JP5688895B2 - 微小銀粒子粉末と該粉末を使用した銀ペースト - Google Patents
微小銀粒子粉末と該粉末を使用した銀ペースト Download PDFInfo
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- JP5688895B2 JP5688895B2 JP2009285691A JP2009285691A JP5688895B2 JP 5688895 B2 JP5688895 B2 JP 5688895B2 JP 2009285691 A JP2009285691 A JP 2009285691A JP 2009285691 A JP2009285691 A JP 2009285691A JP 5688895 B2 JP5688895 B2 JP 5688895B2
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- silver
- particles
- reaction
- copper
- powder
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- IJFXRHURBJZNAO-UHFFFAOYSA-N meta--hydroxybenzoic acid Natural products OC(=O)C1=CC=CC(O)=C1 IJFXRHURBJZNAO-UHFFFAOYSA-N 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- PSZYNBSKGUBXEH-UHFFFAOYSA-M naphthalene-1-sulfonate Chemical class C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-M 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical group O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 1
- 150000004690 nonahydrates Chemical class 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001467 poly(styrenesulfonates) Chemical class 0.000 description 1
- 229920000058 polyacrylate Chemical class 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920001281 polyalkylene Polymers 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000011970 polystyrene sulfonate Chemical class 0.000 description 1
- 229960002796 polystyrene sulfonate Drugs 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 1
- 229940071536 silver acetate Drugs 0.000 description 1
- 229910001958 silver carbonate Inorganic materials 0.000 description 1
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
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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
- 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
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/62—Metallic pigments or fillers
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/006—Metal
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
- C22C5/08—Alloys based on silver with copper as the next major constituent
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- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
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Description
乾燥状態の銀粒子粉末2質量部をシクロヘキサン96質量部とオレイン酸2質量部との混合溶液に添加し、超音波によって分散させた。分散溶液を支持膜付きCuマイクログリッドに滴下し、乾燥させることでTEM試料とした。作成したマイクログリッドを透過型電子顕微鏡(日本電子株式会社製JEM−100CXMark−II型)を使用し、100kVの加速電圧で、明視野で粒子を観察した像を、倍率30,000倍及び174,000倍で撮影した。
上記の測定方法での1000個以上での測定値から平均値、標準偏差を算出し、標準偏差を平均値で割った値を変動係数として算出した。
銀成分が残留していると分析誤差が発生する可能性があるため、銀成分を除くため、以下の前処理を施した。300mlコニカルビーカーに銀粒子粉末10gを入れ、次に硝酸溶液15mlを添加して銀粒子粉末を溶解させる。溶解した溶液を250℃に設定したホットプレート上で加熱し、蒸発乾固にならない程度まで濃縮する。濃縮された溶液を放冷した後、純水を添加する。溶液中に白濁や浮遊物がないことを確認する。もし溶液中に白濁や浮遊物がある場合には、なくなるまで硝酸添加、加熱濃縮、放冷の工程を繰り返す。白濁や浮遊物がない溶液に塩酸を添加し、塩化銀を生成する。その後濾過で固液分離して塩化銀と濾液を分別し、該濾液をICP−MS(アジレントテクノロジー株式会社製AGILENT7500i)を用いて銅量の分析を行った。
