TWI725345B - Method for peeling attached metal from metal plate - Google Patents
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- TWI725345B TWI725345B TW107135033A TW107135033A TWI725345B TW I725345 B TWI725345 B TW I725345B TW 107135033 A TW107135033 A TW 107135033A TW 107135033 A TW107135033 A TW 107135033A TW I725345 B TWI725345 B TW I725345B
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Abstract
本發明之自金屬板剝離附著金屬之方法係藉由使用平坦之直流電壓之電解裝置將附著於金屬板之金屬剝離之方法，其特徵在於：將附著有金屬之金屬板浸漬於電解液中之後，將該金屬板作為陽極，於使陽極電位處在0.1〜3.0 V（Ag/AgCl參考電極）之條件下進行電解，藉此將該附著金屬自金屬板剝離。本發明之目的在於：能於同一時期使附著於金屬板上之一種以上金屬溶解，從而縮短附著金屬之剝離時間。The method of peeling the attached metal from the metal plate of the present invention is a method of peeling the metal attached to the metal plate by using a flat DC voltage electrolytic device, which is characterized in that the metal plate with the attached metal is immersed in the electrolyte solution Using the metal plate as the anode, electrolysis was performed under the condition that the anode potential was at 0.1~3.0 V (Ag/AgCl reference electrode), thereby peeling the attached metal from the metal plate. The purpose of the present invention is to dissolve more than one metal attached to the metal plate at the same time, thereby shortening the peeling time of the attached metal.
Description
本發明係關於一種將附著於例如成膜裝置中所使用之防黏板一類之金屬板的金屬有效率地剝離之方法。The present invention relates to a method for efficiently peeling metal attached to a metal plate such as a release plate used in a film forming device.
於PVD或CVD之成膜裝置中，構成膜之金屬亦會附著於成膜用基板以外的地方，故而於腔室內設置防黏板，以防於腔室內壁等形成被膜。但若防黏板被持續使用，則有所附著之金屬層之厚度逐漸變厚而脫落之虞，因此要於適當時期將防黏板自成膜裝置拆下，將所附著之金屬剝離、洗淨後，再進行利用。In PVD or CVD film forming equipment, the metal constituting the film will also adhere to places other than the film-forming substrate, so a release plate is installed in the chamber to prevent the formation of a film on the inner wall of the chamber. However, if the anti-sticking plate is used continuously, the thickness of the attached metal layer will gradually become thicker and may fall off. Therefore, the anti-sticking plate should be removed from the film forming device at an appropriate time, and the attached metal should be peeled off and washed. After cleaning, use it again.
又，於成膜用基板之上方，配置金屬板之遮罩，而僅於必要部分成膜金屬膜，形成電極圖案等。此時，成分與膜相同之金屬會附著於遮罩用金屬板上，故而為了防止所附著之金屬脫落而造成污染，或維持其遮蔽性能，與防黏板同樣地，要於適當時期將遮罩用金屬板自成膜裝置拆下，將所附著之金屬剝離等。In addition, a mask of a metal plate is arranged above the substrate for film formation, and a metal film is formed only on necessary parts to form electrode patterns and the like. At this time, the metal with the same composition as the film will adhere to the metal plate for the mask. Therefore, in order to prevent the attached metal from falling off and cause pollution, or to maintain its shielding performance, similar to the release sheet, the shield must be covered at an appropriate time. The cover metal plate is removed from the film forming device, and the attached metal is peeled off.
作為上述成膜裝置內之金屬板，通常使用耐腐蝕性較高之不鏽鋼。又，作為附著之金屬，其種類根據膜之用途而決定，主要使用銅、鋁、金、銀、鎳、鉻、鈷。例如，要形成金電極之情形時，為了提高密合性，於成長鎳基底膜或鉻基底膜之後，將進行金成膜。As the metal plate in the above-mentioned film forming device, stainless steel with high corrosion resistance is usually used. In addition, as the metal to be attached, the type is determined according to the use of the film, and copper, aluminum, gold, silver, nickel, chromium, and cobalt are mainly used. For example, when a gold electrode is to be formed, in order to improve adhesion, a gold film is formed after a nickel base film or a chromium base film is grown.
