JPWO2019073819A1 - How to peel off adhered metal from metal plate - Google Patents
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- 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
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract
平坦な直流電圧を用いた電解装置によって金属板に付着した金属を剥離する方法であって、金属が付着した金属板を電解液に浸漬した後、該金属板を陽極として、陽極電位を０．１〜３．０Ｖ（Ａｇ／ＡｇＣｌ参照電極）の条件で電解することにより、該付着金属を金属板から剥離することを特徴とする金属板から付着金属を剥離する方法。本発明は、金属板に付着した一種以上の金属を同時期に溶解することができ、付着金属の剥離時間を短縮することを目的とする。
【選択図】図１This is a method of peeling off the metal attached to the metal plate by an electrolytic device using a flat DC voltage. After immersing the metal plate to which the metal is attached in an electrolytic solution, the metal plate is used as an anode and the anode potential is set to 0. A method for peeling an adhered metal from a metal plate, which comprises peeling the adhered metal from the metal plate by electrolyzing under the condition of 1 to 3.0 V (Ag / AgCl reference electrode). An object of the present invention is to be able to dissolve one or more metals adhering to a metal plate at the same time, and to shorten the peeling time of the adhering metal.
[Selection diagram] Fig. 1
Description
本発明は、例えば、成膜装置で用いられる防着板のような金属板に、付着した金属を効率的に剥離する方法に関する。 The present invention relates to, for example, a method for efficiently peeling off metal adhering to a metal plate such as an adhesive plate used in a film forming apparatus.
ＰＶＤやＣＶＤの成膜装置では、成膜用基板以外にも、膜を構成する金属が付着することから、チャンバー内に防着板を設け、チャンバー内壁等に被膜が形成するのを防止している。しかし、防着板も使用し続けると、次第に付着した金属層の厚みが厚くなって、脱落するおそれがあることから、適当な時期に成膜装置から取り外して、付着した金属を剥離、洗浄した後、再利用することが行われている。 In PVD and CVD film forming equipment, in addition to the film forming substrate, the metal constituting the film adheres, so a protective plate is provided in the chamber to prevent the film from forming on the inner wall of the chamber. There is. However, if the adhesive plate is also used continuously, the thickness of the adhered metal layer gradually increases and may fall off. Therefore, the adhered metal was peeled off and washed by removing it from the film forming apparatus at an appropriate time. Later, it is being reused.
また、成膜用基板の上方に、金属板のマスクを配置して、必要な部分のみに金属膜を成膜して、電極パターンなどを形成することが行われている。このとき、マスク用金属板には膜と同一成分の金属が付着することから、その付着した金属の脱落による汚染を防止したり、マスキングとしての性能を維持するために、防着板と同様、適当な時期に成膜装置から取り外して、付着した金属を剥離等することが行われている。 Further, a mask of a metal plate is arranged above the film-forming substrate, and a metal film is formed only on a necessary portion to form an electrode pattern or the like. At this time, since a metal having the same composition as the film adheres to the metal plate for the mask, in order to prevent contamination due to the adhered metal falling off and to maintain the performance as masking, the same as the protective plate. It is removed from the film forming apparatus at an appropriate time to peel off the adhered metal.
上記成膜装置内の金属板としては通常、耐食性が高いステンレスが用いられている。また、付着する金属としては、膜の用途に応じて、その種類は決定されるが、主として銅、アルミニウム、金、銀、ニッケル、クロム、コバルトが用いられている。例えば、金電極を形成する場合、密着性向上のためにニッケルやクロムの下地膜を成膜した後、金を成膜することが行われている。 As the metal plate in the film forming apparatus, stainless steel having high corrosion resistance is usually used. The type of metal to be adhered is determined according to the use of the film, but mainly copper, aluminum, gold, silver, nickel, chromium and cobalt are used. For example, in the case of forming a gold electrode, a nickel or chromium base film is formed to improve the adhesion, and then gold is formed.
