JP2003055701A - Silver powder for conductive paste and its manufacturing method and conductive paste using the silver powder - Google Patents
Silver powder for conductive paste and its manufacturing method and conductive paste using the silver powderInfo
- Publication number
- JP2003055701A JP2003055701A JP2001244169A JP2001244169A JP2003055701A JP 2003055701 A JP2003055701 A JP 2003055701A JP 2001244169 A JP2001244169 A JP 2001244169A JP 2001244169 A JP2001244169 A JP 2001244169A JP 2003055701 A JP2003055701 A JP 2003055701A
- Authority
- JP
- Japan
- Prior art keywords
- silver powder
- conductor paste
- flake
- container
- cured coating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 238000004519 manufacturing process Methods 0.000 title claims abstract 7
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 239000002245 particle Substances 0.000 claims abstract description 15
- 239000004020 conductor Substances 0.000 claims description 55
- 239000011248 coating agent Substances 0.000 claims description 27
- 238000000576 coating method Methods 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 10
- 229930195729 fatty acid Natural products 0.000 claims description 10
- 239000000194 fatty acid Substances 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 150000004665 fatty acids Chemical class 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 238000007561 laser diffraction method Methods 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims 1
- 238000004438 BET method Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 16
- 238000000034 method Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000000523 sample Substances 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- -1 polyoxyethylene Polymers 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 4
- 239000005642 Oleic acid Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 4
- 235000021313 oleic acid Nutrition 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 1
- 235000021360 Myristic acid Nutrition 0.000 description 1
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 239000011805 ball Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000155 melt Substances 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
- 239000002736 nonionic surfactant Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、電子部品の実装分
野において使用される導体ぺ一スト用フィラーとしての
銀粉に関するものである。本発明は、更に詳しくは、印
刷回路導体、導電接着剤、プリント配線基板のビア穴埋
め、電磁波シールドおよび電極用ぺ一ストに使用するフ
レーク状銀粉に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to silver powder as a filler for conductor paste used in the field of mounting electronic parts. More specifically, the present invention relates to a flake silver powder used for printed circuit conductors, conductive adhesives, filling via holes in printed wiring boards, electromagnetic wave shields, and electrode pastes.
【０００２】[0002]
【従来の技術】従来より、フィラー、樹脂および溶媒を
混合してなる導体ペーストが電子部品の実装分野におい
て使用されている。このような導体ペースト用のフィラ
ーとしては、フレーク状銀粉が配合されている。フレー
ク状銀粉は、比表面積が大きくしかも見掛密度が低いの
で、フレーク状銀粉を配合した導体ペーストは優れた導
電性を有している。2. Description of the Related Art Conventionally, a conductor paste obtained by mixing a filler, a resin and a solvent has been used in the field of mounting electronic parts. Flake-shaped silver powder is blended as a filler for such a conductor paste. Since the flake silver powder has a large specific surface area and a low apparent density, the conductor paste containing the flake silver powder has excellent conductivity.
【０００３】従来、フレーク状銀粉は、一般的に、アト
マイズ法、電解法または化学還元法などの方法で得られ
た粒状銀粉をボールミル内でフレーク化することによっ
て得られていた。通常、ボールミルは円筒状または球状
の内面を有する容器を備えており、この容器内には粒状
銀粉やボール、更に必要に応じて溶媒や処理剤が仕込ま
れる。そしてこのボールミルを作動すると、容器が回転
して粒状銀粉がフレーク化される。このように、容器が
回転して、その内容物をフレーク化するボールミルの場
合、容器を高速で回転してその内容物に１Ｇ以上の遠心
力が掛かるとその内容物は容器の内面に押し付けられた
まま動かなくなるので、銀粉のフレーク化は実質的に進
まなくなる。従って、このようなボールミルの場合、容
器の内容物に加わる遠心力が１Ｇ未満になるように容器
を回転する必要がある。Conventionally, flake-shaped silver powder has generally been obtained by flake-forming granular silver powder obtained by a method such as an atomizing method, an electrolytic method or a chemical reduction method in a ball mill. Usually, a ball mill is provided with a container having a cylindrical or spherical inner surface, and granular silver powder, balls, and if necessary, a solvent and a treating agent are charged in the container. Then, when this ball mill is operated, the container is rotated and the granular silver powder is made into flakes. In this way, in the case of a ball mill in which the container is rotated and the contents are flaked, when the container is rotated at a high speed and a centrifugal force of 1 G or more is applied to the contents, the contents are pressed against the inner surface of the container. Since it does not move as it is, flake formation of silver powder does not substantially progress. Therefore, in the case of such a ball mill, it is necessary to rotate the container so that the centrifugal force applied to the contents of the container is less than 1G.
【０００４】しかしながら、近年、より薄くて細かいフ
レーク状銀粉、並びにこれを含む導電性に優れた低コス
トの導体ペーストが要求されており、そのために粒状銀
粉のフレーク化技術の改良が求められている。However, in recent years, there has been a demand for thinner and finer flake-like silver powder and a low-cost conductor paste containing the same and having excellent conductivity, and for this reason, improvement of the flake formation technique of granular silver powder is required. .
【０００５】[0005]
【発明が解決しようとする課題】そこで本発明は、薄く
て細かい形状を有するフレーク状銀粉を提供するととも
に、このフレーク状銀粉を配合した導電性に優れた導体
ペーストを提供することを課題とする。SUMMARY OF THE INVENTION It is therefore an object of the present invention to provide a flake-shaped silver powder having a thin and fine shape and a conductive paste containing the flake-shaped silver powder and having excellent conductivity. .
【０００６】[0006]
【課題を解決するための手段】本発明者らは上記の課題
を解決すべく種々検討を重ねた結果、フレーク状の粒形
を有し、レーザー回折法５０％粒径が３〜８μｍであ
り、見掛密度が０．４〜１．１／ｃｍ3 であり、ＢＥＴ
法比表面積値が１．５〜４．０ｍ2 ／ｇであることを特
徴とする導体ペースト用銀粉を調製することによって解
決できることを見出した。以下に、本発明を更に詳細に
説明する。As a result of various investigations to solve the above problems, the present inventors have found that they have a flake-like particle shape and a 50% particle diameter by laser diffraction method of 3 to 8 μm. , The apparent density is 0.4 to 1.1 / cm 3 , and the BET
It was found that this can be solved by preparing a silver powder for a conductor paste, which has a specific surface area value of 1.5 to 4.0 m 2 / g. Hereinafter, the present invention will be described in more detail.