若反覆實施如上所述之成膜步驟，則於金屬板之上，金與鎳或鉻會逐漸交替地積層。通常，要自此種金屬板剝離附著金屬之情形時，會將金屬板浸漬於溶液中，使附著金屬溶解。例如，金與鎳之溶解係於氰化鹼溶液中進行，另一方面，鉻之溶解係於鈰化酸性溶液中進行，執行交替地反覆實施上述兩種溶解操作之處理。If the film forming steps as described above are repeatedly performed, gold and nickel or chromium will gradually alternately layer on the metal plate. Generally, when peeling the adhered metal from such a metal plate, the metal plate is immersed in a solution to dissolve the adhered metal. For example, the dissolution of gold and nickel is carried out in an alkali cyanide solution. On the other hand, the dissolution of chromium is carried out in a cerium acid solution, and the above-mentioned two dissolving operations are performed alternately and repeatedly.
但該方法需實施使金屬板交替地浸漬於兩種溶液中之作業，從而有更替作業耗費時間之問題。尤其是遮罩之情形時，金屬層數較多，若藉由交替浸漬而進行溶解處理，則將所有金屬層剝離需耗費較多處理天數。進而，於防黏板之情形時，膜厚較厚，故而有藉由浸漬處理無法完全溶解之情況，從而需實施以手動方式進行物理剝離之作業。However, this method requires the operation of alternately immersing the metal plate in the two solutions, so there is a problem that the replacement operation takes time. Especially in the case of a mask, the number of metal layers is large, and if the dissolution treatment is performed by alternate dipping, it will take a lot of processing days to peel off all the metal layers. Furthermore, in the case of the release plate, the film thickness is relatively thick, so it cannot be completely dissolved by the dipping treatment, so it is necessary to perform a manual physical peeling operation.
針對於此，作為自積層有多層金屬層之金屬板剝離該金屬層之其他方法，提出有如下方案，即，於氰化系鹼溶液內，將金屬板作為陽極，進行交替地反覆實施通電與不通電之脈衝電解，藉此將所積層之金屬層依序剝離（專利文獻1）。但於此種進行脈衝通電之情形時，需根據對象金屬層來設定適當之通電/不通電時間，而有條件設定較為複雜之問題。 先前技術文獻 專利文獻In response to this, as another method of peeling off the metal layer from a metal plate laminated with multiple metal layers, the following proposal has been proposed. That is, in a cyanide-based alkaline solution, the metal plate is used as an anode, and energization and energization are alternately performed repeatedly. Pulse electrolysis without current is used to sequentially peel off the laminated metal layers (Patent Document 1). However, in the case of pulse energization, it is necessary to set an appropriate energization/non-energization time according to the target metal layer, and there is a problem that the condition setting is more complicated. Prior art literature Patent literature
專利文獻1：日本特開2009-102704號公報Patent Document 1: Japanese Patent Application Publication No. 2009-102704
[發明所欲解決之課題][The problem to be solved by the invention]
本發明係鑒於上述先前技術之問題點而完成者，其目的在於：於使用平坦之直流電壓之電解裝置中，能於同一時期使附著於金屬板上之一種以上金屬溶解，從而縮短附著金屬之剝離時間。 [解決課題之技術手段]The present invention was completed in view of the above-mentioned problems of the prior art, and its purpose is to dissolve more than one metal attached to the metal plate at the same time in an electrolytic device using a flat DC voltage, thereby shortening the amount of metal attached. Stripping time. [Technical means to solve the problem]
本發明人為了解決上述課題進行了努力研究，結果得出如下結論：於使用平坦之直流電壓之電解裝置中，藉由適當地調整陽極電位，亦能效率良好地剝離附著金屬。In order to solve the above-mentioned problems, the inventors have made diligent research, and as a result, have come to the following conclusion: In an electrolytic device using a flat DC voltage, by appropriately adjusting the anode potential, the attached metal can also be peeled off efficiently.