上記のような成膜工程を繰り返し行うと、金属板の上には、次第に金とニッケル又はクロムが交互に積層されることになる。通常、このような金属板から付着金属を剥離する場合、金属板を溶液に浸漬して、付着金属を溶解することが行われる。例えば、金とニッケルの溶解はシアン化アルカリ溶液で行い、一方、クロムの溶解はセリウム化酸性溶液で行い、これら二つの溶解操作を交互に繰り返す処理が行われる。 When the film forming process as described above is repeated, gold and nickel or chromium are gradually laminated on the metal plate alternately. Usually, when the attached metal is peeled from such a metal plate, the metal plate is immersed in a solution to dissolve the attached metal. For example, gold and nickel are dissolved in an alkaline cyanide solution, while chromium is dissolved in a ceriumized acidic solution, and these two dissolution operations are alternately repeated.
しかし、この方法は、二種類の溶液に交互に浸漬させる作業が必要であり、入れ替え作業に時間が掛かるという問題があった。特に、マスクの場合は、金属層の数が多く、交互浸漬によって溶解処理していくと、全ての金属層を剥離するために多くの処理日数を要していた。さらに、防着板の場合は、膜厚が厚いことから、浸漬処理で完全に溶解しないことがあり、物理的に手作業で剥離するという作業が必要であった。 However, this method requires a work of alternately immersing the two kinds of solutions, and has a problem that the replacement work takes time. In particular, in the case of a mask, the number of metal layers is large, and when the dissolution treatment is carried out by alternating immersion, a large number of treatment days are required to peel off all the metal layers. Further, in the case of the adhesive plate, since the film thickness is thick, it may not be completely dissolved by the dipping treatment, and it is necessary to physically peel it off manually.
これに対し、複数の金属層が積層した金属板から該金属層を剥離する他の方法として、シアン化系アルカリ溶液内において、金属板を陽極として、通電と無通電を交互に繰り返すパルス電解を行うことで、積層された金属層を順次剥離する方法が提案されている（特許文献１）。しかし、このようなパルス通電を行う場合、対象金属層により適切な通電／無通電時間を設定する必要があり、条件設定が複雑であるという問題があった。 On the other hand, as another method of peeling the metal layer from the metal plate in which a plurality of metal layers are laminated, pulse electrolysis in which the metal plate is used as an anode in a cyanide-based alkaline solution and energization and non-energization are alternately repeated is performed. By doing so, a method of sequentially peeling off the laminated metal layers has been proposed (Patent Document 1). However, when such pulse energization is performed, it is necessary to set an appropriate energization / non-energization time depending on the target metal layer, and there is a problem that the condition setting is complicated.
本発明は、上記従来技術の問題点に鑑みてなされたものであって、平坦な直流電圧を用いた電解装置において、金属板に付着した一種以上の金属を同時期に溶解することができ、付着金属の剥離時間を短縮することを目的とする。 The present invention has been made in view of the above-mentioned problems of the prior art, and can dissolve one or more metals adhering to a metal plate at the same time in an electrolytic device using a flat DC voltage. The purpose is to shorten the peeling time of the adhered metal.
本発明者は、上記課題を解決するために鋭意研究を行った結果、平坦な直流電圧を用いた電解装置においても、陽極電位を適切に調整することにより、付着金属を効率よく剥離することができるという知見を見出した。
この知見に基づき、以下の発明を提供する。As a result of diligent research to solve the above problems, the present inventor has been able to efficiently peel off adhered metals by appropriately adjusting the anodic potential even in an electrolytic device using a flat DC voltage. I found the finding that it can be done.
Based on this finding, the following inventions are provided.
