JPH01129982A - Recycling method and etching method of ferric chloride etchant - Google Patents

Recycling method and etching method of ferric chloride etchant

Info

Publication number
JPH01129982A
JPH01129982A JP28793487A JP28793487A JPH01129982A JP H01129982 A JPH01129982 A JP H01129982A JP 28793487 A JP28793487 A JP 28793487A JP 28793487 A JP28793487 A JP 28793487A JP H01129982 A JPH01129982 A JP H01129982A
Authority
JP
Japan
Prior art keywords
etchant
etching
ferric chloride
chloride etchant
etching method
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
JP28793487A
Other languages
Japanese (ja)
Inventor
Tsukasa Chiba
千葉 司
Minoru Manome
馬目 稔
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.)
Hitachi Cable Ltd
Original Assignee
Hitachi Cable 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 Hitachi Cable Ltd filed Critical Hitachi Cable Ltd
Priority to JP28793487A priority Critical patent/JPH01129982A/en
Publication of JPH01129982A publication Critical patent/JPH01129982A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-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
    • C23F1/00Etching metallic material by chemical means
    • C23F1/46Regeneration of etching compositions

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)

Abstract

(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。
(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】 [発明の対象] 本発明は、塩化第2鉄エッチャントの再生方法とエツチ
ング方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] The present invention relates to a method for regenerating and etching a ferric chloride etchant.

[従来の技術] 老化した塩化第2鉄エッチャントを再生する方法として
は、過酸化水素や次亜塩素酸ナトリウム等の酸化剤を添
加する方法、又は、塩素ガスと接触させる方法、或いは
、電解による方法がある。
[Prior Art] Methods for regenerating aged ferric chloride etchant include adding an oxidizing agent such as hydrogen peroxide or sodium hypochlorite, contacting it with chlorine gas, or electrolysis. There is a way.

過酸化水素を添加する方法は、反応効率が悪く、目的と
する再生を行うためには、多量に添加しなければならな
い。従って、エッチエンドはかなり希釈されること叫な
り、エツチング性能に悪影響を及ぼすので好ましくない
。コスト的にもかなり問題の多い方法である。
The method of adding hydrogen peroxide has poor reaction efficiency, and a large amount must be added in order to achieve the desired regeneration. Therefore, the etch end is likely to be considerably diluted, which is undesirable since it will adversely affect etching performance. This method is quite problematic in terms of cost.

次亜塩素酸ナトリウムを用いる方法は、濃厚溶液で添加
すると塩素ガスを発生させるため、危険である。従って
、希釈した状態で添加しなければならず過酸化水素の場
合と同様エッチャントを希釈するという問題がある。又
、食塩が蓄積するので繰返し再生する方法には不都合で
ある。
The method of using sodium hypochlorite is dangerous because it generates chlorine gas when added as a concentrated solution. Therefore, the etchant must be added in a diluted state, resulting in the problem of diluting the etchant as in the case of hydrogen peroxide. In addition, salt accumulates, which is inconvenient for repeated regeneration methods.

同様に塩素酸ソーダ等の塩素酸塩を用いる方法もアルカ
リ塩類の蓄積の点で好ましくない。
Similarly, a method using a chlorate such as sodium chlorate is also unfavorable in terms of accumulation of alkali salts.

以上の通り、薬品を用いて酸化再生づる方法は、本発明
で目的とする再生装置と、エツチング装置とを接続し連
続的にエッチャントを再生して利用する方法には不向き
である。
As described above, the method of oxidation regeneration using chemicals is not suitable for the method of the present invention, in which a regeneration device and an etching device are connected to continuously regenerate and utilize the etchant.

塩素ガスを用いて再生する方法は、最も効率がよく化学
反応的には理想的な方法であるが、塩素ガスは非常に有
害であり、作業環境や公害上問題がある。
Although the regeneration method using chlorine gas is the most efficient and ideal method in terms of chemical reactions, chlorine gas is extremely harmful and poses problems in terms of the working environment and pollution.

電解法は、以上説明した方法の様な問題点がなく、しか
もエツチングで溶解させた金属を析出°、分離でき再生
という点からは理想的な方法であるが、安定性に欠ける
ため保守管理に問題が生じ実用されていないのが現状で
ある。
The electrolytic method does not have the problems of the methods explained above, and it is an ideal method in terms of regeneration because it allows the metal dissolved by etching to be precipitated and separated, but it lacks stability and is difficult to maintain. Currently, there are problems and it is not put into practical use.

従来の再生方法を述べてきたが、連続的にしがも安全に
エッチャントを再生してエツチング装置に供給し環境使
用には何れの方法にも問題がある。
Although conventional regeneration methods have been described, there are problems with any of the methods when it comes to continuously and safely regenerating the etchant and supplying it to an etching device for environmental use.

[発明の目的] 本発明は、前記した従来方法の欠点を解消し、安価に且
つ安全にエッヂヤントを再生する方法とそれを利用した
エツチング方法を提供することにある。
[Object of the Invention] An object of the present invention is to eliminate the drawbacks of the conventional methods described above, and to provide a method for inexpensively and safely regenerating an edger, and an etching method using the method.