【０００７】〔フレーク状銀粉〕本発明のフレーク状銀
粉は、ボールミルを使用して製造されるが、特に本発明
では攪拌ボールミルが使用される。この攪拌ボールミル
は、円筒状の内面を有する容器と、この容器内に設けら
れた攪拌翼とを備えている。この攪拌ボールミルの容器
内には、粒状銀粉、ボール、溶媒および処理剤が仕込ま
れるようになっている。従来のボールミルと異なり、容
器が回転することなく、容器内に設けられた攪拌翼が回
転して粒状銀粉をフレーク化するようになっている。上
記の攪拌ボールミルを使用すると、攪拌翼によって容器
の内容物を勢いよく攪拌することができる。従って、従
来のボールミルでは不可能であった１Ｇ以上の遠心力を
容器の内容物に加わえることができる。[Flake Silver Powder] The flake silver powder of the present invention is produced by using a ball mill, and in particular, a stirring ball mill is used in the present invention. This stirring ball mill includes a container having a cylindrical inner surface, and a stirring blade provided inside the container. Granular silver powder, balls, a solvent, and a treating agent are charged in the container of this stirring ball mill. Unlike the conventional ball mill, the stirring blade provided inside the container rotates to turn the granular silver powder into flakes without rotating the container. When the above stirring ball mill is used, the contents of the container can be vigorously stirred by the stirring blade. Therefore, it is possible to apply a centrifugal force of 1 G or more, which is impossible with the conventional ball mill, to the contents of the container.
【０００８】本発明によると、攪拌ボールミルの容器の
内容物（即ち、粒状銀粉、ボール、溶媒および処理剤）
に対して加えられる遠心力の大きさは、特に限定されな
いが、好ましくは、容器の内容物に対して５Ｇ〜３００
Ｇの遠心力が加わるように攪拌翼は回転される。これに
よって、粒状銀粉のフレーク化を促進することができ
る。According to the present invention, the contents of the vessel of the stirred ball mill (ie, granular silver powder, balls, solvent and treating agent).
The magnitude of the centrifugal force applied to is not particularly limited, but is preferably 5 G to 300 with respect to the content of the container.
The stirring blade is rotated so that the G centrifugal force is applied. This can promote flake formation of the granular silver powder.
【０００９】本発明によると、容器に仕込まれる粒状銀
粉は、特に限定されず、従来周知のアトマイズ法、電解
法または化学還元法などの方法で得られた粒状銀粉が使
用される。According to the present invention, the granular silver powder charged in the container is not particularly limited, and the granular silver powder obtained by a conventionally known method such as atomizing method, electrolytic method or chemical reduction method is used.
【００１０】また、本発明においては、従来周知のボー
ルを使用して粒状銀粉のフレーク化を行うことができる
が、好ましくは、ボールとして、１ｍｍ以下、特に０．
１〜１ｍｍの直径を有するチタンまたはジルコニア製の
ものが使用される。特に、本発明においては、プラズマ
回転電極法によって製造されたチタン製のボールが好適
に使用される。このようなプラズマ回転電極法によって
製造された直径が１ｍｍ以下のチタン製ボールは、均一
な球形を有しており、本発明のフレーク状銀粉を得るた
めのボールとして特に好ましい。Further, in the present invention, it is possible to make flakes of granular silver powder by using conventionally well-known balls, but it is preferable that the balls have a diameter of 1 mm or less, particularly 0.
Those made of titanium or zirconia having a diameter of 1-1 mm are used. In particular, in the present invention, titanium balls produced by the plasma rotating electrode method are preferably used. Titanium balls having a diameter of 1 mm or less produced by such a plasma rotary electrode method have a uniform spherical shape and are particularly preferable as the balls for obtaining the flake silver powder of the present invention.
【００１１】また、本発明において、攪拌ボールミルの
容器に仕込まれる溶媒も、特に限定されない。このよう
な溶媒としては、例えば水（特にイオン交換水）、メタ
ノール、エタノール、プロパノール、ブタノール、ペン
タノール、ジメチルケトン、ジエチルケトン、ジエチル
エーテル、ジメチルエーテル、ジフェニルエーテル、ト
ルエンおよびキシレンが挙げられる。これらの溶媒は、
単独で、または適宜組み合わせて使用される。Further, in the present invention, the solvent charged in the container of the stirring ball mill is not particularly limited. Examples of such a solvent include water (particularly ion-exchanged water), methanol, ethanol, propanol, butanol, pentanol, dimethyl ketone, diethyl ketone, diethyl ether, dimethyl ether, diphenyl ether, toluene and xylene. These solvents are
They are used alone or in appropriate combination.
【００１２】さらに、本発明において、容器に仕込まれ
る処理剤も、特に限定されない。このような処理剤とし
ては、例えば界面活性剤および／または脂肪酸が挙げら
れる。Further, in the present invention, the treating agent charged in the container is not particularly limited. Examples of such a treating agent include a surfactant and / or a fatty acid.
【００１３】ここで、上記の界面活性剤としては、特に
非イオン界面活性剤が挙げられ、さらに具体的には、例
えばポリオキシエチレンアルキルエーテル、ポリオキシ
エチレンアルキルフェニルエーテル、ポリオキシエチレ
ン脂肪酸エステル、ポリオキシエチレンソルビタン脂肪
酸エステル、およびソルビタン脂肪酸エステルが挙げら
れる。これらの界面活性剤は、単独でまたは２種類以上
が組み合わせて使用される。Here, as the above-mentioned surfactants, nonionic surfactants are particularly mentioned, and more specifically, for example, polyoxyethylene alkyl ether, polyoxyethylene alkylphenyl ether, polyoxyethylene fatty acid ester, Examples include polyoxyethylene sorbitan fatty acid ester, and sorbitan fatty acid ester. These surfactants are used alone or in combination of two or more kinds.