１）平坦な直流電圧を用いた電解装置によって金属板に付着した金属を剥離する方法であって、金属が付着した金属板を電解液に浸漬した後、該金属板を陽極として、陽極電位を０．１〜３．０Ｖ（Ａｇ／ＡｇＣｌ参照電極）の条件で電解することにより、該付着金属を金属板から剥離することを特徴とする金属板から付着金属を剥離する方法。
２）付着金属が、銅、アルミニウム、金、銀、ニッケル、クロム、コバルトの中から選択されるいずれか一種以上の金属であることを特徴とする上記１）記載の金属板から付着金属を剥離する方法。
３）付着金属が、銅、アルミニウム、金、銀、ニッケル、クロム、コバルトの場合、電解液としてシアン化アルカリ溶液を用い、付着金属が、銅、ニッケル、コバルトの場合、電解液として硫酸塩溶液を用いる、ことを特徴とする上記１）又は２）記載の金属板から付着金属を剥離する方法。
４）電圧値を０．５Ｖ〜３０Ｖ、電流値を０．０５Ａ／ｄｍ２〜１Ａ／ｄｍ２とすることを特徴とする上記１）〜３）のいずれか一に記載の金属板から付着金属を剥離する方法。
５）電解液温度を２０℃〜６０℃とすることを特徴とする上記１）〜４）のいずれか一に記載の金属板から付着金属を剥離する方法。1) This is a method of peeling off the metal adhering to a metal plate by an electrolytic device using a flat DC voltage. After immersing the metal plate to which the metal adheres in an electrolytic solution, the metal plate is used as an anode to set the anode potential. A method for peeling an adhering metal from a metal plate, which comprises peeling the adhering metal from the metal plate by electrolyzing under the condition of 0.1 to 3.0 V (Ag / AgCl reference electrode).
2) The attached metal is peeled off from the metal plate according to 1) above, wherein the adhered metal is one or more metals selected from copper, aluminum, gold, silver, nickel, chromium, and cobalt. how to.
3) When the adhering metal is copper, aluminum, gold, silver, nickel, chromium, cobalt, an alkali cyanide solution is used as the electrolytic solution, and when the adhering metal is copper, nickel, cobalt, a sulfate solution is used as the electrolytic solution. The method for peeling the adhered metal from the metal plate according to 1) or 2) above, which comprises using.
4) Adhering metal from the metal plate according to any one of 1) to 3) above, wherein the voltage value is 0.5V to 30V and the current value is 0.05A / dm 2 to 1A / dm 2. How to peel off.
5) The method for peeling adhered metal from the metal plate according to any one of 1) to 4) above, wherein the electrolytic solution temperature is set to 20 ° C to 60 ° C.
本発明は、平坦な直流電流を用いた電解装置においても、その陽極電圧を適切に調整することによって、一種以上の付着金属を、同時期に溶解することができるので、付着する金属の種類に応じて、溶液の種類や、電解条件（通電／無通電）を変更する必要がなく、付着金属の剥離に伴う時間を短縮することができるという優れた効果を有する。本方法は、付着金属が均一に付着（積層）していない場合においても、有効である。 According to the present invention, even in an electrolyzer using a flat direct current, one or more kinds of adhered metals can be melted at the same time by appropriately adjusting the anode voltage, so that the type of adhered metal can be selected. Therefore, it is not necessary to change the type of solution and the electrolysis conditions (energized / de-energized), and it has an excellent effect that the time required for peeling of the adhered metal can be shortened. This method is effective even when the adhered metal is not uniformly adhered (laminated).
本発明は、平坦な直流電圧を用いた電解法によって、金属板から付着金属を剥離する方法である。ここで平坦な直流電圧とは、電圧波形がパルス波形ではなく、平坦な波形であることを意味する。本発明は、平坦な直流電圧を用いた電解装置においても、陽極電位を適切に調整することにより、金属板から一種以上の付着金属を同時期に剥離することを可能とすることができ、ひいては、剥離の処理時間と処理工程を短縮することができるというものである。 The present invention is a method of peeling adhered metal from a metal plate by an electrolysis method using a flat DC voltage. Here, the flat DC voltage means that the voltage waveform is not a pulse waveform but a flat waveform. According to the present invention, even in an electrolyzer using a flat DC voltage, by appropriately adjusting the anodic potential, it is possible to peel off one or more adhered metals from the metal plate at the same time, and by extension, , The peeling processing time and processing process can be shortened.