[発明の要点] 本発明の要旨は、塩化第2鉄エッチャントを再生する方
法として硝酸の存在下で空気酸化を利用することにある
Summary of the Invention The summary of the invention is to utilize air oxidation in the presence of nitric acid as a method to regenerate ferric chloride etchant.

それによって安全上不備な問題がなく良好な性状のエッ
チャントを再生して循環使用を可能にさせたものである
As a result, an etchant with good properties without any safety issues can be regenerated and recycled.

硝酸の添加量は、特に規定するものではないが、微量で
あれば触媒効果が弱く、人情であればレジストによって
は損傷する可能性があり、ニッケル等の不導体を形成す
る金属を含むものは、エツチング性の影響を及ぼす。
The amount of nitric acid added is not particularly specified, but if it is in a small amount, the catalytic effect will be weak, and if it is humane, it may damage some resists. , affects etching properties.

常識的には、エッヂヤント中の鉄分1 K9に対し硝酸
根濃度として5〜500gが適当と考えられる範囲であ
る。
Common sense suggests that a range of 5 to 500 g of nitrate radicals is considered to be appropriate for 1 K9 of iron in edgeants.

空気酸化は、温度が75〜80℃が効率がよく望ましい
範囲であるが、循環経路の配管域は、ポンプ等の耐熱性
が制約を受ける。−膜内には、高密度ポリエチレンの耐
熱性の50〜70℃に限定されるが、場合によっては、
チタン等の高耐腐食性材料或いは、テフ1」ン等の高熱
高耐薬品性の有機物を循環経路に使用する配管等の内面
にライニングしたものを用い、空気酸化温度を高くする
ことも可能である。
For air oxidation, a temperature range of 75 to 80° C. is efficient and desirable, but the heat resistance of pumps and the like is limited in the piping area of the circulation route. - Inside the membrane, the heat resistance of high-density polyethylene is limited to 50-70°C, but in some cases,
It is also possible to increase the air oxidation temperature by lining the inner surface of the piping used in the circulation route with a highly corrosion-resistant material such as titanium or an organic material with high heat and high chemical resistance such as Teflon. be.

[実 施 例] 第1図は、本発明のエツチング方法を示す系統図であり
、1は空気酸化装置本体、1aはミスト除去装置、1b
はスプレー、1Cは充填物、1dは送風機、1eは送風
管、1fは保温材、2は薬品添加槽本体、2eは撹拌機
、2bは酸化還元電位計、2Cは比重測定センサー、2
dは酸濃度測定電位計、2eは薬品供給管、3はエツチ
ング装置、4はポンプ、5は輸送管である。
[Example] Fig. 1 is a system diagram showing the etching method of the present invention, in which 1 is an air oxidizer main body, 1a is a mist removal device, and 1b is a system diagram showing the etching method of the present invention.
is a spray, 1C is a filling material, 1d is a blower, 1e is a blower pipe, 1f is a heat insulator, 2 is a chemical addition tank body, 2e is a stirrer, 2b is an oxidation-reduction electrometer, 2C is a specific gravity measurement sensor, 2
d is an electrometer for measuring acid concentration, 2e is a chemical supply pipe, 3 is an etching device, 4 is a pump, and 5 is a transport pipe.

第1図において、空気酸化装置本体1は、スプレー1b
、及び、充填物1Cから成り、それに、送風機1d、送
風管1e、ミスト除去装置1a、及び、ポンプ4から構
成される。ポンプ4は、10Kyf/aAの圧力で50
1!/win(7)輸送能力を持ち、エッチャントをス
プレー1bから賞状にエッヂヤントを噴震する。
In FIG. 1, the air oxidizer main body 1 includes a sprayer 1b
, a filling material 1C, and a blower 1d, a blower pipe 1e, a mist removing device 1a, and a pump 4. Pump 4 has a pressure of 50Kyf/aA.
1! /win (7) Has the ability to transport and ejects the etchant from spray 1b to the award certificate.

エッチャントの温度は60℃である。送[41111d
が1 m3/1linの割合で空気を送り込みエッチャ
ントを酸化させる。酸化したエッチャントは薬品添加槽
2に移され酸化還元電位計2b、比重測定センサー2c
、酸濃度測定電位計2dで測定された値を基に薬品供給
管2eから自動的に適切な塩酸、水が加えられる。
The temperature of the etchant is 60°C. Sending [41111d
Air is sent in at a rate of 1 m3/1 lin to oxidize the etchant. The oxidized etchant is transferred to the chemical addition tank 2, and the oxidation-reduction potentiometer 2b and specific gravity measurement sensor 2c
, appropriate hydrochloric acid and water are automatically added from the chemical supply pipe 2e based on the value measured by the acid concentration measuring electrometer 2d.

