JPS6026675A - Etching solution - Google Patents
Etching solutionInfo
- Publication number
- JPS6026675A JPS6026675A JP13457783A JP13457783A JPS6026675A JP S6026675 A JPS6026675 A JP S6026675A JP 13457783 A JP13457783 A JP 13457783A JP 13457783 A JP13457783 A JP 13457783A JP S6026675 A JPS6026675 A JP S6026675A
- Authority
- JP
- Japan
- Prior art keywords
- etching
- concd
- time
- soln
- hydrochloric acid
- 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
Links
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
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明はコンピュータデークや音楽、映像情報を磁気記
録によって行なう記録媒体の製造過程中に用い、金属膜
の厚みを容易に測定する際に用いられるエツチング溶液
に関するものである。[Detailed Description of the Invention] Industrial Application Field The present invention is an etching method used during the manufacturing process of recording media for recording computer disks, music, and video information by magnetic recording, and used to easily measure the thickness of metal films. It concerns solutions.
従来例の構成とその問題点
近年磁気記録は大きな発展を示し、テープやシート、固
定ディスクなどの形状の媒体が使用されている。一般に
は、残溜磁化を保つ磁性粉(フェライトや鉄系金属粉末
)を樹脂などのバインダーにより高分子フィルムや金属
非磁性盤上に塗布したものが用いられてきた。最近では
より高密度記録への要求から、磁性層に金属薄膜を真空
中などで直接積層した媒体が用いられるようになり、一
部Co−Ni 、 Co−P系は市販されている。又、
開発中の磁性材料としてco、l!:Crの合金を薄膜
積層した媒体が提言されており、高密度化への要求から
膜厚も1ミクロン以下の構成になっている。媒体の製造
上はこの膜厚を精度良く測定することが要求され、針接
触による触針測定が行われるか、Co−Cr の合金に
関しては、その耐候性が強く耐酸、耐アルカリ性が強い
故に、膜厚計測時のエツチングが通常用いられる溶液で
は非常に時間がかXシ、又きれいな溶解面が得られ難く
て、正確な膜厚測定が困難であった。Conventional configurations and their problems Magnetic recording has made great progress in recent years, and media in the form of tapes, sheets, fixed disks, etc. are being used. Generally, magnetic powder (ferrite or iron-based metal powder) that maintains residual magnetization has been applied to a polymer film or metal nonmagnetic disk using a binder such as resin. Recently, due to the demand for higher density recording, media in which a thin metal film is directly laminated on the magnetic layer in a vacuum or the like have been used, and some Co--Ni and Co--P systems are commercially available. or,
co, l! as magnetic materials under development! A medium in which a thin film of a Cr alloy is laminated has been proposed, and due to the demand for high density, the film thickness has become 1 micron or less. In the production of media, it is necessary to accurately measure this film thickness, and stylus measurement is performed using needle contact.As for Co-Cr alloys, because of their strong weather resistance and strong acid and alkali resistance, Etching when measuring the film thickness is very time-consuming with the solution normally used, and it is difficult to obtain a clean dissolution surface, making it difficult to accurately measure the film thickness.
発明の目的
本発明は、上記のC,o −Cr合金薄膜の膜厚測定を
容易、かつ正確に行うため、触剣法利用時の膜面エツチ
ングを容易に行なえる新規なエツチング液を提供するこ
とを目的とする。OBJECTS OF THE INVENTION The present invention provides a novel etching solution that allows easy etching of the film surface when using the tactile method, in order to easily and accurately measure the thickness of the C,o-Cr alloy thin film described above. With the goal.
発明の構成
本発明は上記目的を達成するもので、濃塩酸(1oN)
と濃硝酸(1oN )の混合比率を、塩酸50%から2
5%までの範囲に保った混合物からなる溶液によって、
Coと0を主成分とする合金を腐蝕溶解することを特徴
とするエツチング溶液を提供するものである。Structure of the Invention The present invention achieves the above object, and uses concentrated hydrochloric acid (1oN).
The mixing ratio of nitric acid and concentrated nitric acid (1oN) was changed from 50% hydrochloric acid to 2
By a solution consisting of a mixture kept in the range of up to 5%
The present invention provides an etching solution that corrodes and dissolves an alloy whose main components are Co and O.
実施例の説明
Co−Cr合金系に対する腐蝕性の強い酸を選定する目
的で以下の酸と組合わせ配合につきエツチングテストを
行った。1oN−HCl、 1N−HCl。Description of Examples In order to select an acid that is highly corrosive to the Co--Cr alloy system, an etching test was conducted on the following acids and combinations. 1oN-HCl, 1N-HCl.
