JPH031386B2 - - Google Patents
Info
- Publication number
- JPH031386B2 JPH031386B2 JP58110313A JP11031383A JPH031386B2 JP H031386 B2 JPH031386 B2 JP H031386B2 JP 58110313 A JP58110313 A JP 58110313A JP 11031383 A JP11031383 A JP 11031383A JP H031386 B2 JPH031386 B2 JP H031386B2
- Authority
- JP
- Japan
- Prior art keywords
- copper
- rust preventive
- solution
- alcohol
- rust
- 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.)
- Expired - Lifetime
Links
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 26
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 24
- 239000010949 copper Substances 0.000 claims description 21
- 229910052802 copper Inorganic materials 0.000 claims description 20
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 230000003449 preventive effect Effects 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- BOSAWIQFTJIYIS-UHFFFAOYSA-N 1,1,1-trichloro-2,2,2-trifluoroethane Chemical compound FC(F)(F)C(Cl)(Cl)Cl BOSAWIQFTJIYIS-UHFFFAOYSA-N 0.000 claims description 6
- 125000003354 benzotriazolyl group Chemical class N1N=NC2=C1C=CC=C2* 0.000 claims description 5
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 4
- 239000012964 benzotriazole Substances 0.000 claims description 4
- 238000013020 steam cleaning Methods 0.000 claims description 3
- 238000011282 treatment Methods 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 230000002265 prevention Effects 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000000576 coating method Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 238000007772 electroless plating Methods 0.000 description 3
- 238000007602 hot air drying Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229920000768 polyamine Polymers 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/14—Nitrogen-containing compounds
- C23F11/149—Heterocyclic compounds containing nitrogen as hetero atom
-
- 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
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/28—Applying non-metallic protective coatings
- H05K3/282—Applying non-metallic protective coatings for inhibiting the corrosion of the circuit, e.g. for preserving the solderability
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
- Ceramic Capacitors (AREA)
- Manufacturing Of Printed Wiring (AREA)
Description
【発明の詳細な説明】
この発明は銅または銅合金の防錆処理方法に関
するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for rustproofing copper or copper alloys.
たとえば、セラミツクスなどの絶縁体の表面に
無電解メツキ法により銅被膜を形成し、この銅被
膜を導電部分とすることは知られている。このよ
うな例としては、セラミツクコンデンサの銅電極
回路基板の導電パターンなどへの応用がある。そ
して銅被膜はそのままでは酸化されやすい性質を
有しているため、通常防錆処理が施される。 For example, it is known that a copper coating is formed on the surface of an insulator such as ceramics by electroless plating, and this copper coating is used as a conductive portion. An example of this is application to a conductive pattern on a copper electrode circuit board of a ceramic capacitor. Since the copper coating has the property of being easily oxidized as it is, it is usually subjected to anti-corrosion treatment.
従来の防錆処理は次のようにして実施されてい
た。つまり、防錆剤であるベンゾトリアゾールま
たはベンゾトリアゾール誘導体を溶媒である水ま
たはアルコールに溶解し、この溶液に銅製品また
は銅合金製品を浸漬するか、または前記溶液を銅
製品または銅合金製品に吹き付け、塗布などの手
段で接触させることによつて防錆処理を行い、次
いで水またはアルコール類を除去し、さらに室温
乾燥や沸点以上の高温で乾燥していた。 Conventional rust prevention treatment was carried out as follows. In other words, benzotriazole or a benzotriazole derivative as a rust preventive agent is dissolved in water or alcohol as a solvent, and a copper product or copper alloy product is immersed in this solution, or the solution is sprayed onto the copper product or copper alloy product. Rust prevention treatment is carried out by contacting the material with means such as coating, water or alcohol is removed, and the material is dried at room temperature or at a high temperature above the boiling point.
