JPS60250077A - Preparation of electrically conductive paste filled with base metal powder - Google Patents

Preparation of electrically conductive paste filled with base metal powder

Info

Publication number
JPS60250077A
JPS60250077A JP10446384A JP10446384A JPS60250077A JP S60250077 A JPS60250077 A JP S60250077A JP 10446384 A JP10446384 A JP 10446384A JP 10446384 A JP10446384 A JP 10446384A JP S60250077 A JPS60250077 A JP S60250077A
Authority
JP
Japan
Prior art keywords
powder
base metal
metal powder
organic
organic solvent
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.)
Pending
Application number
JP10446384A
Other languages
Japanese (ja)
Inventor
Takashi Ogata
緒方　俊
Masashi Kumagai
正志 熊谷
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Eneos Corp
Original Assignee
Nippon Mining Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nippon Mining Co Ltd filed Critical Nippon Mining Co Ltd
Priority to JP10446384A priority Critical patent/JPS60250077A/en
Publication of JPS60250077A publication Critical patent/JPS60250077A/en
Pending legal-status Critical Current

Links

Classifications

    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/09—Use of materials for the conductive, e.g. metallic pattern
    • H05K1/092—Dispersed materials, e.g. conductive pastes or inks
    • H05K1/095—Dispersed materials, e.g. conductive pastes or inks for polymer thick films, i.e. having a permanent organic polymeric binder

Abstract

PURPOSE:To prepare the titled paste which is inexpensive and provides an electrical connection not susceptible to changes with time, by treating base metal powder in a specified process for removal of surface oxides and mixing the powder with a resin in an inert gas atmosphere. CONSTITUTION:Base metal powder (e.g. copper, nickel or iron in powder) is dipped in an organic solvent soln. of an organic acid (ester, oxime), e.g. fatty acid or phosphonic ester, for removal of metal oxides deposited on the surface. The powder is washed with a low-boiling organic solvent (e.g. hexane) so that pick-up of the organic solvent used above may be reduced to below about 1%. The powder is dried in an inert gas atmosphere and is mixed into an organic material (e.g. epoxy or xylene resin) to prepare the electrically conductive paste.

Description

【発明の詳細な説明】 発明の目的 急速な電子工業技術の進歩忙伴ない、製作容易外電子回
路印刷配線用材料、導電性接着剤あるいは近年とみに問
題となっている電磁シールド用材料として導電性ペース
トの重要性が叫ばれている、現在、貴金属特に銀粉末乃
至銀コート粉末を用いた導電塗料が多く用いられている
が、貴金属系粉末は高価であるという問題がち杭 電気的特性が良好でかつ安価な卑金属粉としては銅粉を
はじめとしてニッケル粉その他があるが、耐酸化性が劣
る故に実用化が困難であった。しかしこれが実用化すれ
ば大きなコストダウン効果が期待されるため、従来から
種々の工夫がなされて来た、 従来の技術 例えば金属粉製造時に樹脂や脂肪酸を混入し。[Detailed Description of the Invention] Purpose of the Invention With the rapid progress of electronic industry technology, it is easy to manufacture, and is useful as a material for printed wiring of electronic circuits, a conductive adhesive, or a material for electromagnetic shielding, which has become a problem in recent years. The importance of pastes has been emphasized.Currently, conductive paints using precious metals, especially silver powders or silver-coated powders, are often used, but noble metal powders tend to be expensive and do not have good electrical properties. Although there are copper powder, nickel powder, and other inexpensive base metal powders, it has been difficult to put them into practical use because of their poor oxidation resistance. However, if this is put into practical use, it is expected to have a significant cost reduction effect, so various innovations have been made to date, such as mixing resins and fatty acids during the production of metal powder.

金属粉表面を被覆する方法（特開昭５１−４７９２４゜
同５３−１３３７９９　）、あるいは金属水素化物や有
機物系還元剤を添加する方法（特開昭５３−６３５９４
、同５４−２２４４９　）がある。しかし。A method of coating the surface of metal powder (JP-A-51-47924, JP-A-53-133799), or a method of adding a metal hydride or an organic reducing agent (JP-A-53-63594)
, 54-22449). but.

前者においては好適な範囲の粒度分布の金属粉を製造す
ることが困難である。すなわち、この方法によって製造
される金属粉の形状は扁平であシ、厚さは薄くなるが粒
径は比較的大きく（２０〜４０μ）なるのでスクリーン
印刷等が困難となる。また、粉砕時に装置から混入する
不純物を除去することはできない。In the former case, it is difficult to produce metal powder with a particle size distribution within a suitable range. That is, the shape of the metal powder produced by this method is flat and thin, but the particle size is relatively large (20 to 40 microns), making screen printing difficult. Furthermore, it is not possible to remove impurities that enter the equipment during pulverization.