1oN−HNO3,1N−HNO3,1oN−H2SO
4゜1N H2SO2,150″cHP O4、1N
N a OH+HCl−HNO3系、HCl−)(2S
o4系、HCl−HPO4系、HNO3−H2SO4系
。これらのテストの中で最もエツチング効果のあったの
は塩酸が強く、中でも塩酸と硝酸の混合溶液であった。1oN-HNO3, 1N-HNO3, 1oN-H2SO
4゜1N H2SO2, 150″cHP O4, 1N
Na OH+HCl-HNO3 system, HCl-) (2S
o4 system, HCl-HPO4 system, HNO3-H2SO4 system. Among these tests, the one with the strongest etching effect was hydrochloric acid, especially a mixed solution of hydrochloric acid and nitric acid.
そこで塩酸と硝酸との混合液の配分によるエツチング効
果を調べる目的で、以下のテストを行った。検査試料は
、C0−ClのCr10〜30重量パーセントの合金を
RFスパッタ及びDCスパッタリングで表面の平坦な高
分子フィルム上に積層し、フィルムの一部をビニールテ
ープ又はセロファンテープにておおい、エツチング溶液
に含浸する。目視によりCo−Cr金属面が溶解するの
を、テープでかXっだ部分と対比しながら確認し、その
時までの経過時間を図に示す、縦軸はエツチング時間、
横軸は混合後の経過時間である。図において1は塩酸:
硝酸の混合比率が3:1(塩酸75係)のもの、以下そ
れぞれ、2は1: 1 (50%)、3は1:2(33
%)、4は1:3(25係)、5は1:4(20%)の
混合比率のものである。Therefore, in order to investigate the etching effect of the distribution of a mixed solution of hydrochloric acid and nitric acid, the following test was conducted. The test sample was prepared by laminating a C0-Cl alloy containing 10 to 30 weight percent Cr on a polymer film with a flat surface by RF sputtering and DC sputtering, covering a part of the film with vinyl tape or cellophane tape, and applying an etching solution. Impregnate. The melting of the Co-Cr metal surface was visually confirmed by comparing it with the large X-shaped part of the tape, and the elapsed time up to that point is shown in the figure. The vertical axis is the etching time;
The horizontal axis is the elapsed time after mixing. In the figure, 1 is hydrochloric acid:
The mixing ratio of nitric acid is 3:1 (hydrochloric acid 75 parts), below, 2 is 1:1 (50%), 3 is 1:2 (33
%), 4 has a mixing ratio of 1:3 (25 parts), and 5 has a mixing ratio of 1:4 (20%).
図から明らかなように、混合比率3:1(1)のものは
、混合後の経過時間とともにだらだらとエツチング時間
が短かぐなっているが、エツチング時間が、1分以上で
エンチングできた膜の溶解端は、テープ端の通りでなく
、溶解面の段差が急激でないため、接針法による膜厚測
定の精度が悪くなった。この混合比率では、所定のエツ
チング能力を発揮するまでに時間がかかるという欠点を
有している。As is clear from the figure, the etching time of the mixture with a mixing ratio of 3:1 (1) gradually decreases as time elapses after mixing, but the etching time of the film that was etched in 1 minute or more was longer. The melting edge did not follow the tape edge and the steps on the melting surface were not sharp, so the accuracy of film thickness measurement by the contact method was poor. This mixing ratio has the disadvantage that it takes time to achieve a predetermined etching ability.
混合比率1 :1 (2)のものは、溶液作製後、約8
分でエツチング時間が30秒となり、この時にエツチン
グした膜の端面はすっばりと切れている。この溶液は、
24時間経過後も十分なエツチング能力を持っているこ
とも確認できた。The mixture ratio of 1:1 (2) is approximately 8% after the solution is prepared.
The etching time becomes 30 seconds, and the end face of the etched film is sharply cut at this time. This solution is
It was also confirmed that sufficient etching ability was maintained even after 24 hours had passed.
混合比率1:2(3)および混合比率1:3(4)のも
のについても、それぞれ、3では9分で、4では6分で
、エツチング時間が30秒となっておシ、3のものでは
9分、4のものでは5分経過した溶液でエツチングした
膜の溶解端は、すっばりと切れている。For the mixture ratio 1:2 (3) and the mixture ratio 1:3 (4), the etching time was 9 minutes for 3 and 6 minutes for 4, and the etching time was 30 seconds. The dissolution edge of the film etched with the solution after 9 minutes in case No. 4 and 5 minutes after etching in case No. 4 is sharply cut.