銀粒子粉末0.2gを25℃、45cc/minのN2雰囲気下で20分間前処理を行った後、ユアサアイオニクス製の4S−U2若しくはこの製品の同等品を用いて行った。
特開2007−263860号に記載されている測定法を用いて行った。本測定法を概略的に説明すると、所定のホルダーに測定対象の粉体を充填して粉体層を形成し、当該粉体層へ、0.14N/m2以上、0.18N/m2以下の圧力を加えた後、粉体層の高さを測定し、当該粉体層の高さの測定値と、充填された粉体の重量とから測定対象の粉体の密度を求めるタップ密度測定方法である。
作製した銀粒子粉末6gとターピネオール4gを混合した。その後、ディスパーを用いて1400rpmで90秒間処理し、三本ロールで10パスさせて銀粒子含有分散液を作製した。
作製した銀粒子含有分散液を、スライドガラス上にアプリケーターを用いて塗布した。その後、乾燥機(ヤマト科学株式会社製)を用いて150℃で30分間焼成した。また、200℃で30分間焼成したサンプルも作製した。焼成した膜の厚さ1μm当りの体積抵抗値を抵抗率計(三菱化学アナリテック株式会社製ロレスタGP)を用いて測定し、膜の厚さは表面粗度計(株式会社東京精密製サーフコム1500D)を用いて測定をすることで膜の体積抵抗値を算出した。
得られた銀粒子粉末を溶媒および分散剤へ添加して分散液を作成し、溶媒に対する粒子の分散性を確認した。具体的な手法としては銀粒子粉末1.0g、ブチルカルビトールアセテート(和光純薬工業株式会社製)10.0g、分散剤としてDisperBYK2020(ビックケミー・ジャパン社製)0.1gをそれぞれ秤量し、それらを試験管中で混合し、超音波分散機で10分間分散することにより分散液を作成した。得られた液中における粒子の分散状態を目視により確認することで、粉末の溶媒に対する分散性を確認した。
表面を被覆する有機物は、粒子もしくは分散液、あるいはペーストを被覆する有機物の分解温度以下の温度、例えば150℃程度の温度で30分程度加熱して発生するガスを捕集し、ガスクロマトグラフ/マススペクトルグラフィ(GC/MS)で解析することにより知ることができる。
5Lビーカーを使用し(実施例1〜7および比較例1〜7について同じ)、反応槽の中心に撹拌羽を備えた攪拌棒を設置する。反応槽には温度をモニターするための温度計を設置し、また溶液に下部より窒素を供給できるようにノズルを配設した。以上の構成を備えた装置を反応槽Aとする。
銀に対する銅の添加量を各々変化させた以外は、実施例1を繰り返した。得られた粒子の物性等を表1にあわせて示す。
銅の種類を変化させ、かつ添加量を変化させた。反応装置ならびに反応フローについては同じにしてある。得られた粒子の物性等を表1にあわせて示した。
容積が200Lのステンレス製反応槽(実施例8〜13および比較例8について同じ)、を準備し、反応槽A(5L反応槽)同様に攪拌棒、温度計、窒素ノズルを設置することで、反応槽Bを構成した。
銀に対する銅の添加量を各々変化させた以外は、実施例8を繰り返した。得られた粒子の物性等を表1にあわせて示す。
樹脂としてフェノール樹脂レヂトップPL−4348(群栄化学工業株式会社製/固形分77.5wt%)3.9gをテルピネオール14.0gに溶解させ、次に高分子系顔料分散剤アジスパーPA111(味の素ファインテクノ株式会社製)1.3gをその溶液に溶解させる。この中に実施例8と同様にして作成した、ヘキサン酸(炭素数:6)で被覆された一次粒子の平均粒径が20nmの銀粒子94.3gを加え、手攪拌で10分間混合させ導電性ペーストを得た。
樹脂としてアクリル樹脂BR−102(三菱レイヨン株式会社製)を5.0g用意し、分散媒であるテルピネオール(和光純薬工業株式会社製)44.0gに溶解し、この中にこの中に実施例8と同様にして作成した、ヘキサン酸(炭素数:6)で被覆された一次粒子の平均粒径が20nmの銀粒子95.0gを加え、実施例14を繰り返したところ、比抵抗が7.7μΩ・cmである良好な導電性を呈した薄膜が得られた。
銅を添加しなかったこと以外は、実施例1を繰り返した。得られた粒子の物性等を表1にあわせて示す。
還元剤のヒドラジン水和物量を銀に対して9.6当量となる量に変更した以外は、比較例1を繰り返した。なお、還元反応開始後直ちに反応スラリーの色変化が終了し、反応が完結していることが確認された。
還元反応完了後に、硝酸銅三水和物水溶液を銀に対して3000ppm相当量添加し、5分間撹拌した以外は、比較例1を繰り返した。
銀に対する銅の添加量を各々変化させた以外は、実施例1を繰り返した。得られた粒子の物性等を表1にあわせて示す。
添加物質を硝酸ニッケル六水和物水溶液(比較例6、和光純薬工業株式会社製)もしくは硝酸鉄(III)九水和物水溶液(比較例7、和光純薬工業株式会社製)とし、その添加量を実施例4と同じ銀に対して100ppmとした以外は、実施例4と同じ反応操作とした。得られた粒子の物性等を表1にあわせて示す。
銅を添加しなかったこと以外は、実施例8を繰り返した。得られた粒子の物性等を表1にあわせて示す。
Claims (4)
- 粒子表面が炭素数5〜8の有機物からなる保護剤により被覆され、TEM写真から算出される平均粒子径(DTEM)が5〜100nmであって、BETが15〜40m 2 /gであり、1〜200ppmの銅を含有する銀粒子粉末。
- BET法により算出される比表面積は15〜40m2/gの範囲にあるとともに、さらにはTEM写真から算出される粒子径の変動係数(CV値(%)=100×標準偏差/平均粒子径)が30%未満である。請求項1に記載の銀粉末。
- 請求項1または2に記載の銀粉末を極性溶媒に分散させて得られる銀粒子分散液。
- 請求項3に記載の分散液に樹脂を添加して得られる銀粒子が含有されたペースト。
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