基於該結論，提供以下發明。 1)一種自金屬板剝離附著金屬之方法，係藉由使用平坦之直流電壓之電解裝置將附著於金屬板之金屬剝離之方法，其特徵在於：將附著有金屬之金屬板浸漬於電解液中之後，將該金屬板作為陽極，於使陽極電位處在0.1〜3.0 V（Ag/AgCl參考電極）之條件下進行電解，藉此將該附著金屬自金屬板剝離。 2)如上述1)所記載之自金屬板剝離附著金屬之方法，其中，附著金屬係選自銅、鋁、金、銀、鎳、鉻、鈷中任一種以上之金屬。 3)如上述1)或2)所記載之自金屬板剝離附著金屬之方法，其中，於附著金屬為銅、鋁、金、銀、鎳、鉻、鈷之情形時，使用氰化鹼溶液作為電解液，於附著金屬為銅、鎳、鈷之情形時，使用硫酸鹽溶液作為電解液。 4)如上述1)〜3)中任一項所記載之自金屬板剝離附著金屬之方法，其中，將電壓值設定為0.5 V〜30 V，將電流值設定為0.05 A/dm2 〜1 A/dm2 5)如上述1)〜4)中任一項所記載之自金屬板剝離附著金屬之方法，其中，將電解液溫度設定為20℃〜60℃。 [發明之效果]Based on this conclusion, the following invention is provided. 1) A method of peeling the attached metal from the metal plate by using a flat DC voltage electrolytic device to peel off the metal attached to the metal plate, which is characterized in that the metal plate with the metal attached is immersed in the electrolyte After that, the metal plate is used as an anode, and electrolysis is performed under the condition that the anode potential is at 0.1-3.0 V (Ag/AgCl reference electrode), thereby peeling the attached metal from the metal plate. 2) The method of peeling the adhered metal from the metal plate as described in 1) above, wherein the adhered metal is any one or more metals selected from copper, aluminum, gold, silver, nickel, chromium, and cobalt. 3) The method for peeling the attached metal from the metal plate as described in 1) or 2) above, wherein when the attached metal is copper, aluminum, gold, silver, nickel, chromium, or cobalt, an alkali cyanide solution is used as For the electrolyte, when the adhesion metal is copper, nickel, or cobalt, a sulfate solution is used as the electrolyte. 4) The method for peeling the attached metal from the metal plate as described in any one of 1) to 3) above, wherein the voltage value is set to 0.5 V to 30 V, and the current value is set to 0.05 A/dm 2 〜1 A/dm 2 5) The method for peeling adhered metal from a metal plate as described in any one of 1) to 4) above, wherein the temperature of the electrolyte is set to 20°C to 60°C. [Effects of Invention]
本發明具有如下優異效果，即，於使用平坦之直流電流之電解裝置中，藉由適當地調整其陽極電壓，亦能於同一時期使一種以上附著金屬溶解，故而無需根據附著之金屬種類，變更溶液之種類或電解條件（通電/不通電），從而能縮短伴隨於附著金屬之剝離而產生之時間。本方法於附著金屬未均勻地附著（積層）之情形時亦有效。The present invention has the following excellent effects. That is, in an electrolysis device using a flat DC current, by appropriately adjusting the anode voltage, more than one attached metal can be dissolved at the same time, so there is no need to change according to the type of attached metal. The type of solution or electrolysis conditions (electricity/non-electricity) can shorten the time associated with the peeling of the attached metal. This method is also effective when the adhesion metal is not uniformly adhered (layered).
本發明係藉由使用平坦之直流電壓之電解法，自金屬板剝離附著金屬之方法。此處所謂之平坦之直流電壓，係指電壓波形為平坦之波形而非脈衝波形。本發明係於使用平坦之直流電壓之電解裝置中，藉由適當地調整陽極電位，亦能於同一時期將一種以上附著金屬自金屬板剝離，進而能縮短剝離之處理時間及減少處理步驟者。The present invention is a method of peeling the attached metal from the metal plate by the electrolysis method using a flat DC voltage. The so-called flat DC voltage here means that the voltage waveform is a flat waveform rather than a pulse waveform. The present invention is an electrolysis device using a flat DC voltage. By appropriately adjusting the anode potential, more than one attached metal can be peeled from the metal plate at the same time, thereby shortening the peeling processing time and reducing the processing steps.