しかしながら、このような方法によれば、溶媒
として高沸点のものを使用しているため、乾燥工
程において結露状態が実現されることになり、銅
製品または銅合金製品の表面に染みが発生した
り、アルコール濃度管理の不備によつて染みが発
生したりして外観不良を起こしていた。 However, according to this method, since a solvent with a high boiling point is used, dew condensation occurs during the drying process, and stains may occur on the surface of copper products or copper alloy products. Inadequate control of alcohol concentration caused stains and poor appearance.
また、この従来方法によれば、防錆処理後、い
わゆる水切り工程や熱風乾燥工程が必要となり、
これらの工程が入ることにより、一連の防錆処理
の自動化が行えなかつた。 In addition, according to this conventional method, a so-called draining process and hot air drying process are required after the rust prevention treatment.
Because of these steps, it was not possible to automate the series of rust prevention treatments.
したがつて、この発明は水切り工程や高温熱風
乾燥工程などが不要な銅または銅合金の防錆処理
方法を提供することを目的とする。 Therefore, it is an object of the present invention to provide a method for rustproofing copper or copper alloys that does not require a draining step or a high-temperature hot air drying step.
すなわち、この発明の要旨とするところは、溶
媒であるトリクロルトリフロロエタンとアルコー
ルの混合溶液に、防錆剤であるベンゾトリアゾー
ルまたはベンゾトリアゾール誘導体を飽和濃度以
下に溶解させて防錆溶液を作り、この防錆溶液と
銅または銅合金と接触させ、次いで防錆剤を含ま
ない前記溶媒の混合溶液で濯ぎ、さらに低沸点の
前記溶媒の混合溶液にて蒸気洗浄することを特徴
とする銅または銅合金の防錆処理方法である。 That is, the gist of the present invention is to prepare a rust preventive solution by dissolving benzotriazole or a benzotriazole derivative, which is a rust preventive agent, in a mixed solution of trichlorotrifluoroethane, a solvent, and alcohol, to a concentration below saturation. The copper or copper alloy is brought into contact with the rust preventive solution, and then rinsed with a mixed solution of the above solvent that does not contain a rust preventive agent, and further steam-cleaned with a mixed solution of the above solvent with a low boiling point. This is an anti-rust treatment method for alloys.
ここで、防錆処理の対象である銅または銅合金
としては、
セラミツクス、プラスチツクなどの非処理物
に電解メツキまたは無電解メツキにより形成さ
れた銅または銅合金被膜
銅または銅合金そのものからなるものなどが
ある。 Here, the copper or copper alloy that is subject to rust prevention treatment includes copper or copper alloy coatings formed by electroplating or electroless plating on non-treated materials such as ceramics and plastics, copper or copper alloys themselves, etc. There is.
そして、の銅または銅合金は通常湿式で処理
されるため水分を含んでおり、水置換乾燥ととも
に、防錆処理が必要とされる。 Since copper or copper alloys are usually processed wet, they contain moisture, and require rust prevention treatment as well as water displacement drying.
またの銅または銅合金は水を含んでいない
が、高温の熱処理を経るため、表面が非常に化学
的活性を有しており、放置すると大気中の湿気に
より酸化が急激に進行することになり、やはり防
錆処理が必要とされる。 Copper or copper alloys do not contain water, but because they undergo high-temperature heat treatment, their surfaces are extremely chemically active, and if left untreated, oxidation will progress rapidly due to atmospheric moisture. However, rust prevention treatment is still required.
溶媒であるトリクロルトリフロロエタンとアル
コールの混合溶液は、アルコール含有量を共沸点
温度以下で混合したものが使用される。 A mixed solution of trichlorotrifluoroethane and alcohol, which is a solvent, is used in which the alcohol content is mixed at a temperature below the azeotropic point.
また、防錆剤としはベンゾトリアゾールまたは
その誘導体が使用される。ベンゾトリアゾールの
誘導体としては、たとえばポリアミン誘導体があ
る。 Furthermore, benzotriazole or a derivative thereof is used as a rust preventive agent. Examples of benzotriazole derivatives include polyamine derivatives.
