TWI790142B - Hydrofluoric acid treatment monitoring system and method of monitoring hydrofluoric acid treatment - Google Patents

Hydrofluoric acid treatment monitoring system and method of monitoring hydrofluoric acid treatment Download PDF

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TWI790142B
TWI790142B TW111109509A TW111109509A TWI790142B TW I790142 B TWI790142 B TW I790142B TW 111109509 A TW111109509 A TW 111109509A TW 111109509 A TW111109509 A TW 111109509A TW I790142 B TWI790142 B TW I790142B
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hydrofluoric acid
color saturation
image
monitoring system
return pipe
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TW202338608A (en
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鍾昭銘
吳宗勳
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臺灣塑膠工業股份有限公司
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Abstract

The present disclosure provides a hydrofluoric acid treatment monitoring system and a method of monitoring the hydrofluoric acid treatment by the system. The hydrofluoric acid treatment monitoring system includes a treatment tank including a hydrofluoric acid filling port, an oxidant filling port, a refluxing port, and an outlet. The hydrofluoric acid treatment monitoring system also includes a fluid pipeline connected to the outlet of the treatment tank, a reflux line connecting the fluid pipeline and the refluxing port of the treatment tank and including a transparent window, a video camera for filming the transparent window of the reflux line to obtain an image, an image recognition unit for determining a color saturation of the image, and a monitoring unit for alarming when the color saturation is lower than a standard color saturation.

Description

氫氟酸處理監控系統和監控氫氟酸處理方法Hydrofluoric acid treatment monitoring system and monitoring method for hydrofluoric acid treatment

本公開內容是關於氫氟酸處理製程,且特別是關於監控氫氟酸處理製程的系統與方法。The present disclosure relates to hydrofluoric acid treatment processes, and more particularly to systems and methods for monitoring hydrofluoric acid treatment processes.

為達到電子級氫氟酸對於品質之要求,氫氟酸中的不純物應小於標準值。常採用氧化劑將氫氟酸中的不純物氧化成具有高沸點的化合物,從而後續的精餾系統可以將氫氟酸和不純物的化合物進一步分離,以達到處理氫氟酸的效果。在上述氧化過程中需要控制氧化劑的當量,使得氧化劑足以持續氧化氫氟酸中的不純物。然而,為了確認氫氟酸中的氧化劑當量,需要進行現場分階段人工取樣進行試驗。這不僅需要耗費大量時間和人力成本,更造成現場操作者的危險。因此,如何安全且方便監控氫氟酸處理製程中的氧化劑當量是相關領域待解決的問題。In order to meet the quality requirements of electronic grade hydrofluoric acid, the impurities in hydrofluoric acid should be less than the standard value. Oxidants are often used to oxidize the impurities in hydrofluoric acid into compounds with high boiling points, so that the subsequent rectification system can further separate hydrofluoric acid and the compounds of impurities to achieve the effect of treating hydrofluoric acid. In the above oxidation process, the equivalent of the oxidizing agent needs to be controlled so that the oxidizing agent is sufficient to continuously oxidize the impurities in the hydrofluoric acid. However, in order to confirm the oxidant equivalent in hydrofluoric acid, it is necessary to carry out on-site staged manual sampling for testing. This not only takes a lot of time and labor costs, but also causes danger to the on-site operators. Therefore, how to safely and conveniently monitor the oxidant equivalent in the hydrofluoric acid treatment process is a problem to be solved in related fields.

根據本公開的一實施方式,一種氫氟酸處理監控系統包括處理槽,其中處理槽包括氫氟酸注入口、氧化劑注入口、回流注入口和出口處。氫氟酸處理監控系統還包括連接至處理槽的出口處的流體管線,以及連接流體管線和處理槽的回流注入口的回流管,其中回流管包括透明視窗。氫氟酸處理監控系統還包括用以拍攝回流管的透明視窗以獲得影像的攝影機、用以判讀影像的色彩飽和度的影像辨識單元,以及用以在色彩飽和度低於色彩飽和度標準值時發出提示的監控單元。According to an embodiment of the present disclosure, a hydrofluoric acid treatment monitoring system includes a treatment tank, wherein the treatment tank includes a hydrofluoric acid injection port, an oxidant injection port, a reflux injection port and an outlet. The hydrofluoric acid treatment monitoring system also includes a fluid pipeline connected to the outlet of the treatment tank, and a return pipe connecting the fluid pipeline and the return flow inlet of the treatment tank, wherein the return pipe includes a transparent window. The hydrofluoric acid treatment monitoring system also includes a camera for shooting the transparent window of the return pipe to obtain an image, an image recognition unit for judging the color saturation of the image, and an image recognition unit for judging the color saturation of the image when the color saturation is lower than the standard value of the color saturation. A monitoring unit that issues prompts.

在一些實施方式中,氫氟酸處理監控系統更包括用以控制氫氟酸注入口和氧化劑注入口的控制單元。In some embodiments, the hydrofluoric acid treatment monitoring system further includes a control unit for controlling the hydrofluoric acid injection port and the oxidant injection port.