金属板は、防着板やマスク等に使用されるものであって、通常、ステンレスのような表面が酸化膜に覆われている材料が用いられる。ステンレス以外にも、表面に酸化膜が形成されたアルミニウム板などが用いられる場合がある。このような金属板は、防着材やマスク等として一定期間使用し続けると、その表面には成膜に伴う金属が付着、積層する。そして、金属の付着量が多くなると、次第に付着した金属が脱落して、基板を汚染等することになる。したがって、金属板は、定期的に付着した金属を剥離、洗浄する必要がある。 The metal plate is used for a protective plate, a mask, or the like, and a material such as stainless steel whose surface is covered with an oxide film is usually used. In addition to stainless steel, an aluminum plate having an oxide film formed on its surface may be used. When such a metal plate is continuously used as an adhesive material, a mask, or the like for a certain period of time, the metal accompanying the film formation adheres to and is laminated on the surface thereof. Then, when the amount of metal adhered increases, the adhered metal gradually falls off and contaminates the substrate. Therefore, it is necessary to periodically peel off and clean the adhered metal on the metal plate.
付着する金属の種類は、成膜する膜の種類（用途）によって異なる。例えば、半導体配線用膜を成膜する場合には、配線材としての銅やアルミニウム、コバルトなどが付着することになる。また、水晶振動子等における電極用膜を成膜する場合には、電極としての金や銀と、下地層としてのニッケルやクロムとが、交互に積層されることになる。なお、本発明は、金属板に銅、アルミニウム、金、銀、ニッケル、クロム、コバルトのいずれいか一種以上の金属が付着している場合に対して、有効であり、どのような用途（過程）で付着された金属であるかについては、特に問わない。 The type of metal to be attached differs depending on the type (use) of the film to be formed. For example, when a film for semiconductor wiring is formed, copper, aluminum, cobalt, or the like as a wiring material adheres to the film. Further, when forming a film for an electrode in a crystal oscillator or the like, gold or silver as an electrode and nickel or chromium as a base layer are alternately laminated. The present invention is effective when any one or more metals such as copper, aluminum, gold, silver, nickel, chromium, and cobalt are attached to the metal plate, and what kind of application (process) is used. It does not matter whether the metal is attached in.
本発明の剥離方法について具体的に説明する。
まず、図１に示すように、金属が付着する金属板を、電解槽の電解液中に浸漬する。電解液には、付着金属と安定な溶存形態を形成する成分を含み、且つ、金属板の金属酸化膜が不溶性である液種を選択する。例えば、付着金属が銅、アルミニウム、金、銀、ニッケル、クロム、コバルトであり、金属板がステンレスの場合には、電解液として、シアン化ナトリウム溶液を使用することができる。また、付着金属が銅、ニッケル、コバルトであり、金属板がアルミニウム（表面には酸化膜が形成されている）の場合には硫酸アンモニウム溶液を用いることができる。The peeling method of the present invention will be specifically described.
First, as shown in FIG. 1, a metal plate to which metal adheres is immersed in an electrolytic solution in an electrolytic cell. Select a liquid type in which the electrolytic solution contains a component that forms a stable dissolved form with the adhered metal and the metal oxide film of the metal plate is insoluble. For example, when the adhered metal is copper, aluminum, gold, silver, nickel, chromium, or cobalt and the metal plate is stainless steel, a sodium cyanide solution can be used as the electrolytic solution. When the adhered metal is copper, nickel, or cobalt and the metal plate is aluminum (an oxide film is formed on the surface), an ammonium sulfate solution can be used.
図１では、金属板を金属製（例えば、ステンレス）カゴに設置して、そのカゴ本体を電解液に浸漬させている。このようにすることで、陽極とした金属板の陽極電位を厳密に調整することができると共に、複数の金属板を同時に処理することができるので作業効率が高めることができる。このように、陽極として金属板の場合だけでなく、金属製のカゴを用いることも有効である。また、陰極には、ステンレスなど、本発明の電解条件において不溶性である材質のものを使用する。 In FIG. 1, a metal plate is placed in a metal (for example, stainless steel) basket, and the basket body is immersed in an electrolytic solution. By doing so, the anode potential of the metal plate used as the anode can be precisely adjusted, and a plurality of metal plates can be processed at the same time, so that the work efficiency can be improved. As described above, it is effective not only to use a metal plate as the anode but also to use a metal basket. Further, as the cathode, a material such as stainless steel, which is insoluble under the electrolytic conditions of the present invention, is used.