この発明方法によれば、溶媒としてトリクロル
トリフロロエタンとアルコールの混合溶液を用い
るため、従来のように水または水を含むアルコー
ルからなる溶媒で処理したものにくらべ酸化を促
進する要素を含んでおらず、したがつて酸化や表
面の染みの発生が認められない。 According to the method of this invention, since a mixed solution of trichlorotrifluoroethane and alcohol is used as a solvent, it does not contain elements that promote oxidation compared to conventional treatments using water or a solvent consisting of water-containing alcohol. Therefore, no oxidation or surface stains are observed.
また、この発明方法によれば、従来のように水
や水を含むアルコールを溶媒として用いた場合、
水切り工程や高温熱風乾燥処理が必要であつた
が、このような工程が省略でき、連続して防錆処
理が実現でき、防錆処理の自動化が容易に実現す
ることができる。 Furthermore, according to the method of this invention, when water or an alcohol containing water is used as a solvent as in the past,
Although a draining process and a high-temperature hot air drying process were required, these processes can be omitted, rust prevention treatment can be carried out continuously, and automation of rust prevention treatment can be easily realized.
さらに、従来方法によれば、水または水を含む
アルコールが汚染されたとき、廃液処理が必要で
あつたが、この発明方法のようにトリクロルトリ
フロロエタンとアルコールの混合溶液を用いるこ
とによつて、蒸気再生が可能となり、大幅な節水
ができることになる。 Furthermore, according to the conventional method, waste liquid treatment was required when water or alcohol containing water was contaminated, but by using a mixed solution of trichlorotrifluoroethane and alcohol as in the method of the present invention, , steam regeneration becomes possible, resulting in significant water savings.
さらに、また、この発明方法においては、防錆
溶液と銅または銅合金を接触させたのち、防錆剤
を含まない混合溶媒でリンス処理を施し、さらに
低沸点の混合溶媒にて蒸気洗浄するが、この低沸
点の混合溶媒は沸点が50℃以下に設定される。し
たがつて、蒸気洗浄を低温で実施でき、防錆処理
対象である銅または銅合金の酸化も防止すること
ができる。 Furthermore, in the method of the present invention, after bringing the rust preventive solution into contact with copper or copper alloy, rinsing treatment is performed with a mixed solvent that does not contain a rust preventive agent, and further steam cleaning is performed with a low boiling point mixed solvent. The boiling point of this low boiling point mixed solvent is set to 50°C or lower. Therefore, steam cleaning can be performed at low temperatures, and oxidation of the copper or copper alloy to be treated for rust prevention can also be prevented.
以下、この発明を実施例に従つて詳細に説明す
る。 Hereinafter, this invention will be explained in detail according to examples.
実施例 １
処理対象品として、セラミツクスの表面に銅の
無電解メツキ被膜を形成したものを準備し、さら
にメツキ処理後水洗した。Example 1 A product to be treated was prepared by forming a copper electroless plating film on the surface of ceramics, which was further washed with water after the plating treatment.
一方、ベンゾトリアゾールのポリアミン誘導体
をトリクロルトリフロロエタンとアルコールの共
沸点混合溶液に20％加えて防錆溶液を作つた。こ
の防錆溶液に上記セラミツクスを浸漬した。ここ
で、浸漬の他、吹き付け、筆塗などで接触させて
もよい。そののち防錆溶液からセラミツクスを引
き上げ、さらに防錆剤を含まない前記溶媒の混合
溶液で濯いだ。次いで低沸点（45℃）の前記溶媒
の混合溶媒にて蒸気洗浄した。 On the other hand, a rust preventive solution was made by adding 20% of a polyamine derivative of benzotriazole to an azeotropic mixed solution of trichlorotrifluoroethane and alcohol. The above ceramics were immersed in this antirust solution. Here, in addition to dipping, contact may be made by spraying, brush painting, or the like. Thereafter, the ceramics were removed from the rust preventive solution and further rinsed with a mixed solution of the above solvents that did not contain a rust preventive agent. Next, it was steam-cleaned using a mixed solvent of the above-mentioned solvents having a low boiling point (45°C).