後者においては、還元剤を用いた場合２反応により生成
する水素ガスまたは水分がペーストに悪影響を及ばずこ
とがある。また、金属粉が有機物被膜で防錆されている
場合には還元剤の種類および添加量の選定が困難である
。In the latter case, when a reducing agent is used, the hydrogen gas or moisture produced by the two reactions may not have an adverse effect on the paste. Furthermore, when the metal powder is rust-proofed with an organic coating, it is difficult to select the type and amount of reducing agent to be added.

発明の構成 前述のことに鑑み９本発明者らは導電性を低下させる金
属酸化物の除去および酸化物除去後の再酸化防止につい
て効率的な方法を探求すべく種々の検討を行なった結果
２本発明をなすに至った。以下図のフローシートに沿っ
て具体的に説明する。Structure of the Invention In view of the above, the present inventors have conducted various studies in order to find an efficient method for removing metal oxides that reduce conductivity and preventing re-oxidation after oxide removal.2 The present invention has been accomplished. A detailed explanation will be given below according to the flow sheet shown in the figure.

まず使用する卑金属粉の表面に形成された金属酸化物を
有機酸、有機酸エステル、オキシムから選択された一種
以上を含有する有機溶媒と該卑金属粉とを接触させるこ
とによって除去する、上記有機溶媒に含有される有機酸
などとしてＵ、ＩＪン酸エステル、ホスホン酸エステル
。First, the metal oxide formed on the surface of the base metal powder to be used is removed by bringing the base metal powder into contact with an organic solvent containing one or more selected from organic acids, organic acid esters, and oximes. Examples of organic acids contained in U, IJ, phosphonic acid esters, and phosphonic acid esters.

ヒドロキシオキシムあるいは脂肪酸が挙げられ。Examples include hydroxyoximes or fatty acids.

卑金属粉の種類および反応条件により、上記のうち一種
あるいは二種以上が選択される。以上の卑金属粗表面の
酸化物除去方法は１本出願人が先年出願した特願昭５７
−２０３６５６の方法である。ここで卑金属粉は微細に
なれば有機物との濡れ性が良くなるため、この反応にお
いては金属粉は有機相に覆われるため、水分の存在は支
障とならない。One or more of the above may be selected depending on the type of base metal powder and reaction conditions. The above method for removing oxides from rough surfaces of base metals is described in a patent application filed in 1983 by the applicant last year.
-203656 method. Here, the finer the base metal powder, the better its wettability with organic matter, so the presence of water does not pose a problem since the metal powder is covered with the organic phase in this reaction.

酸化物除去後の卑金属粉は、沈降、濾過等圧よシ液から
分離し、ヘキサン等の低沸点有機洗浄剤で付着有機溶剤
を付着率１ｅｌｊ以下となるまで洗浄除去する。ここで
卑金属とは貴金属以外の金属を意味し、特に銅、ニッケ
ル、コバルト。The base metal powder after oxide removal is separated from the isobaric liquid by sedimentation, filtration, and is washed with a low boiling point organic detergent such as hexane until the adhesion rate becomes 1elj or less. Base metals here mean metals other than precious metals, especially copper, nickel, and cobalt.

錫あるいは鉄が好適に用いられる。また、卑金属粉とし
ては・、単一金属粉以外に１合金粉あるいは複合粉も対
象となる。Tin or iron is preferably used. Furthermore, as base metal powders, in addition to single metal powders, 1-alloy powders or composite powders are also applicable.

洗浄終了後、水素ガスあるいは窒素ガスなどの不活性ガ
スの雰囲気中で固液分離し、更に該雰囲気中で乾燥させ
る。前記有機洗浄剤として低沸点洗浄剤を用いるのは、
乾燥を容易にするためである。After cleaning, solid-liquid separation is performed in an atmosphere of an inert gas such as hydrogen gas or nitrogen gas, and the product is further dried in the atmosphere. The use of a low boiling point detergent as the organic detergent is because
This is to facilitate drying.

乾燥後の卑金属粉を水素ガスあるいは不活性ガス雰囲気
中で例えばエポキシ樹脂、キシレン等から成るペースト
製造用有機材料と混練する。The dried base metal powder is kneaded with an organic material for paste production, such as epoxy resin, xylene, etc., in a hydrogen gas or inert gas atmosphere.