次に、整流器を用いて電解を行う。電解中は、陽極電位が０．１Ｖ〜３．０Ｖ（参照電極：Ａｇ／ＡｇＣｌ）となるように調整することが、重要である。上記の電位範囲においては、付着金属（銅、アルミニウム、金、銀、ニッケル、クロム、コバルト）が、電極反応により効率的に酸化されて、剥離することが可能となる。一方、０．１Ｖ未満であると、電流値が小さいために剥離速度が遅く、３．０Ｖ超であると、水の電気分解が優勢となり、付着金属の剥離が進まない。したがって、陽極電位はこの範囲とする。 Next, electrolysis is performed using a rectifier. During electrolysis, it is important to adjust the anodic potential to be 0.1 V to 3.0 V (reference electrode: Ag / AgCl). In the above potential range, adherent metals (copper, aluminum, gold, silver, nickel, chromium, cobalt) can be efficiently oxidized by the electrode reaction and peeled off. On the other hand, if it is less than 0.1 V, the peeling speed is slow because the current value is small, and if it exceeds 3.0 V, the electrolysis of water becomes predominant and the peeling of the adhered metal does not proceed. Therefore, the anodic potential is in this range.
本発明において電解条件は、電圧値を０．５Ｖ〜３０Ｖとし、電流値を０．０５Ａ／ｄｍ２〜１Ａ／ｄｍ２とすることが好ましい。また、電解液の温度は２０℃〜６０℃とすることが好ましい。電解液の温度が２０℃未満であると、電力消費量が増加し、一方、６０℃を超えると、電解液が揮発することがあるためである。
そして、電流値が１ｍＡ／ｄｍ２未満となった時点で、付着金属がほぼ無くなったと判断して、電解を停止する。In the present invention, the electrolytic conditions are preferably such that the voltage value is 0.5V to 30V and the current value is 0.05A / dm 2 to 1A / dm 2 . The temperature of the electrolytic solution is preferably 20 ° C to 60 ° C. This is because if the temperature of the electrolytic solution is less than 20 ° C., the power consumption increases, while if it exceeds 60 ° C., the electrolytic solution may volatilize.
Then, when the current value becomes less than 1 mA / dm 2 , it is determined that the adhered metal has almost disappeared, and the electrolysis is stopped.
電解終了後は、電解槽から金属板あるいは金属板が設置された金属製かごを取り出し、金属板を洗浄する。洗浄には、純水を用いることができるが特に制限はない。洗浄後、金属板は、再度、防着板あるいはマスク等として、再利用することができる。一方、電解液中に溶解した各種金属は電解採取することによって、有価金属として、分離、回収することができる。なお、金については、電解中に陰極に電着するので、電着金属として、回収することができる。 After the electrolysis is completed, the metal plate or the metal basket in which the metal plate is installed is taken out from the electrolytic cell, and the metal plate is washed. Pure water can be used for cleaning, but there is no particular limitation. After cleaning, the metal plate can be reused as a protective plate, a mask, or the like. On the other hand, various metals dissolved in the electrolytic solution can be separated and recovered as valuable metals by electrowinning. Since gold is electrodeposited on the cathode during electrolysis, it can be recovered as an electrodeposited metal.
以上より、複雑な電解工程を行うことなく、一般的な電解装置を用いて、金属板から付着金属を剥離することができるので、処理時間及び処理工程を大幅に短縮することができる。また、本発明の方法は、付着金属が交互に積層された場合だけでなく、同一面内に複数の付着金属が存在するような場合であっても、同時期に付着金属を剥離することができる。 From the above, since the adhering metal can be peeled off from the metal plate by using a general electrolysis device without performing a complicated electrolysis step, the treatment time and the treatment step can be significantly shortened. Further, the method of the present invention can peel off the adhered metal at the same time not only when the adhered metals are alternately laminated but also when a plurality of adhered metals are present in the same plane. it can.