金屬板係用作防黏板或遮罩等者，通常使用不鏽鋼一類之表面被氧化膜覆蓋之材料。除不鏽鋼以外，亦有使用表面形成有氧化膜之鋁板等之情形時。此類金屬板若作為防黏材或遮罩等而持續使用一定期間，則其表面上會附著、積層伴隨於膜成長而產生之金屬。而且，若金屬之附著量增多，則所附著之金屬會逐漸地脫落，而對基板造成污染等。因此，對於金屬板，需定期地將所附著之金屬剝離、洗淨。Metal plates are used as anti-sticking plates or masks, and usually use materials such as stainless steel whose surface is covered by an oxide film. In addition to stainless steel, there are also cases where aluminum plates with oxide films formed on the surface are used. If such a metal plate is continuously used for a certain period of time as a release material or a mask, the metal produced by the growth of the film will adhere to and build up on the surface. Moreover, if the amount of metal attached increases, the attached metal will gradually fall off, causing contamination to the substrate. Therefore, for metal plates, it is necessary to peel off and clean the attached metal regularly.
附著之金屬之種類因所成之膜之種類（用途）而異。例如，於要成長半導體配線用膜之情形時，會有作為配線材之銅、鋁或鈷等附著。又，於要成長水晶振子等中之電極用膜之情形時，會有作為電極之金或銀與作為基底層之鎳或鉻交替地積層。再者，本發明對金屬板上附著有銅、鋁、金、銀、鎳、鉻、鈷中任一種以上之金屬之情形有效，無論其係於何種用途（過程）中附著之金屬。The type of attached metal varies with the type (purpose) of the film formed. For example, when a film for semiconductor wiring is to be grown, copper, aluminum, or cobalt as wiring materials may adhere. In addition, when a film for electrodes in a crystal vibrator or the like is to be grown, gold or silver as the electrode and nickel or chromium as the base layer are alternately laminated. Furthermore, the present invention is effective in the case where any one or more of copper, aluminum, gold, silver, nickel, chromium, and cobalt is attached to the metal plate, regardless of the application (process) of the attached metal.
對本發明之剝離方法具體地進行說明。 首先，如圖1所示，將附著金屬之金屬板浸漬於電解槽之電解液中。關於電解液，選擇含有與附著金屬形成穩定之溶存形態之成分，且對金屬板之金屬氧化膜具有不溶性之液種。例如，於附著金屬為銅、鋁、金、銀、鎳、鉻、鈷，且金屬板為不鏽鋼之情形時，可使用氰化鈉溶液作為電解液。又，於附著金屬為銅、鎳、鈷，且金屬板為鋁（表面形成有氧化膜）之情形時，可使用硫酸銨溶液作為電解液。The peeling method of the present invention will be specifically described. First, as shown in Fig. 1, the metal plate to which the metal is attached is immersed in the electrolyte of the electrolytic cell. Regarding the electrolyte, select a solution that contains a component that forms a stable dissolved form with the attached metal and is insoluble to the metal oxide film of the metal plate. For example, when the attachment 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 electrolyte. In addition, when the adhesion metal is copper, nickel, or cobalt, and the metal plate is aluminum (with an oxide film formed on the surface), an ammonium sulfate solution can be used as the electrolyte.