【００１４】また、上記の脂肪酸としては、例えばオレ
イン酸、ステアリン酸およびミリスチン酸が挙げられ
る。これらの脂肪酸は単独でまたは２種類以上が組み合
わせて使用される。Examples of the above-mentioned fatty acids include oleic acid, stearic acid and myristic acid. These fatty acids may be used alone or in combination of two or more.
【００１５】界面活性剤および／または脂肪酸が処理剤
として使用される場合、この界面活性剤および／または
脂肪酸は、合計で、得られるフレーク状銀粉の表面積１
ｍ2 あたり０．００５ｇ〜０．１ｇとなるように、容器
内に仕込まれる。なお、処理剤として界面活性剤が単独
使用される場合、容器に入れる溶媒としては水が特に好
ましい、また、処理剤として脂肪酸が単独使用される場
合には、容器に入れる溶媒としては、エタノールが特に
好ましい。When a surfactant and / or a fatty acid is used as the treating agent, this surfactant and / or fatty acid is added in total to a surface area of 1 of the obtained flake silver powder.
It is charged in a container so that it is 0.005 g to 0.1 g per m 2 . When the surfactant is used alone as the treating agent, water is particularly preferable as the solvent to be placed in the container.When the fatty acid is used alone as the treating agent, ethanol is used as the solvent to be placed in the container. Particularly preferred.
【００１６】本発明によると、得られたフレーク状銀粉
は、レーザー回折法５０％粒径が３〜８μｍ（更には３
〜６μｍ、最適には４〜５μｍ）であり、見掛密度が
０．４〜１．１／ｃｍ3 であり、しかもＢＥＴ法比表面
積値が１．５〜４．０ｍ2 ／ｇになっている。According to the present invention, the obtained flaky silver powder has a 50% particle size by laser diffraction of 3 to 8 μm (further 3
～6Myuemu, ideal for a is 4 to 5 [mu] m), a apparent density 0.4 to 1.1 / cm 3, yet BET specific surface area value becomes 1.5~4.0m 2 / g There is.
【００１７】〔導体ペースト〕このようにして得られた
フレーク状銀粉は、例えば、樹脂と混合されて導体ペー
ストとして利用される。本発明によるフレーク状銀粉
は、従来法によって得られたフレーク状銀粉よりも、粒
径が小さく、見掛密度が小さく、且つ比表面積が大きい
ので、導体ペーストへの銀粉の配合量を減らしても、優
れた導電率を有する導体ペーストの調製が可能である。[Conductor Paste] The flaky silver powder thus obtained is mixed with a resin and used as a conductor paste. Since the flake silver powder according to the present invention has a smaller particle size, a smaller apparent density, and a larger specific surface area than the flake silver powder obtained by the conventional method, even if the compounding amount of the silver powder in the conductor paste is reduced. It is possible to prepare a conductor paste having excellent conductivity.
【００１８】なお、本発明の導体ペーストを得るための
樹脂としては、エポキシ樹脂やアクリル樹脂など、従来
周知の樹脂が任意に使用される。なお、導体ペーストに
は、さらに、溶剤を添加してもよい。As the resin for obtaining the conductor paste of the present invention, any conventionally known resin such as epoxy resin or acrylic resin may be used. A solvent may be further added to the conductor paste.
【００１９】本発明の導体ペースト中の銀粉の配合量
は、特に限定されないが、本発明によると、導体ペース
ト中の固形分中の銀粉含有量〔（銀粉の質量）÷（銀粉
の質量＋樹脂の質量）×１００〕は、好ましくは５５〜
８０質量％、更に好ましくは６０〜８０質量％、最適に
は６５〜８０質量％になっている。この点において本発
明のフレーク状銀粉および導体ペーストは、従来のもの
と顕著に相違する。即ち、従来の導体ペーストでは、十
分な導電性を確保するためには銀粉が８５質量％以上配
合されている必要があり、銀粉の含有量が８０質量％以
下でれば電気抵抗率が極めて大きくなったが、本発明の
導体ペーストでは、銀粉が８５質量％以上配合されてい
る場合に優れた導電性を有していることは当然である
が、銀粉が８０質量％以下であっても優れた導電性を有
している点で、従来の導体ペーストと顕著に相違する。The content of silver powder in the conductor paste of the present invention is not particularly limited, but according to the present invention, the content of silver powder in the solid content of the conductor paste [(mass of silver powder) / (mass of silver powder + resin) Mass) × 100] is preferably 55 to
It is 80% by mass, more preferably 60 to 80% by mass, and most preferably 65 to 80% by mass. In this respect, the flake silver powder and the conductor paste of the present invention are significantly different from the conventional ones. That is, in the conventional conductor paste, silver powder needs to be blended in an amount of 85 mass% or more in order to secure sufficient conductivity, and if the content of the silver powder is 80 mass% or less, the electrical resistivity is extremely high. However, it is natural that the conductor paste of the present invention has excellent conductivity when the silver powder is blended in an amount of 85 mass% or more, but is excellent even when the silver powder is 80 mass% or less. In addition, the conductive paste is remarkably different from the conventional conductive paste.
【００２０】具体的に示すと、本発明の導体ペースト中
に、８０〜８５質量％のフレーク状銀粉が配合されてい
る場合、導体ペーストの硬化塗膜は、１０×１０ -7 Ω
・ｍ以下の電気抵抗率を有している。また、本発明の導
体ペースト中に、７０〜８０質量％のフレーク状銀粉が
配合されている場合、導体ペーストの硬化塗膜は、３０
×１０-7Ω・ｍ以下、具体的には１０×１０-7Ω・ｍ〜
３０×１０-7Ω・ｍの電気抵抗率を有している。さら
に、本発明の導体ペースト中に、６０〜７０質量％のフ
レーク状銀粉が配合されている場合、導体ペーストの硬
化塗膜は、１００×１０-7Ω・ｍ以下、具体的には３０
×１０-7Ω・ｍ〜１００×１０-7Ω・ｍの電気抵抗率を
有している。また更に、本発明の導体ペースト中に、５
５〜６０質量％のフレーク状銀粉が配合されている場
合、導体ペーストの硬化塗膜は、５００×１０-7Ω・ｍ
以下、具体的には１００×１０-7Ω・ｍ〜５００×１０
-7Ω・ｍの電気抵抗率を有している。Specifically, when 80 to 85% by mass of flake-shaped silver powder is mixed in the conductor paste of the present invention, the cured coating film of the conductor paste is 10 × 10 -7 Ω.