ステンレス（ＳＵＳ３０４）製の金属板に、金層とクロム層とを積層させて、金属が付着した金属板のサンプルを作製した。金層の膜厚は０．１μｍとし、クロム層の膜厚は０．０１μｍ、全体の膜厚は５μｍとした。次に、このサンプルをシアン化ナトリウム溶液の電解液に浸漬して、各サンプルに対して、それぞれの陽極電位を０．０５Ｖ〜５．０Ｖ（参照電極：Ａｇ／ＡｇＣｌ）に設定して、電解処理を行った。そして、電流値が１ｍＡ／ｄｍ２未満になった時点で、付着金属が剥離したものとして、その剥離に要した時間を計測した。なお、電解液温度を２０℃に設定した。A gold layer and a chromium layer were laminated on a metal plate made of stainless steel (SUS304) to prepare a sample of a metal plate to which metal was attached. The film thickness of the gold layer was 0.1 μm, the film thickness of the chromium layer was 0.01 μm, and the overall film thickness was 5 μm. Next, this sample is immersed in an electrolytic solution of sodium cyanide solution, and for each sample, the respective anode potential is set to 0.05V to 5.0V (reference electrode: Ag / AgCl) for electrolysis. Processing was performed. Then, when the current value became less than 1 mA / dm 2 , it was assumed that the adhered metal had peeled off, and the time required for the peeling was measured. The electrolyte temperature was set to 20 ° C.
下記の表１に示される通り、陽極電位を０．１Ｖ〜３．０Ｖの範囲では、剥離時間がいずれも１００分以内と剥離時間の短縮が確認された。一方、陽極電位が０．０５Ｖ、あるいは、３．５Ｖ以上の場合には、剥離時間が２００分超と長くなっていた。なお、従来技術に基づき、シアン化アルカリ溶液とセリウム化酸性溶液に交互に浸漬し、それぞれ金層とクロム層を交互に溶かした場合の剥離時間は１３０分であり、この従来技術の方法と比べて、剥離時間の大幅な短縮が確認できる。 As shown in Table 1 below, when the anode potential was in the range of 0.1 V to 3.0 V, the peeling time was confirmed to be within 100 minutes and the peeling time was shortened. On the other hand, when the anodic potential was 0.05 V or 3.5 V or more, the peeling time was as long as more than 200 minutes. In addition, based on the prior art, the peeling time is 130 minutes when the gold layer and the chromium layer are alternately immersed in the alkali cyanide solution and the cerium acid solution, respectively, which is compared with the method of the prior art. Therefore, it can be confirmed that the peeling time is significantly reduced.
本発明によれば、付着する金属の種類に応じて、電解条件等を変更する必要がなく、付着金属の剥離に伴う処理時間や処理工程を大幅に短縮することができる。さらに、本発明は、付着金属を剥離した金属板を防着板やマスクとして、再利用することができ、また、電解液中に溶出させた各種金属を有価物として回収することができる。さらに、金属回収後の電解液を廃液にすることなく再利用することができる。本発明は、成膜装置の防着板やマスク、メッキ治具など、金属が付着した金属板の再生方法として有用である。 According to the present invention, it is not necessary to change the electrolysis conditions and the like according to the type of the adhered metal, and the treatment time and the treatment step associated with the peeling of the adhered metal can be significantly shortened. Further, in the present invention, the metal plate from which the adhered metal has been peeled off can be reused as an adhesive plate or a mask, and various metals eluted in the electrolytic solution can be recovered as valuable resources. Further, the electrolytic solution after metal recovery can be reused without being made into waste liquid. The present invention is useful as a method for regenerating a metal plate to which metal is attached, such as a protective plate, a mask, and a plating jig of a film forming apparatus.
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