このようにして処理したセラミツクス表面の銅
の無電解メツキ被膜を観察したところ、染みの発
生は見られなかつた。また処理後1000時間空気中
に放置したところ、酸化現象の発生は見られなか
つた。 When the electroless copper plating film on the surface of the ceramic thus treated was observed, no staining was observed. Further, when the sample was left in the air for 1000 hours after treatment, no oxidation phenomenon was observed.
実施例 ２
この実施例では処理対象品として銅線を選ん
だ。Example 2 In this example, copper wire was selected as the product to be treated.
この銅線は特性改善のために100℃以上の温度
で熱処理工程に付されるが、この実施例では200
℃で熱処理したものを用いた。 This copper wire is subjected to a heat treatment process at a temperature of 100℃ or higher to improve its characteristics, but in this example
The one heat-treated at ℃ was used.
この銅線をすでに上記した実施例１と同様にし
て処理した。得られた銅線の表面を観察したとこ
ろ、染みの発生は見られなかつた。また処理後
1000時空気中に放置したところ、酸化現象の発生
は認められなかつた。 This copper wire was treated in the same manner as in Example 1 above. When the surface of the obtained copper wire was observed, no stains were observed. Also after processing
When it was left in the air for 1000 hours, no oxidation phenomenon was observed.
Claims (1)
ルコールの混合溶液に、防錆剤であるベンゾトリ
アゾールまたはベンゾトリアゾール誘導体を飽和
濃度以下に溶解させて防錆溶液を作り、この防錆
溶液と銅または銅合金と接触させ、次いで防錆剤
を含まない前記溶媒の混合溶液で濯ぎ、さらに低
沸点の前記溶媒の混合溶液にて蒸気洗浄すること
を特徴とする銅または銅合金の防錆処理方法。1. A rust preventive solution is prepared by dissolving benzotriazole or a benzotriazole derivative, which is a rust preventive agent, in a mixed solution of trichlorotrifluoroethane and alcohol to a saturation concentration or less, and this rust preventive solution is mixed with copper or copper alloy. 1. A method for rust-preventing copper or copper alloys, which comprises bringing them into contact with each other, followed by rinsing with a mixed solution of the above-mentioned solvents that does not contain a rust preventive agent, and further steam cleaning with a mixed solution of the above-mentioned solvents having a low boiling point.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58110313A JPS602681A (en) | 1983-06-16 | 1983-06-16 | Rust preventive treatment of copper or copper alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58110313A JPS602681A (en) | 1983-06-16 | 1983-06-16 | Rust preventive treatment of copper or copper alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS602681A JPS602681A (en) | 1985-01-08 |
| JPH031386B2 true JPH031386B2 (en) | 1991-01-10 |
Family
ID=14532540
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58110313A Granted JPS602681A (en) | 1983-06-16 | 1983-06-16 | Rust preventive treatment of copper or copper alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS602681A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61287155A (en) * | 1985-06-14 | 1986-12-17 | Hitachi Ltd | Semiconductor device |
| JPH0878281A (en) * | 1994-09-05 | 1996-03-22 | Matsushita Electric Ind Co Ltd | Electronic component manufacturing method |
| US7264740B2 (en) * | 2003-03-28 | 2007-09-04 | David Hughes Horne | Process for increasing strength, flexibility and fatigue life of metals |
| CN102064020B (en) * | 2010-10-28 | 2012-04-25 | 吴浩 | Manufacturing method of terminal electrode of microwave high-frequency capacitor |
| JP6848243B2 (en) * | 2016-07-25 | 2021-03-24 | 住友金属鉱山株式会社 | Manufacturing method of conductive substrate |
-
1983
- 1983-06-16 JP JP58110313A patent/JPS602681A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS602681A (en) | 1985-01-08 |
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