ここで使用するペースト製造用有機材料も予め脱気等に
より溶解混入した酸素を除去しておくことが好ましい。It is preferable that the organic material used for producing the paste used here also be degassed or the like to remove dissolved oxygen in advance.

卑金属粗表面の酸化物除去作業によって生成する金属イ
オン含有有機溶媒は逆抽出用水溶液としての硫酸、塩酸
などの鉱酸を含む水溶液と接触することにより再生され
、くり返し使用さ−れる。逆抽出後の水溶液は〈シ返し
逆抽出に使用され、金属イオンが適当な濃度まで蓄積し
た段階で水素還元、電解採取など罠よシ金属粉が回収さ
れ、鉱酸が再生される。The metal ion-containing organic solvent produced by removing oxides from the rough base metal surface is regenerated by contacting with an aqueous solution containing a mineral acid such as sulfuric acid or hydrochloric acid as an aqueous solution for back extraction, and is used repeatedly. The aqueous solution after back extraction is used for back extraction, and when the metal ions have accumulated to an appropriate concentration, the metal powder is recovered by hydrogen reduction, electrowinning, etc., and the mineral acid is regenerated.

洗浄工程で用いられた有機洗浄剤は蒸留により気化後冷
却回収される。卑金属粉を洗浄した際に卑金属粗表面か
ら有機洗浄剤中に移行した有機溶媒社、上記蒸留工程に
て蒸留残物として残るので、逆抽出工程へくシ返す。乾
燥工程で気化した有機洗浄剤も冷却回収後洗浄工程へく
り返される。The organic cleaning agent used in the cleaning process is vaporized by distillation and then cooled and recovered. The organic solvent that migrates from the rough surface of the base metal into the organic cleaning agent when the base metal powder is washed remains as a distillation residue in the above distillation process, so it is returned to the back extraction process. The organic cleaning agent vaporized during the drying process is also recycled to the cleaning process after being cooled and collected.

発明の効果 本発明は１以上述べた如く、卑金属粗表面の金属酸化物
を有機酸等を含有する有機溶媒と接触させることＫよっ
て除去し１次いで卑金属粗表面に付着した有機溶媒を有
機洗浄剤を用いて洗浄除去し、その後水素ガスあるいは
不活性ガス雰囲気中で乾燥およびペースト製造用有機材
料との混練を行々う方法であシ、特殊な添加剤を必要と
せずクローズドシステム化可能な容易な導電性ペースト
製造方法を供するものであり。Effects of the Invention As described above, the present invention removes metal oxides on the rough surface of a base metal by bringing them into contact with an organic solvent containing an organic acid, etc., and then removes the organic solvent adhering to the rough surface of the base metal using an organic cleaning agent. This method involves cleaning and removing the material using hydrogen gas or inert gas, followed by drying in a hydrogen gas or inert gas atmosphere, and kneading it with an organic material for paste production.It does not require any special additives and can be easily constructed into a closed system. The present invention provides a method for producing a conductive paste.

その効果は大きい。なお近年種々の目的で複合粉の開発
が盛んであるが１本発明は表面が卑金属で覆われた複合
粉をも含むものである。The effect is great. In recent years, development of composite powders has been active for various purposes, and the present invention also includes composite powders whose surfaces are covered with base metals.

以下、卑金属粉として最も汎用性のある銅粉を用いた導
電ペーストについて実施例を示して説明する。Hereinafter, a conductive paste using copper powder, which is the most versatile base metal powder, will be described with reference to examples.

実施例 電解銅粉１０ｆと、Ｄ２ＥＨＰＡを８０容積パーセント
になるようにノルマルヘキサンで稀釈した有機溶媒１．
５ｔとを４０℃で３時間攪拌し。Example Electrolytic copper powder 10f and D2EHPA diluted with n-hexane to 80% by volume in an organic solvent 1.
5t and stirred at 40°C for 3 hours.

固液分離後、ノルマルヘキサンで有機相がほぼ無色にな
るまでデカンテーションを行なった。After solid-liquid separation, decantation was performed with n-hexane until the organic phase became almost colorless.

次いで該銅粉を窒素ガス雰囲気中で固液分離および乾燥
をし、更にビスフェノールＡ型エポキシ樹脂、ポリアミ
ド系硬化剤、キシレンおよびエタノールからなるペース
ト製造用有機材料を。Next, the copper powder is subjected to solid-liquid separation and drying in a nitrogen gas atmosphere, and an organic material for paste production consisting of a bisphenol A type epoxy resin, a polyamide curing agent, xylene and ethanol is obtained.