於圖1中，金屬板被設置於金屬製（例如，不鏽鋼）籠中，且該籠本體被浸漬於電解液中。藉由如此設置，能嚴謹地調整作為陽極之金屬板之陽極電位，並且能同時處理多個金屬板，因此能提高作業效率。如此，不僅於將金屬板作為陽極之情形時有效，於使用金屬製籠時亦有效。又，關於陰極，使用不鏽鋼等於本發明之電解條件下具有不溶性之材質之陰極。In FIG. 1, the metal plate is set in a metal (for example, stainless steel) cage, and the cage body is immersed in an electrolyte. With this arrangement, the anode potential of the metal plate as the anode can be adjusted rigorously, and multiple metal plates can be processed at the same time, so the work efficiency can be improved. This is effective not only when a metal plate is used as an anode, but also when a metal cage is used. In addition, as for the cathode, a stainless steel cathode is used which is equivalent to a material that is insoluble under the electrolysis conditions of the present invention.
其次，使用整流器進行電解。電解過程中，較重要為以使陽極電位成為0.1 V〜3.0 V（參考電極：Ag/AgCl）之方式進行調整。於上述電位範圍內，附著金屬（銅、鋁、金、銀、鎳、鉻、鈷）藉由電極反應被有效率地氧化，而變得可剝離。另一方面，若未達0.1 V，則會因電流值較小而導致剝離速度緩慢，若超過3.0 V，則水之電解成為優勢，附著金屬之剝離停滯不前。因此，陽極電位要處在該範圍內。Second, use a rectifier for electrolysis. During the electrolysis process, it is more important to adjust the anode potential to 0.1 V~3.0 V (reference electrode: Ag/AgCl). Within the above potential range, the attached metals (copper, aluminum, gold, silver, nickel, chromium, cobalt) are efficiently oxidized by the electrode reaction and become peelable. On the other hand, if the current value is less than 0.1 V, the peeling speed will be slow due to the small current value. If it exceeds 3.0 V, the electrolysis of water becomes an advantage, and the peeling of the attached metal stagnates. Therefore, the anode potential must be within this range.
本發明中，關於電解條件，較佳為將電壓值設定為0.5 V〜30 V，將電流值設定為0.05 A/dm2 〜1 A/dm2 。又，關於電解液之溫度，較佳為將其設定為20℃〜60℃。其理由在於：若電解液之溫度未達20℃，則電力消耗量增加，另一方面，若超過60℃，則電解液揮發。 然後，於電流值變成未達1 mA/dm2 之時間點，判定附著金屬大致消除，而停止電解。In the present invention, regarding the electrolysis conditions, it is preferable to set the voltage value to 0.5 V to 30 V and the current value to 0.05 A/dm 2 to 1 A/dm 2 . In addition, the temperature of the electrolyte is preferably set to 20°C to 60°C. The reason is that if the temperature of the electrolyte solution does not reach 20°C, the power consumption will increase, while if it exceeds 60°C, the electrolyte solution will volatilize. Then, at the time point when the current value became less than 1 mA/dm 2 , it was determined that the attached metal was almost eliminated, and the electrolysis was stopped.
電解結束後，自電解槽將金屬板或設置有金屬板之金屬製籠取出，並將金屬板洗淨。關於洗淨，可使用純水，但無特別限制。洗淨後，金屬板可再次作為防黏板或遮罩等加以再利用。另一方面，溶解於電解液中之各種金屬可藉由電解提取，而作為有價金屬加以分離、回收。再者，關於金，電解過程中會電沈積於陰極，故而可作為電沈積金屬加以回收。After the electrolysis, the metal plate or the metal cage provided with the metal plate is taken out from the electrolytic tank, and the metal plate is washed. Regarding washing, pure water can be used, but there is no particular limitation. After washing, the metal plate can be reused as an anti-sticking plate or mask. On the other hand, various metals dissolved in the electrolyte can be separated and recovered as valuable metals by electrolysis. Furthermore, as for gold, it is electrodeposited on the cathode during electrolysis, so it can be recovered as an electrodeposited metal.
