついた容器に移してオイルバスに載せ、容器内に不活性ガスとして窒素ガスを400mL/minの流量で吹込みながら、該溶液をマグネットスターラーにより200rpmの回転速度で撹拌しつつ加熱し、100℃の温度で5時間の還流を行って、反応を終了した。100℃に至るまでの昇温速度は2℃/min である。
1.反応後のスラリーを日立工機(株)製の遠心分離器CF7D2を用いて5000rpmで60分固液分離し、上澄みは廃棄する。
2.沈殿物にエタノールを加え、超音波分散機にかけて分散させる。
3.前記の1→2の工程を3回繰り返す。
4.前記の1を実施し,上澄みを廃棄して沈殿物を得る。
イ.TEM観察および動的光散乱による粒度分布の測定には,該沈殿物にケロシンに添加して分散液とし,その分散液を、遠心分離機にかけ、粗粒子・凝集粒子を沈殿後、沈殿物を取り除いた分散液を得た。その分散液について評価を行った。
ロ.X線回折並びに結晶粒子径の測定には、イで作成した粗粒子・凝集体を除去した分散液を濃縮し、ペースト状にしたものを無反射板に塗布してX線回折装置で測定した。
ハ.Ag純度と収率を求める場合には,該沈殿物を真空乾燥機で200℃で12時間乾燥し,その乾燥品の重量を測定して求めた。より具体的には,その乾燥品を重量法(硝酸溶解後、HCl添加し塩化銀沈殿物を作成し,その重量で純度を測定する方法)でAg純度を測定した。収率に関しては、1バッチ分の(反応後に実際に得られた乾燥品/添加した硝酸銀から計算により得られる収量)×100(%)により求めた。
溶媒兼還元剤としてプロパノールを使用し、反応温度を80℃とした以外は実施例1を繰り返した。その結果,銀の収率は1.1%と極めて低く,その沈殿物のX線回折では銀に由来するピークしか観察されなかったが,Dx=15.9nmであった。X線回折測定以外の測定は、サンプル量が少ないために実施できなかった。
溶媒兼還元剤としてエタノールを使用し、反応温度を75℃にした以外は実施例1を繰り返した。その結果は、銀の収率は0.9%と極めて低く,その沈殿物のX線回折では銀に由来するピークしか観察されなかったが,Dx=25.4nmであった。X線回折測定以外の測定は、サンプル量が少ないために実施できなかった。
Claims (6)
- TEM観察により測定される平均粒径(DTEM ) が30nm以下,アスペクト比が1.5未満,X線結晶粒子径(Dx )が30nm以下,単結晶化度〔(DTEM ) /(Dx )〕が5.0以下,およびCV値〔=100×標準偏差(σ)/個数平均粒径(DTEM 〕が40%未満の銀の粒子粉末であって,粒子表面に分子量100〜400の有機保護剤が被着している銀の粒子粉末。
- 有機保護剤は,アミノ化合物である請求項1に記載の銀の粒子粉末。
- 請求項1に記載の銀の粒子粉末を有機溶媒に分散させてなる銀粒子の分散液であって,動的光散乱法による平均粒径(D50)が100nm以下および分散度=(D50)/(DTEM ) が5.0以下である銀粒子の分散液。
- 沸点が85〜150℃のアルコール中で銀塩を有機保護剤の共存下で85〜150℃の温度で還元処理することからなる,有機保護剤が被着した銀の粒子粉末の製造法。
- 有機保護剤は,分子量100〜400のアミノ化合物である請求項4に記載の銀の粒子粉末の製造法。
- アルコールは,イソブタノール、n―ブタノール、s―ブタノールまたはt−ブタノールのいずれか1種もしくは2種以上の混合物である請求項4または5に記載の銀の粒子粉末の製造法。
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US20080152912A1 (en) | 2008-06-26 |
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Free format text: JAPANESE INTERMEDIATE CODE: R250 |
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R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
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