在一些實施方式中,氫氟酸處理監控系統更包括連接至影像辨識單元、控制單元和監控單元的管理單元,其中管理單元用以根據影像的色彩飽和度向控制單元和監控單元發出指令。In some embodiments, the hydrofluoric acid treatment monitoring system further includes a management unit connected to the image recognition unit, the control unit and the monitoring unit, wherein the management unit is used to send instructions to the control unit and the monitoring unit according to the color saturation of the image.

在一些實施方式中,回流管位於透明視窗的管徑介於1吋至2吋之間。In some embodiments, the diameter of the return pipe located at the transparent window is between 1 inch and 2 inches.

在一些實施方式中,透明視窗包括含氟樹脂。In some embodiments, the transparent window includes a fluororesin.

根據本公開的一實施方式,一種監控氫氟酸處理的方法包括以下步驟。將氫氟酸和第一劑量的氧化劑注入處理槽中,以形成氫氟酸混合液。使氫氟酸混合液經由回流管回流至處理槽中,其中回流管包括透明視窗。拍攝回流管的透明視窗,以獲得氫氟酸混合液的影像。藉由影像辨識單元判讀影像的色彩飽和度,且比較色彩飽和度和色彩飽和度標準值。當影像的色彩飽和度低於色彩飽和度標準值時,監控單元發出提示,且將第二劑量的氧化劑注入處理槽中。According to an embodiment of the present disclosure, a method of monitoring hydrofluoric acid treatment includes the following steps. Hydrofluoric acid and a first dose of oxidant are injected into the treatment tank to form a hydrofluoric acid mixture. The hydrofluoric acid mixture is returned to the treatment tank through the return pipe, wherein the return pipe includes a transparent window. Photograph the clear window of the return line to obtain an image of the hydrofluoric acid mixture. The color saturation of the image is judged by the image recognition unit, and the color saturation is compared with a standard value of the color saturation. When the color saturation of the image is lower than the color saturation standard value, the monitoring unit sends out a prompt, and injects a second dose of oxidant into the processing tank.

在一些實施方式中,藉由影像辨識單元判讀影像的色彩飽和度包括藉由影像辨識單元判讀影像的RGB參數,以及將RGB參數轉換成HSV參數以獲得色彩飽和度。In some embodiments, judging the color saturation of the image by the image recognition unit includes judging RGB parameters of the image by the image recognition unit, and converting the RGB parameters into HSV parameters to obtain the color saturation.

在一些實施方式中,色彩飽和度標準值介於影像辨識單元可判讀的最大色彩飽和度的25%至30%之間。In some embodiments, the color saturation standard value is between 25% and 30% of the maximum color saturation that can be judged by the image recognition unit.

在一些實施方式中,藉由影像辨識單元判讀影像的色彩飽和度更包括隨時間連續判讀影像的色彩飽和度,且將連續判讀的色彩飽和度繪製成時間變化曲線。In some embodiments, judging the color saturation of the image by the image recognition unit further includes continuously judging the color saturation of the image over time, and plotting the continuously judging color saturation as a time-varying curve.

在一些實施方式中,氧化劑包括高錳酸離子。In some embodiments, the oxidizing agent includes permanganate ions.

為了實現提及主題的不同特徵,以下公開內容提供了許多不同的實施例或示例。以下描述組件、操作、配置等的具體示例以簡化本公開。當然,這些僅僅是示例,而不是限制性的。此外,為簡化圖式起見,一些習知慣用的結構與元件在圖式中將以簡單示意的方式繪示之。The following disclosure presents many different embodiments or examples in order to achieve the different features of the mentioned subject matter. Specific examples of components, operations, configurations, etc. are described below to simplify the present disclosure. Of course, these are examples only, not limiting. In addition, for the sake of simplifying the drawings, some well-known structures and components will be shown in a simple and schematic manner in the drawings.

本公開內容提供一種氫氟酸處理監控系統,以及使用此系統監控氫氟酸處理的方法。氫氟酸處理監控系統包括處理槽、連接處理槽的流體管線和回流管,其中回流管包括透明視窗。氫氟酸處理監控系統中的攝影機拍攝透明視窗中的氫氟酸混合液,並藉由影像辨識單元判讀氫氟酸混合液的色彩飽和度值,以判斷氫氟酸混合液中的氧化劑當量是否適量。由於處理槽、流體管線和回流管形成封閉的流體路徑,氫氟酸處理監控系統可以避免人工取樣的危險性。此外,攝影機和影像辨識單元連續監控色彩飽和度的變化,使得氫氟酸處理監控系統可以連續性監控而增加對製程的控制精確性。The present disclosure provides a hydrofluoric acid treatment monitoring system and a method of monitoring hydrofluoric acid treatment using the system. The hydrofluoric acid treatment monitoring system includes a treatment tank, a fluid pipeline connected to the treatment tank and a return pipe, wherein the return pipe includes a transparent window. The camera in the hydrofluoric acid treatment monitoring system shoots the hydrofluoric acid mixture in the transparent window, and uses the image recognition unit to interpret the color saturation value of the hydrofluoric acid mixture to determine whether the oxidant equivalent in the hydrofluoric acid mixture is Appropriate amount. The hydrofluoric acid process monitoring system eliminates the hazards of manual sampling due to the closed fluid path formed by the process tank, fluid lines, and return lines. In addition, the camera and image recognition unit continuously monitor the change of color saturation, so that the hydrofluoric acid treatment monitoring system can continuously monitor and increase the control accuracy of the process.