混合比率1 :4(5)のものでは、混合直後ではエツ
チング時間が他の例に比べて、比較的短がいが、その後
、時間経過しても、はとんど変化なぐ1最も短いエツチ
ング時間でも35秒程度で、10分以上経過すると、逆
にエツチング能力が落ちてしまう。In the case of a mixture ratio of 1:4(5), the etching time is relatively short immediately after mixing compared to other examples, but after that, the etching time remains almost unchanged even after the passage of time.1 The shortest etching time However, if it takes about 35 seconds or more than 10 minutes, the etching ability will decrease.
以上のように、濃塩酸(1ON)と濃硝酸(1oN)の
混合比率を1:1〜1:3にした混合液は、C0−Or
合金薄膜のエツチングした場合、混合液作成後5分経過
後から、溶解でき、その溶解端も段差がきれいにでき、
触針法による薄膜測定が正確にできるという特徴を有し
ている。As mentioned above, the mixed liquid containing concentrated hydrochloric acid (1ON) and concentrated nitric acid (1oN) at a mixing ratio of 1:1 to 1:3 is C0-Or
When etching a thin alloy film, it can be melted 5 minutes after the mixture is prepared, and the melted edge has a clean step.
It is characterized by the ability to accurately measure thin films using the stylus method.
なお上記実施例はCo 、!: Or金合金場合につい
て述べたが、本発明のエツチング溶液は、Co 、 C
rを主成分とする合金であればよく、Co、Cr微量た
とえば0.1 %以下ノCu 、 S i 、 AI
、 Ca 、 Mg 。Note that the above example uses Co,! :Although the case of Or gold alloy has been described, the etching solution of the present invention can be used for Co, C
Any alloy containing r as a main component may be used, with a trace amount of Co, Cr, for example 0.1% or less, Cu, Si, AI.
, Ca, Mg.
Mn等を添加したものに訃いても同様の効果を奏する。A similar effect can be obtained even if Mn or the like is added.
発明の効果
以上要するに本発明は、濃塩酸(1ON)と濃硝酸(1
ON)の混合比率を1:1〜1:3の範囲とした、Co
Crを主成分とする合金を腐蝕溶解させるエツチング溶
液を提供するもので混合液作成後5分経過すれば、1分
以内で1μm程度の薄膜が溶解可能となり、又、この効
果は1時間以上〜1昼夜程続くので、す早いデータの収
集ができる。又、30秒程度ご溶解できるエツチング液
で断面を作ったCoCrの端部は、段差が明確にできて
分り、触針法によるデータも正確に得られるという効果
も有している。Effects of the Invention In short, the present invention provides concentrated hydrochloric acid (1ON) and concentrated nitric acid (1ON).
ON) with a mixing ratio of 1:1 to 1:3.
This product provides an etching solution that corrodes and dissolves alloys whose main component is Cr.If 5 minutes have passed after preparing the mixed solution, a thin film of about 1 μm can be dissolved within 1 minute, and this effect remains for more than 1 hour. Since it lasts about one day and night, data can be collected quickly. In addition, the edge of CoCr whose cross section is made with an etching solution that can be dissolved for about 30 seconds has the effect of clearly forming a step and making it possible to accurately obtain data using the stylus method.
図は、RFスパッタリングでポリエステル膜」−に積層
したCo−’Cr合金約0.5μmのエツチング時間を
、溶液混合後の経過時間の関数として表示した図である
。The figure shows the etching time of approximately 0.5 μm of a Co-'Cr alloy deposited on a polyester film by RF sputtering as a function of the elapsed time after solution mixing.
Claims (1)
塩酸50%から25%までの範囲に保った混合物からな
る溶液によって、COとCrを主成分とする合金を腐蝕
溶解することを特徴とするエツチング溶液。The mixing ratio of concentrated hydrochloric acid (1oN) and concentrated nitric acid (1oN) is
An etching solution characterized in that an alloy containing CO and Cr as main components is corroded and dissolved by a solution consisting of a mixture of hydrochloric acid kept in a range of 50% to 25%.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP13457783A JPS6026675A (en) | 1983-07-22 | 1983-07-22 | Etching solution |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP13457783A JPS6026675A (en) | 1983-07-22 | 1983-07-22 | Etching solution |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS6026675A true JPS6026675A (en) | 1985-02-09 |
Family
ID=15131603
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP13457783A Pending JPS6026675A (en) | 1983-07-22 | 1983-07-22 | Etching solution |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS6026675A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2022513244A (en) * | 2018-12-14 | 2022-02-07 | テック メット インコーポレイテッド | Cobalt chrome etching method |
-
1983
- 1983-07-22 JP JP13457783A patent/JPS6026675A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2022513244A (en) * | 2018-12-14 | 2022-02-07 | テック メット インコーポレイテッド | Cobalt chrome etching method |
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