-It has an electrical resistivity of m or less. Moreover, when 70-80 mass% of flake silver powder is mix | blended with the conductor paste of this invention, the hardened coating film of a conductor paste will be 30.
× 10 −7 Ω · m or less, specifically 10 × 10 −7 Ω · m
It has an electric resistivity of 30 × 10 −7 Ω · m. Furthermore, when 60 to 70% by mass of flake-shaped silver powder is mixed in the conductor paste of the present invention, the cured coating film of the conductor paste is 100 × 10 −7 Ω · m or less, specifically 30
It has an electrical resistivity of × 10 -7 Ω · m~100 × 10 -7 Ω · m. Furthermore, in the conductor paste of the present invention, 5
When 5 to 60% by mass of flake silver powder is blended, the cured coating film of the conductor paste is 500 × 10 −7 Ω · m.
Hereinafter, specifically, 100 × 10 −7 Ω · m to 500 × 10
-It has an electrical resistivity of -7 Ω · m.
【００２１】[0021]
【実施例】次に本発明を実施例に基づいて更に詳細に説
明する。EXAMPLES The present invention will be described in more detail based on examples.
【００２２】（実施例１）半径が１５ｃｍで、高さが３
０ｃｍの円筒容器と、この円筒容器内に配置された攪拌
翼（半径１４ｃｍ）とを備えた攪拌ボールミルを用意し
た。Example 1 A radius of 15 cm and a height of 3
A stirring ball mill provided with a 0 cm cylindrical container and a stirring blade (radius 14 cm) arranged in the cylindrical container was prepared.
【００２３】１０ｋｇの粒状銀紛（ＢＥＴ法比表面積値
１．０ｍ2 ／ｇ）、および３０ｋｇのチタン製ボール
（直径０．８ｍｍ）を攪拌ボールミルの円筒容器内に仕
込んだ。また、８ｋｇのエタノール、および０．２ｋｇ
のオレイン酸を、併せて円筒容器内に仕込んだ。10 kg of granular silver powder (BET specific surface area value 1.0 m 2 / g) and 30 kg of titanium balls (diameter 0.8 mm) were placed in a cylindrical container of a stirring ball mill. Also, 8 kg of ethanol and 0.2 kg
The oleic acid of was also charged in a cylindrical container.
【００２４】攪拌翼の回転数を１０００ｒｐｍに設定し
て、攪拌ボールミルを始動させて粒状銀粉のフレーク化
を開始した。攪拌ボールミルを３時間運転した後に、攪
拌翼の回転を停止した。その後、円筒容器の内容物をろ
過し、ろ液から溶媒を除去して乾燥させてフレーク状銀
粉１を得た。The rotation speed of the stirring blade was set to 1000 rpm and the stirring ball mill was started to start flake formation of the granular silver powder. After the stirring ball mill was operated for 3 hours, the rotation of the stirring blade was stopped. Then, the content of the cylindrical container was filtered, the solvent was removed from the filtrate, and the filtrate was dried to obtain flake silver powder 1.
【００２５】（実施例２）実施例１で使用したのと同じ
攪拌ボールミルを用意した。１０ｋｇの粒状銀紛（ＢＥ
Ｔ法比表面積値１．０ｍ2 ／ｇ）、および３７ｋｇのジ
ルコニア製ボール（直径０．８ｍｍ）を攪拌ボールミル
の円筒容器内に仕込んだ。また、１０ｋｇのイオン交換
水、および０．６ｋｇのジオレイン酸ポリエチレングリ
コールを、併せて円筒容器内に仕込んだ。(Example 2) The same stirred ball mill as that used in Example 1 was prepared. 10 kg of granular silver powder (BE
A T method specific surface area value of 1.0 m 2 / g) and 37 kg of zirconia balls (diameter 0.8 mm) were placed in a cylindrical container of a stirring ball mill. Further, 10 kg of ion-exchanged water and 0.6 kg of polyethylene glycol dioleate were charged together in a cylindrical container.
【００２６】攪拌翼の回転数を１０００ｒｐｍに設定し
て、攪拌ボールミルを始動させて粒状銀粉のフレーク化
を開始した。攪拌ボールミルを３時間運転した後に、攪
拌翼の回転を停止した。その後、円筒容器の内容物をろ
過し、水洗して乾燥させてフレーク状銀粉２を得た。The rotation speed of the stirring blade was set to 1000 rpm and the stirring ball mill was started to start flake formation of the granular silver powder. After the stirring ball mill was operated for 3 hours, the rotation of the stirring blade was stopped. Then, the contents of the cylindrical container were filtered, washed with water and dried to obtain flake silver powder 2.
【００２７】（実施例３）実施例１で使用したのと同じ
攪拌ボールミルを用意した。１０ｋｇの粒状銀紛（ＢＥ
Ｔ法比表面積値１．０ｍ2 ／ｇ）、および３０ｋｇのチ
タン製粉砕ボール（直径０．８ｍｍ）を攪拌ボールミル
の円筒容器内に仕込んだ。また、１０ｋｇのイオン交換
水、０．１ｋｇのオレイン酸、および０．６ｋｇのジオ
レイン酸ポリエチレングリコールを併せて円筒容器内に
仕込んだ。Example 3 The same stirred ball mill used in Example 1 was prepared. 10 kg of granular silver powder (BE
A T method specific surface area value of 1.0 m 2 / g) and 30 kg of titanium crushed balls (diameter 0.8 mm) were placed in a cylindrical container of a stirring ball mill. Further, 10 kg of ion-exchanged water, 0.1 kg of oleic acid, and 0.6 kg of polyethylene glycol dioleate were put together into a cylindrical container.