上記乾燥後銅粉含量が８０重量パーセントとなるように
窒素ガス雰囲気中で混練した。After drying, the mixture was kneaded in a nitrogen gas atmosphere so that the copper powder content was 80% by weight.

こうして得られたペーストをガラス板上にアプリケータ
で塗布し、１００℃以下で３０分間硬化乾燥させ象。乾
燥後のペーストの体積固有抵抗値の経時変化の測定結果
を表に示す。この結果から、殆ど経時変化がないことが
判る。The paste thus obtained was applied onto a glass plate with an applicator and cured and dried at 100°C or less for 30 minutes. The table shows the measurement results of the change in volume resistivity of the paste after drying over time. This result shows that there is almost no change over time.

表 比較例 乾燥後の銅粉とペースト製造用有機材料との混線を大気
中で行なった以外は実施例と同様な条件で導電性ペース
トを製造し、該ペーストを実施例の方法で塗布した後乾
燥し２体積固有抵抗値を測定したが、乾燥直後から導電
性は殆ど認められなかった。Table Comparative Example A conductive paste was produced under the same conditions as in the example except that the copper powder after drying and the organic material for paste production were mixed in the atmosphere, and the paste was applied by the method of the example. After drying, the 2-volume resistivity value was measured, but almost no conductivity was observed immediately after drying.

【図面の簡単な説明】[Brief explanation of the drawing]

図は２本発明に係る方法のフローシートである。 特許出願人　日本鉱業株式会社 代理人　弁理士（７５６９）並用啓志 −面の浄書（内容に変更ない フローンート ｌ＋９ 昭和５９年９月亭日 特許庁長官　志賀　学　殿 ■、事件の表示 昭和５９年特許願第１０４４６５号 ２、発明の名称 卑金属粉充填導電性ペーストの製造方法３　補正をする
者 事件との関係　特許出願人 住　所　東京都港区虎ノ門二丁目１０番１号名　称　日
本鉱業株式会社 代表者笠原幸雄 ４、代　理　人 〒１０５　電話５８２−２１１１ 住　所　東京都港区虎ノ門二丁目１０番１号Ｚ補正の内
容 （１）　願書に最初に添付した明細書の浄書・別紙のと
おり（内容に変更なし） （２）　図面の浄書・別紙のとおシ（内容に変更なし） （３）　委任状・別紙のとおり 以　上 １、事件の表示 昭和５９年特許願第１０４４６５号 ２、発明の名称 卑金属粉充填導電性ペーストの製造方法３　補正をする
者 事件との関係　特許出願人 住　所　東京都港区虎ノ門二丁目ｌＯ番１号日本鉱業株
式会社内 ６、補正の対象 明細書の特許請求の範囲の欄 ７−　補正の内容　特許請求の範囲を別紙のとおり補正
する。 別紙 ２、特許請求の範囲 （１）卑金属粉を有機酸、有機酸エステル、オキシムか
ら選択された一種以上を含有する有機溶媒と接触させる
ことによって該卑金属粉表面の金属酸化物を除去し２次
いで表面の金属酸化物が除去された該卑金属貝を低沸点
の有機洗浄剤で洗浄することによシ前記有機溶媒を除き
、しかるのち水素ガスあるいは不活性ガス雰囲気中で乾
燥し、更に水素ガスあるいは不活性ガス雰囲気中でペー
スト製造用有機材料と混合することを特徴とする卑金属
粉充填導電性ペーストの製造方法。 （２）　前記有機溶媒がリン酸エステル、ホスホン酸エ
ステル、ヒドロキシオキシム、脂肪酸から選択された二
種以上を含有するものである特許請求の範囲第１項記載
の方法。 （３）　前記卑金属粉が銅、ニッケル、コバルト。 錫もしくは鉄の粉、これらから選択された一種以上の金
属を含むあるいは複合粉である特許請求の範囲第１項記
載の方法。The figure is a flow sheet of two methods according to the present invention. Patent applicant Nippon Mining Co., Ltd. Agent Patent attorney (7569) General use Keishi - surface engraving (no change in content Flow route l + 9 September 1980) Commissioner of the Patent Office Mr. Manabu Shiga■, Indication of case Patent application No. 1988 104465 No. 2, Name of the invention Method for manufacturing conductive paste filled with base metal powder 3 Relationship to the case of the person making the amendment Patent applicant Address 2-10-1 Toranomon, Minato-ku, Tokyo Name Name Kasahara, Representative of Nippon Mining Co., Ltd. Yukio 4, Agent Address: 105 Phone: 582-2111 Address: 2-10-1 Toranomon, Minato-ku, Tokyo Contents of the Z amendment (1) As per the engraving and attached sheet of the specification originally attached to the application (contents changed) None) (2) Engraving of the drawings and attachment (no change in content) (3) Power of attorney and attachment as above 1. Indication of the case Patent Application No. 104465 of 1982 2. Name of the invention Base metal powder Manufacturing method of filled conductive paste 3 Relationship with the case of the person making the amendment Patent applicant address 6, Nippon Mining Co., Ltd., No. 1, Toranomon 2-chome, Minato-ku, Tokyo; Column 7 - Contents of amendment The claims are amended as shown in the attached sheet. Attachment 2, Claims (1) Base metal powder is treated with an organic solvent containing one or more selected from organic acids, organic acid esters, and oximes. The metal oxide on the surface of the base metal powder is removed by contacting the base metal powder, and the base metal shell from which the metal oxide on the surface has been removed is then washed with a low boiling point organic detergent to remove the organic solvent. A method for producing a base metal powder-filled conductive paste, which is then dried in a hydrogen gas or inert gas atmosphere, and further mixed with an organic material for paste production in a hydrogen gas or inert gas atmosphere. (2) The above-mentioned method. The method according to claim 1, wherein the organic solvent contains two or more selected from phosphoric acid esters, phosphonic acid esters, hydroxyoximes, and fatty acids. (3) The base metal powder contains copper, nickel, The method according to claim 1, wherein the powder is a powder of cobalt, tin or iron, or a composite powder containing one or more metals selected from these.