硝酸は、化、学分析によりエッチャントの鉄分1Kgに
対し30〜50gになるように制約され薬品添加槽2内
は撹拌機2aで掻き混ぜられている。
The amount of nitric acid is limited by chemical and chemical analysis to 30 to 50 g per 1 kg of iron in the etchant, and the inside of the chemical addition tank 2 is stirred by a stirrer 2a.

薬品添加されたエッチャントは輸送管5を通ってエツチ
ング装置3に流入し、ポンプ4によって再び、空気酸化
装置1のスプレー1bへと循環する。
The chemically added etchant flows into the etching device 3 through the transport pipe 5 and is circulated again by the pump 4 to the spray 1b of the air oxidizer 1.

以上説明した条件で、エッチャントへの溶解債が200
0/hou rの速度で鉄58%、ニッケル42%の合
金製リードフレームを連続してエツチングした時、エッ
チャントの老化度(エッチャント中の全鉄で2価の鉄を
除いた数)が0.12〜0.13の範囲に保つことがで
き、十分な実用性が認められた。硝酸を加えない場合は
老化度が上昇し、前記の老化度に保つことが出来ない。
Under the conditions explained above, the dissolution bond to the etchant is 200
When a lead frame made of an alloy made of 58% iron and 42% nickel was continuously etched at a speed of 0/hour, the degree of aging of the etchant (the total number of iron in the etchant excluding divalent iron) was 0. It was possible to maintain the value within the range of 12 to 0.13, and sufficient practicality was recognized. If nitric acid is not added, the degree of aging increases and it is not possible to maintain the above degree of aging.

本実施例において、薬品添加槽2をエツチング装置3の
前に配置したがエツチング装置3の後でも差支えない。
In this embodiment, the chemical addition tank 2 is placed before the etching device 3, but it may also be placed after the etching device 3.

[発明の効果] 本発明により、アルカリ金属のようなエツチングを妨害
する物質を存在させることなく、塩化第2鉄の濃度を一
定に保つ条件でエツチングすることが可能なしかも安全
なエツチング方法が確立される。
[Effects of the Invention] The present invention establishes a safe etching method that allows etching to be carried out under conditions where the concentration of ferric chloride is kept constant without the presence of substances that interfere with etching such as alkali metals. be done.

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

第1図は、本発明のエツチング方法の系統図である。 1:空気酸化装置本体、 1a:ミスト除去装置、 1bニスプレー、 1C;充填物、 d:送風機、 1e:送風管、 1f:保温材、 2:薬品添加槽本体、 2a:撹拌機、 2b:酸化還元電位計、 2C:比重測定センサー、 2d:酸濃度測定電位計、 2e:薬品供給管、 3:エッチ、ヤング装置、 4:ポンプ、 5:輸送管。 FIG. 1 is a systematic diagram of the etching method of the present invention. 1: Air oxidizer main body, 1a: Mist removal device, 1b Nispray, 1C; filling, d: blower, 1e: Air pipe, 1f: Heat insulation material, 2: Chemical addition tank body, 2a: Stirrer, 2b: redox electrometer, 2C: specific gravity measurement sensor, 2d: acid concentration measuring electrometer, 2e: Chemical supply pipe, 3: Etch, Young device, 4: Pump, 5: Transport pipe.

Claims (2)

【特許請求の範囲】[Claims] (1)塩化第2鉄エッチャントに硝酸根が存在する状態
で、空気酸化により再生することを特徴とする塩化第2
鉄エッチャントの再生方法。
(1) Ferric chloride, which is characterized by being regenerated by air oxidation in the presence of nitrate radicals in the ferric chloride etchant.
How to regenerate iron etchant.
(2)前記方法による再正装置とエッチング装置とを組
み合わせてエッチャントの老化度が一定の範囲に保持で
きる装置を使用することを特徴とするエッチング方法。
(2) An etching method characterized by using a device that can maintain the degree of aging of the etchant within a certain range by combining a reconditioning device according to the method described above and an etching device.
JP28793487A 1987-11-13 1987-11-13 Recycling method and etching method of ferric chloride etchant Pending JPH01129982A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP28793487A JPH01129982A (en) 1987-11-13 1987-11-13 Recycling method and etching method of ferric chloride etchant

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP28793487A JPH01129982A (en) 1987-11-13 1987-11-13 Recycling method and etching method of ferric chloride etchant

Publications (1)

Publication Number Publication Date
JPH01129982A true JPH01129982A (en) 1989-05-23

Family

ID=17723624

Family Applications (1)

Application Number Title Priority Date Filing Date
JP28793487A Pending JPH01129982A (en) 1987-11-13 1987-11-13 Recycling method and etching method of ferric chloride etchant

Country Status (1)

Country Link
JP (1) JPH01129982A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6210650B1 (en) * 1993-07-21 2001-04-03 Andritz-Patentverwaltungs-Gesellschaft M.B.H Process for regenerating hydrochloric acid from pickling plants

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6210650B1 (en) * 1993-07-21 2001-04-03 Andritz-Patentverwaltungs-Gesellschaft M.B.H Process for regenerating hydrochloric acid from pickling plants

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