【００２８】攪拌翼の回転数を１０００ｒｐｍに設定し
て、攪拌ボールミルを始動させて粒状銀粉のフレーク化
を開始した。攪拌ボールミルを３時間運転した後に、攪
拌翼の回転を停止した。その後、円筒容器の内容物をろ
過し、水洗して乾燥させてフレーク状銀粉３を得た。The rotating speed of the stirring blade was set to 1000 rpm and the stirring ball mill was started to start flake formation of the granular silver powder. After the stirring ball mill was operated for 3 hours, the rotation of the stirring blade was stopped. Then, the contents of the cylindrical container were filtered, washed with water and dried to obtain flake silver powder 3.
【００２９】（比較例１）半径が１５ｃｍで高さが３０
ｃｍの回転する円筒容器を備えた従来周知のボールミル
を用意した。１０ｋｇの粒状銀紛（ＢＥＴ法比表面積値
１．０ｍ2 ／ｇ）、および３０ｋｇのチタン製粉砕ボー
ル（直径０．８ｍｍ）を上記ボールミルの円筒容器内に
仕込んだ。また、８ｋｇのエタノール、および０．２ｋ
ｇのオレイン酸を、併せて円筒容器内に仕込んだ。COMPARATIVE EXAMPLE 1 A radius of 15 cm and a height of 30
A conventionally known ball mill having a rotating cylindrical container of cm was prepared. 10 kg of granular silver powder (BET specific surface area value 1.0 m 2 / g) and 30 kg of titanium crushed balls (diameter 0.8 mm) were charged in the cylindrical container of the ball mill. Also, 8 kg of ethanol and 0.2 k
The oleic acid of g was put together in a cylindrical container.
【００３０】円筒容器の回転数を７５ｒｐｍに設定し
て、ボールミルを始動させて粒状銀粉のフレーク化を開
始した。ボールミルを２４時間運転した後に、円筒容器
の回転を停止した。その後、円筒容器の内容物をろ過し
て乾燥させてフレーク状銀粉１１を得た。The rotational speed of the cylindrical container was set to 75 rpm and the ball mill was started to start flake formation of the granular silver powder. After operating the ball mill for 24 hours, the rotation of the cylindrical container was stopped. Then, the contents of the cylindrical container were filtered and dried to obtain flake silver powder 11.
【００３１】上記のようにして本発明に従うフレーク状
銀粉１、２および３、並びに比較例としてのフレーク状
銀粉１１について、レーザー回折５０％粒径、見掛密度
およびＢＥＴ法比表面積値を測定した。これらの測定デ
ータを表１に記載する。As described above, with respect to the flaky silver powders 1, 2 and 3 according to the present invention and the flaky silver powder 11 as a comparative example, the laser diffraction 50% particle size, the apparent density and the BET specific surface area value were measured. . These measurement data are shown in Table 1.
【００３２】なお、レーザー回折５０％粒径、見掛密度
およびＢＥＴ法比表面積値は、次のようにして測定し
た。
レーザー回折５０％粒径； 株式会社島津製作所製ＳＡ
ＬＤ−３０００Ｊを使用して測定した。
見掛密度； ＪＩＳ Ｚ ２５０４に従って測定した。
ＢＥＴ法比表面積値； 株式会社島津製作所製フローソ
ーブＩＩ２３００を使用して測定した。The laser diffraction 50% particle size, the apparent density and the BET specific surface area value were measured as follows. Laser diffraction 50% particle size; Shimadzu Corporation SA
It measured using LD-3000J. Apparent density: Measured according to JIS Z 2504. BET specific surface area value: Measured using a Flowsorb II2300 manufactured by Shimadzu Corporation.
【００３３】[0033]
【表１】 [Table 1]
【００３４】表１の結果より明らかなように、比較例と
してのフレーク状銀粉１１と比べて、本発明に従うフレ
ーク状銀粉１〜３は、いずれも、レーザー回折５０％粒
径が小さく、見掛密度が小さく、しかもＢＥＴ法比表面
積値が大きくなっていることが分かる。As is clear from the results shown in Table 1, all of the flaky silver powders 1 to 3 according to the present invention have a smaller 50% particle size by laser diffraction than the flake silver powder 11 as a comparative example, and the apparent flake silver powders are apparent. It can be seen that the density is low and the BET specific surface area value is high.
【００３５】また、本発明に従うフレーク状銀粉１およ
び比較例としてのフレーク状銀粉１１を使用して導体ペ
ーストを調製した。表２に示す組成にてフレーク状銀
粉、アクリル樹脂およびイソプロピルアルコールを混合
し、本発明に従う導体ペースト１−５５、１−６０、１
−６５、１−７０、１−７５および１−８０、並びに比
較例としての導体ペースト１１−７５、１１−８０およ
び１１−８５を調製した。A conductor paste was prepared using the flake silver powder 1 according to the present invention and the flake silver powder 11 as a comparative example. Flake-shaped silver powder, acrylic resin and isopropyl alcohol are mixed in the composition shown in Table 2, and the conductor pastes 1-55, 1-60, 1 according to the present invention are mixed.
-65, 1-70, 1-75 and 1-80, and conductor pastes 11-75, 11-80 and 11-85 as comparative examples were prepared.
【００３６】[0036]
【表２】 [Table 2]
【００３７】上記のようにして得られた本発明に従う導
体ペースト１−５５、１−６０、１−６５、１−７０、
１−７５および１−８０、並びに比較例としての導体ペ
ースト１１−７５、１１−８０および１１−８５のそれ
ぞれを、ガラス基板上に幅が５ｍｍで長さが５ｃｍのラ
イン状になるように塗布した。その後、１００℃で１５
分間加熱して硬化させて、膜厚１３μｍの硬化塗膜１−
５５、１−６０、１−６５、１−７０、１−７５および
１−８０、並びに硬化塗膜１１−７５、１１−８０およ
び１１−８５を得た。The conductor pastes 1-55, 1-60, 1-65, 1-70 according to the present invention obtained as described above,
1-75 and 1-80, and conductor pastes 11-75, 11-80 and 11-85 as comparative examples, respectively, were applied on a glass substrate in a line shape having a width of 5 mm and a length of 5 cm. did. Then, at 100 ℃ 15
Cured by heating for 1 minute to form a 13 μm thick cured coating film 1-
55, 1-60, 1-65, 1-70, 1-75 and 1-80, and cured coating films 11-75, 11-80 and 11-85 were obtained.