Claims (3)

【特許請求の範囲】[Claims] （１）　卑金属粉を有機酸、有機酸エステル、オキシム
から選択された一種以上を含有する有機溶媒と接触させ
ることによって該卑金属粉表面の金属酸化物を除去し１
次いで表面の金属酸化物が除去された該卑金属粉を低沸
点の有機洗浄剤で洗浄することにより前記有機溶媒を除
き、しかるのち水素ガスあるいは不活性ガス雰囲気中で
乾燥し、更に水素ガスあるいは不活性ガス雰囲気中でペ
ースト製造用有機材料と混合することを特徴とする卑金
属粉充填導電性ペーストの製造方法。(1) removing metal oxides on the surface of the base metal powder by contacting the base metal powder with an organic solvent containing one or more selected from organic acids, organic acid esters, and oximes;
Next, the base metal powder from which surface metal oxides have been removed is washed with a low boiling point organic detergent to remove the organic solvent, dried in a hydrogen gas or inert gas atmosphere, and then washed with a hydrogen gas or inert gas atmosphere. A method for producing a base metal powder-filled conductive paste, which comprises mixing with an organic material for paste production in an active gas atmosphere. （２）　前記有機溶媒がリン酸エステル、ホスホン酸エ
ステル、ヒドロキシオキシム、脂肪酸から選択された１
種以上を含有するものである特許請求の範囲第１項記載
の方法。(2) 1 in which the organic solvent is selected from phosphoric esters, phosphonic esters, hydroxyoximes, and fatty acids;
The method according to claim 1, which contains more than one species. （３）　前記卑金属粉が銅、ニッケル、コバルト。 錫あるいは鉄の粉、これらから選択された１種以上の金
属を含む合金粉あるいけ複合粉である特許請求の範囲第
１項記載の方法。(3) The base metal powder is copper, nickel, or cobalt. The method according to claim 1, which is tin or iron powder, or an alloy powder or composite powder containing one or more metals selected from these.
JP10446384A 1984-05-25 1984-05-25 Preparation of electrically conductive paste filled with base metal powder Pending JPS60250077A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10446384A JPS60250077A (en) 1984-05-25 1984-05-25 Preparation of electrically conductive paste filled with base metal powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP10446384A JPS60250077A (en) 1984-05-25 1984-05-25 Preparation of electrically conductive paste filled with base metal powder

Publications (1)

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JPS60250077A true JPS60250077A (en) 1985-12-10

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Family Applications (1)

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JP10446384A Pending JPS60250077A (en) 1984-05-25 1984-05-25 Preparation of electrically conductive paste filled with base metal powder

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JP (1) JPS60250077A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006169634A (en) * 2004-12-15 2006-06-29 Samsung Electro Mech Co Ltd Surface treatment method for nickel particle using acid solution

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006169634A (en) * 2004-12-15 2006-06-29 Samsung Electro Mech Co Ltd Surface treatment method for nickel particle using acid solution
JP4602238B2 (en) * 2004-12-15 2010-12-22 三星電機株式会社 Surface treatment method of nickel particles using acid solution

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