綜上所述，無需實施複雜之電解步驟，使用一般之電解裝置，即能自金屬板剝離附著金屬，故而能大幅度縮短處理時間及減少處理步驟。又，本發明之方法不僅於附著金屬交替地積層之情形時能於同一時期剝離附著金屬，而且於多種附著金屬存在於同一面內之情形時亦能於同一時期剝離附著金屬。 實施例In summary, there is no need to perform complicated electrolysis steps, and the use of a general electrolysis device can peel off the attached metal from the metal plate, so the processing time and the processing steps can be greatly shortened. In addition, the method of the present invention can not only peel off the adhered metal at the same time when the adhered metals are alternately laminated, but also can peel off the adhered metal at the same time when multiple types of adhered metals exist on the same surface. Example
使金層與鉻層積層於不鏽鋼（SUS304）製之金屬板，製作出附著有金屬之金屬板之樣本。將金層之膜厚設定為0.1 μm，將鉻層之膜厚設定為0.01 μm，將整體之膜厚設定為5 μm。其次，將該樣本浸漬於氰化鈉溶液之電解液中，針對各樣本，將各樣本之陽極電位設定為0.05 V〜5.0 V（參考電極：Ag/AgCl）並進行電解處理。然後，於電流值變成未達1 mA/dm2 之時間點，認定附著金屬已被剝離，而計測出該剝離所耗費之時間。再者，將電解液溫度設定為20℃。Laminate the gold layer and chromium layer on a metal plate made of stainless steel (SUS304) to make a sample of the metal plate with metal attached. The film thickness of the gold layer is set to 0.1 μm, the film thickness of the chromium layer is set to 0.01 μm, and the overall film thickness is set to 5 μm. Next, the sample was immersed in the electrolyte of sodium cyanide solution, and for each sample, the anode potential of each sample was set to 0.05 V~5.0 V (reference electrode: Ag/AgCl) and electrolytic treatment was performed. Then, at the point in time when the current value became less than 1 mA/dm 2 , it was determined that the attached metal had been peeled off, and the time taken for the peeling was measured. In addition, the temperature of the electrolyte was set to 20°C.
如下表1所示，於陽極電位處在0.1 V〜3.0 V之範圍內時，剝離時間均為100分鐘以內，確認到剝離時間縮短。另一方面，於陽極電位為0.05 V或3.5 V以上之情形時，剝離時間延長至200餘分鐘。再者，基於先前技術，交替地浸漬於氰化鹼溶液與鈰化酸性溶液中，而使金層與鉻層分別交替地溶解之情形時的剝離時間為130分鐘，與該先前技術之方法相比，能確認到剝離時間大幅度縮短。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 within 100 minutes, and it was confirmed that the peeling time was shortened. On the other hand, when the anode potential is 0.05 V or above 3.5 V, the peeling time is extended to more than 200 minutes. Furthermore, based on the prior art, the peeling time when the gold layer and the chromium layer are alternately dissolved by immersing in an alkali cyanide solution and a cerium acid solution alternately is 130 minutes, which is similar to the method of the prior art. Compared with, it can be confirmed that the peeling time is greatly shortened.
[表1]
根據本發明，無需根據附著之金屬種類來變更電解條件等，從而能大幅度縮短伴隨於附著金屬之剝離而產生之處理時間或減少處理步驟。進而，本發明能將剝離附著金屬後之金屬板作為防黏板或遮罩加以再利用，又，能將溶出於電解液中之各種金屬作為有價物加以回收。進而，能將金屬回收後之電解液加以再利用而非將其作為廢液。本發明作為成膜裝置之防黏板或遮罩、鍍覆治具等附著有金屬之金屬板之再生方法而有用。According to the present invention, it is not necessary to change the electrolysis conditions etc. according to the type of metal to be attached, so that the processing time or the processing steps associated with peeling of the attached metal can be greatly reduced. Furthermore, the present invention can reuse the metal plate from which the attached metal is peeled off as a release sheet or mask, and can also recover various metals dissolved in the electrolyte as valuables. Furthermore, the electrolyte solution after metal recovery can be reused instead of being used as a waste solution. The present invention is useful as a method of regenerating a metal plate to which metal is attached, such as a release plate, a mask, and a plating jig of a film forming device.
無no
圖1係用以使用本發明之方法之電解裝置之例示（模式圖）。Fig. 1 is an illustration (a schematic diagram) of an electrolysis device used to use the method of the present invention.
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