【００３８】〔室温における電気抵抗率〕上記のように
して得られた長さ５ｃｍを有するライン状の硬化塗膜の
両端部から０．５ｍｍの所に４端子法電気抵抗測定器の
プローブを当てて、その間（即ち、膜厚１３μｍ、幅５
ｍｍおよび長さ４ｃｍ分の硬化塗膜）における室温での
電気抵抗値を測定した。硬化塗膜の膜厚、幅および長さ
から電気抵抗率に換算した結果を、図１に表す。[Electrical Resistivity at Room Temperature] A probe of a four-terminal method electrical resistance measuring device was applied to the area of 0.5 mm from both ends of the line-shaped cured coating film having a length of 5 cm obtained as described above. In the meantime (that is, film thickness 13 μm, width 5
The electric resistance value at room temperature of a cured coating film having a length of 4 mm and a length of 4 mm was measured. The results of converting the film thickness, width and length of the cured coating film into electrical resistivity are shown in FIG.
【００３９】図１に示す結果より明らかなように、本発
明による導体ペーストは、比較例としての導体ペースト
よりも、フレーク状銀粉の含有量が低くても優れた導電
性を有していることが分かる。具体的には、従来の導体
ペーストでは十分な導電性を得るためにはフレーク状銀
粉を８５質量％以上含有させる必要があるのに対し、本
発明の導体ペーストでは、フレーク状銀粉の含有量が８
０質量％以上において良好な導電性を有していることに
加え、フレーク状銀粉の含有率を８０質量％以下（８０
〜６０質量％）に減らしても、優れた導電性を有してい
ることが明らかとなった。As is clear from the results shown in FIG. 1, the conductor paste according to the present invention has better conductivity than the conductor paste as the comparative example even when the content of the flake silver powder is low. I understand. Specifically, in the conventional conductor paste, in order to obtain sufficient conductivity, it is necessary to contain flake-shaped silver powder in an amount of 85% by mass or more, whereas in the conductor paste of the present invention, the content of flake-shaped silver powder is 8
In addition to having good conductivity at 0 mass% or more, the content of flaky silver powder is 80 mass% or less (80
It has been found that even if the amount is reduced to 60% by mass), excellent conductivity is achieved.
【００４０】〔昇温加熱後の電気抵抗値〕また、先に作
製した本発明に従う硬化塗膜１−８０、並びに比較例と
しての硬化塗膜１１−８０および１１−８５について、
１００℃から２００℃への昇温加熱後の電気抵抗値の変
化を測定した。この測定は次のようにして行った。[Electrical resistance value after heating at elevated temperature] In addition, regarding the cured coating films 1-80 according to the present invention prepared above and the cured coating films 11-80 and 11-85 as comparative examples,
The change in electric resistance value after heating by heating from 100 ° C. to 200 ° C. was measured. This measurement was performed as follows.
【００４１】即ち、温度制御が可能なオーブンを用意
し、まず、温度を１００℃に設定してオーブンを作動す
る。３０分後、オーブン内の温度が一定に保たれてか
ら、試料、即ち硬化塗膜が形成されたガラス基板をオー
ブンに入れる。１５分経過後に、試料をオーブンから取
り出すとともにオーブンを１２５℃に再設定する。試料
をオーブンから取り出して１５分間室温で放置し、先に
述べたのと同様にして４端子法電気抵抗測定器を用いて
硬化塗膜の電気抵抗値を測定する。電気抵抗値を測定し
てから約１５分経過後（オーブンを１２５℃に再設定し
てから３０分経過後）に、この試料を再びオーブンに入
れる。以下、同様にして、オーブンを２５℃づつ段階的
に昇温し、３０分間かけてオーブンの温度を安定させた
後にオーブンに試料を入れて１５分間試料を加熱し、そ
の後試料をオーブンから取り出して１５分間室温に放置
してから、その電気抵抗値を測定した。２００℃まで昇
温させた。That is, an oven whose temperature can be controlled is prepared. First, the temperature is set to 100 ° C. and the oven is operated. After 30 minutes, the temperature in the oven is kept constant, and then the sample, that is, the glass substrate on which the cured coating film is formed, is placed in the oven. After 15 minutes, remove the sample from the oven and reset the oven to 125 ° C. The sample is taken out of the oven and left at room temperature for 15 minutes, and the electrical resistance value of the cured coating film is measured using a four-terminal method electrical resistance measuring instrument in the same manner as described above. About 15 minutes after measuring the electric resistance value (30 minutes after resetting the oven to 125 ° C.), the sample is put into the oven again. In the same manner, the temperature of the oven is raised stepwise by 25 ° C., the temperature of the oven is stabilized over 30 minutes, the sample is put in the oven and the sample is heated for 15 minutes, and then the sample is taken out of the oven. After being left at room temperature for 15 minutes, its electric resistance value was measured. The temperature was raised to 200 ° C.
【００４２】図２は、測定された昇温加熱後の電気抵抗
値の測定データから作成した電気抵抗値の変化を表して
いる。また、図３は、図２に示す本発明の導体ペースト
１−７０、１−７５および１−８０に関する測定データ
を編集して、１００℃における電気抵抗値を１として加
熱による電気抵抗値の変化率を表している。FIG. 2 shows the change in the electric resistance value created from the measured data of the electric resistance value after the measured heating and heating. In addition, FIG. 3 is a compilation of the measurement data for the conductor pastes 1-70, 1-75 and 1-80 of the present invention shown in FIG. It represents the rate.
【００４３】図２に示す結果より明らかなように、１５
０℃から２００℃の間（１７５℃付近）において僅かな
電気抵抗値のピークが観測された。このピークは、図３
を参照すると更に明らかである。これは、本発明による
導体ペーストに含まれるフレーク状銀粉が１５０℃から
２００℃の間（１７５℃付近）において溶融しているた
めと考えられる。このように１５０℃から２００℃の間
（１７５℃付近）において溶融する本発明による導体ペ
ーストは、電子部品の確実且つ強固な実装に役立つもの
と考えられる。As is clear from the results shown in FIG.
A slight electric resistance peak was observed between 0 ° C and 200 ° C (around 175 ° C). This peak is shown in FIG.
Will be more apparent with reference to. It is considered that this is because the flake-shaped silver powder contained in the conductor paste according to the present invention is melted between 150 ° C and 200 ° C (around 175 ° C). Thus, the conductor paste according to the present invention that melts between 150 ° C. and 200 ° C. (around 175 ° C.) is considered to be useful for reliable and firm mounting of electronic components.
【００４４】〔表面状態〕本発明に従う硬化塗膜１−８
０および比較例としての硬化塗膜１１−８０について、
１７５℃での加熱処理の前後における表面状態を走査電
子顕微鏡（ＳＥＭ）を使用して観察した。図４は、硬化
塗膜１−８０の１００℃および１７５℃での加熱処理後
の表面状態を示す拡大図であり、図５は硬化塗膜１１−
８０の１７５℃での加熱処理後の表面状態を示す拡大図
である。[Surface Condition] Cured coating film 1-8 according to the present invention
0 and the cured coating film 11-80 as a comparative example,
The surface condition before and after the heat treatment at 175 ° C. was observed using a scanning electron microscope (SEM). FIG. 4 is an enlarged view showing the surface state of the cured coating film 1-80 after heat treatment at 100 ° C. and 175 ° C., and FIG. 5 is the cured coating film 11-.
It is an enlarged view which shows the surface state of 80 after heat processing at 175 degreeC.
【００４５】図４より明らかなように、本発明に従う硬
化塗膜１−８０の場合、１００℃での加熱処理では、フ
レーク状銀粉が鋭いエッジを有しており、鱗状に配列さ
れて硬化塗膜が形成されている様子が観察されたが、１
７５℃での加熱処理後には、フレーク状銀粉のエッジは
僅かに溶融して収縮し、フレーク状銀粉同士の接触がや
や低下している様子が確認された。このフレーク状銀粉
同士の接触の低下が、図２および図３に示す電気抵抗値
のピークを与えているものと考えられる。一方、比較例
としての硬化塗膜１１−８０では、１００℃での加熱処
理では、硬化塗膜１−８０の場合と同様に、フレーク状
銀粉は鋭いエッジを有しており、鱗状に配列されて硬化
塗膜が形成されている様子が観察されたが（図示せ
ず）、図５に示すように、この鋭いエッジは加熱処理を
行った後にも残っており、１７５℃の加熱処理ではフレ
ーク状銀粉の溶融の開始は確認されなかった。図４およ
び図５に示す表面状態の比較より、本発明のフレーク状
銀粉は、従来のフレーク状銀粉よりも細かく且つ薄い形
状を有しており、比較的低温、即ち１５０℃から２００
℃の間（特に１７５℃）においてフレーク状銀粉を部分
的に溶融させることができる。従って、本発明の導体ペ
ーストは電子部品の確実且つ強固な実装に役立つものと
考えられる。As is clear from FIG. 4, in the case of the cured coating film 1-80 according to the present invention, the heat treatment at 100 ° C. causes the flaky silver powder to have sharp edges and be arranged in a scale-like cured coating. It was observed that the film was formed.
After the heat treatment at 75 ° C., it was confirmed that the edges of the flaky silver powder were slightly melted and shrunk, and the contact between the flaky silver powders was slightly lowered. It is considered that the decrease in the contact between the flaky silver powder particles gives the peak of the electric resistance value shown in FIGS. 2 and 3. On the other hand, in the case of the cured coating film 11-80 as a comparative example, in the heat treatment at 100 ° C., the flaky silver powder has sharp edges and is arranged in a scale like the cured coating film 1-80. Although it was observed that a cured coating film had been formed (not shown), as shown in FIG. 5, the sharp edges remained after the heat treatment, and the flake was generated by the heat treatment at 175 ° C. No onset of melting of the powdery silver powder was confirmed. From the comparison of the surface states shown in FIGS. 4 and 5, the flake silver powder of the present invention has a finer and thinner shape than the conventional flake silver powder, and is at a relatively low temperature, that is, 150 ° C. to 200 ° C.
The flaky silver powder can be partially melted between 0 ° C (particularly 175 ° C). Therefore, the conductor paste of the present invention is considered to be useful for reliable and firm mounting of electronic components.
【図１】 本発明による導体ペーストと従来の導体ペー
ストについての、フレーク状銀粉の含有量と電気抵抗率
との関係を示す図である。FIG. 1 is a diagram showing the relationship between the content of flaky silver powder and the electrical resistivity of a conductor paste according to the present invention and a conventional conductor paste.
【図２】 本発明によるフレーク状銀粉と従来のフレー
ク状銀粉についての、昇温加熱後の電気抵抗値の変化を
示す図である。FIG. 2 is a diagram showing changes in the electric resistance values of the flake silver powder according to the present invention and the conventional flake silver powder after heating at elevated temperatures.
【図３】 本発明によるフレーク状銀粉についての昇温
加熱後の電気抵抗値の変化率を示す図である。FIG. 3 is a diagram showing a rate of change in electric resistance value of the flake silver powder according to the present invention after heating at elevated temperature.
【図４】 本発明による硬化塗膜の１００℃と１７５℃
での加熱処理における表面状態を比較する図である。FIG. 4 100 ° C. and 175 ° C. of a cured coating according to the invention
It is a figure which compares the surface state in the heat processing in.
【図５】 比較例としての硬化塗膜の１７５℃での加熱
処理における表面状態を比較する図である。FIG. 5 is a diagram comparing surface states of a cured coating film as a comparative example in a heat treatment at 175 ° C.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 梶田 治 京都府宇治市五ケ庄北ノ庄11−11 Ｆターム(参考） 4K017 AA03 BA02 CA03 DA01 DA07 EA01 EA04 4K018 BA01 BB01 BB04 BC08 BD04 5G301 DA03 DA42 DD01 DE10 ─────────────────────────────────────────────────── ─── Continued front page (72) Inventor Osamu Kajita 11-11 Gonosho Kitanosho, Uji City, Kyoto Prefecture F-term (reference) 4K017 AA03 BA02 CA03 DA01 DA07 EA01 EA04 4K018 BA01 BB01 BB04 BC08 BD04 5G301 DA03 DA42 DD01 DE10
Claims (8)
法５０％粒径が３〜８μｍであり、見掛密度が０．４〜
１．１／ｃｍ3 であり、しかもＢＥＴ法比表面積値が
１．５〜４．０ｍ2 ／ｇであることを特徴とする導体ペ
ースト用銀粉。1. A flake-shaped particle shape, a 50% particle size by laser diffraction method is 3 to 8 μm, and an apparent density is 0.4 to
1.1 / cm 3, and moreover silver conductor paste BET specific surface area value is equal to or is 1.5~4.0m 2 / g.
内に設けられた攪拌翼とを備えた攪拌ボールミルを使用
する導体ペースト用銀粉の製造方法であって、前記製造
方法は、粒状銀粉、前記粒状銀粉をフレーク化するため
のボール、溶媒および処理剤を前記容器内に仕込み、５
〜３００Ｇの遠心力が前記容器内に加わるように、前記
攪拌翼を回転させて、前記粒状銀粉をフレーク化してろ
過し、これによってレーザー回折法５０％粒径が３〜８
μｍであり、見掛密度が０．４〜１．１／ｃｍ3 であ
り、しかもＢＥＴ法比表面積値が１．５〜４．０ｍ2 ／
ｇであるフレーク状銀粉を得ることを特徴とするフレー
ク状銀粉の製造方法。2. A method for producing a silver powder for a conductor paste using a stirring ball mill provided with a container having a cylindrical inner surface and a stirring blade provided in the container, wherein the manufacturing method is granular silver powder. , A ball for flake the granular silver powder, a solvent and a treating agent are charged into the container, and 5
The stirring blade is rotated so that a centrifugal force of up to 300 G is applied to the inside of the container, and the granular silver powder is flaked and filtered, whereby a 50% particle diameter by laser diffraction is 3-8.
μm, the apparent density is 0.4 to 1.1 / cm 3 , and the BET specific surface area value is 1.5 to 4.0 m 2 /
A method for producing flaky silver powder, characterized in that the flaky silver powder of g is obtained.
面活性剤から成り、得られるフレーク状銀粉の表面積１
ｍ2 あたり合計で０．００５〜０．１ｇの前記処理剤が
前記容器内に仕込まれていることを特徴とする請求項２
に記載のフレーク状銀粉の製造方法。3. The surface treatment 1 of the resulting flake-shaped silver powder, wherein the treating agent comprises a fatty acid and / or a surfactant.
A total of 0.005 to 0.1 g of the treating agent per m 2 is charged in the container.
The method for producing a flake-shaped silver powder according to.
から成り、０．１〜１ｍｍの直径を有していることを特
徴とする請求項２に記載のフレーク状銀粉の製造方法。4. The method for producing flaky silver powder according to claim 2, wherein the ball is made of titanium or zirconia and has a diameter of 0.1 to 1 mm.
であり、見掛密度が０．４〜１．１／ｃｍ3 であり、し
かもＢＥＴ法比表面積値が１．５〜４．０ｍ2 ／ｇであ
るフレーク状銀粉、および樹脂からなる導体ペーストで
あって、前記導体ペーストは、１５０〜２００℃の間に
電気抵抗値のピークを有することを特徴とする導体ペー
スト。5. Laser diffraction method 50% particle size is 3 to 8 μm
And a conductor paste composed of a resin and a flaky silver powder having an apparent density of 0.4 to 1.1 / cm 3 and a BET specific surface area value of 1.5 to 4.0 m 2 / g. The conductor paste has a peak electric resistance value in the range of 150 to 200 ° C.
の前記フレーク状銀粉を含んでおり、前記導体ペースト
の硬化塗膜は、１０×１０-7Ω・ｍ以下の電気抵抗率を
有していることを特徴とする請求項５に記載の導体ペー
スト。6. The conductive paste is 80 to 85 mass%.
6. The conductor paste according to claim 5, wherein the conductor paste contains the flake-shaped silver powder, and the cured coating film of the conductor paste has an electric resistivity of 10 × 10 −7 Ω · m or less. .
の前記フレーク状銀粉を含んでおり、前記導体ペースト
の硬化塗膜は、３０×１０-7Ω・ｍ以下の電気抵抗率を
有していることを特徴とする請求項５に記載の導体ペー
スト。7. The conductor paste is 70-80% by mass.
6. The conductor paste according to claim 5, wherein the conductor paste contains the flake-shaped silver powder, and the cured coating film of the conductor paste has an electric resistivity of 30 × 10 −7 Ω · m or less. .
の前記フレーク状銀粉を含んでおり、前記導体ペースト
の硬化塗膜は、１００×１０-7Ω・ｍ以下の電気抵抗率
を有していることを特徴とする請求項５に記載の導体ペ
ースト。8. The conductive paste is 60 to 70 mass%.
6. The conductor paste according to claim 5, wherein the conductor paste contains the flake-shaped silver powder, and the cured coating film of the conductor paste has an electric resistivity of 100 × 10 −7 Ω · m or less. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001244169A JP3874634B2 (en) | 2001-08-10 | 2001-08-10 | Flake-like silver powder for conductor paste and conductor paste using the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001244169A JP3874634B2 (en) | 2001-08-10 | 2001-08-10 | Flake-like silver powder for conductor paste and conductor paste using the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2003055701A true JP2003055701A (en) | 2003-02-26 |
| JP3874634B2 JP3874634B2 (en) | 2007-01-31 |
Family
ID=19074146
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001244169A Expired - Fee Related JP3874634B2 (en) | 2001-08-10 | 2001-08-10 | Flake-like silver powder for conductor paste and conductor paste using the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3874634B2 (en) |
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| CN114888294A (en) * | 2022-05-14 | 2022-08-12 | 安徽纳洛米特新材料科技股份有限公司 | Method for industrially producing flaky nano nickel powder |
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