依據本公開的一實施方式,第1圖繪示氫氟酸處理監控系統10的示意圖。氫氟酸處理監控系統10包括處理槽100、流體管線120、回流管130、攝影機140、影像辨識單元150以及監控單元160。According to an embodiment of the present disclosure, FIG. 1 shows a schematic diagram of a hydrofluoric acid treatment monitoring system 10 . The hydrofluoric acid treatment monitoring system 10 includes a treatment tank 100 , a fluid pipeline 120 , a return pipe 130 , a camera 140 , an image recognition unit 150 and a monitoring unit 160 .

處理槽100用於裝載液體,使得氫氟酸可以在處理槽100中進行處理製程(或可稱為前處理(pretreatment)製程)。具體而言,處理槽100包括氫氟酸注入口102、氧化劑注入口104、回流注入口106以及出口處108。在處理製程期間,氫氟酸110由氫氟酸注入口102注入處理槽100,而氧化劑115由氧化劑注入口104注入處理槽100。氫氟酸110和氧化劑115在處理槽100中充分混和,使得氧化劑115與氫氟酸110形成氫氟酸混合液,從而將氫氟酸110中的不純物氧化成更容易在後續製程中移除的化合物。The treatment tank 100 is used for loading liquid, so that hydrofluoric acid can perform a treatment process (or may be called a pretreatment process) in the treatment tank 100 . Specifically, the treatment tank 100 includes a hydrofluoric acid injection port 102 , an oxidant injection port 104 , a backflow injection port 106 and an outlet 108 . During the treatment process, hydrofluoric acid 110 is injected into the treatment tank 100 from the hydrofluoric acid injection port 102 , and an oxidant 115 is injected into the treatment tank 100 from the oxidant injection port 104 . The hydrofluoric acid 110 and the oxidizing agent 115 are fully mixed in the treatment tank 100, so that the oxidizing agent 115 and the hydrofluoric acid 110 form a hydrofluoric acid mixture, thereby oxidizing the impurities in the hydrofluoric acid 110 to be more easily removed in subsequent processes compound.

流體管線120連接至處理槽100的出口處108,以將氫氟酸混合液導引至處理槽100外部。舉例而言,流體管線120可以將經過處理的氫氟酸混合液導引至後續的精餾系統190,從而透過精餾移除氫氟酸混合液中經氧化的不純物。在一些實施方式中,流體管線120可以與泵浦125連接,從而透過泵浦125的壓力導引氫氟酸混合液的流向。The fluid line 120 is connected to the outlet 108 of the treatment tank 100 to guide the hydrofluoric acid mixture to the outside of the treatment tank 100 . For example, the fluid line 120 can guide the treated hydrofluoric acid mixture to the subsequent rectification system 190 , so as to remove oxidized impurities in the hydrofluoric acid mixture through rectification. In some embodiments, the fluid line 120 can be connected with the pump 125 so that the flow of the hydrofluoric acid mixture can be guided by the pressure of the pump 125 .

回流管130連接流體管線120和處理槽100的回流注入口106,以將流經流體管線120的氫氟酸混合液導引至回流管130中。詳細而言,回流管130連接流體管線120的一端可具有開關閥,以控制氫氟酸混合液進入回流管130或在流體管線120中繼續前進的流向。氫氟酸混合液流經回流管130之後,由回流注入口106回到處理槽100中。The return pipe 130 connects the fluid line 120 and the return flow inlet 106 of the treatment tank 100 to guide the hydrofluoric acid mixture flowing through the fluid line 120 into the return pipe 130 . In detail, the end of the return pipe 130 connected to the fluid line 120 may have a switch valve to control the flow direction of the hydrofluoric acid mixture entering the return pipe 130 or continuing in the fluid line 120 . After the hydrofluoric acid mixture flows through the return pipe 130 , it returns to the processing tank 100 through the return injection port 106 .

此外,回流管130包括透明視窗132,從而可以透過透明視窗132觀察回流管130中的氫氟酸混合液。換而言之,透過透明視窗132可以觀察流體管線120與處理槽100中的氫氟酸混合液。這樣封閉的回流管線設計使得操作者可以直接透過回流管130觀察處理槽100中正在進行處理的氫氟酸混合液,而無須開啟管線進行氫氟酸混合液的人工取樣。因此,具有透明視窗132的回流管130可以避免人工取樣的危險性。此外,透過回流管130可以連續觀察氫氟酸混合液,從而提升監控氫氟酸處理製程的精準度。In addition, the return pipe 130 includes a transparent window 132 , so that the hydrofluoric acid mixture in the return pipe 130 can be observed through the transparent window 132 . In other words, the fluid pipeline 120 and the hydrofluoric acid mixture in the treatment tank 100 can be observed through the transparent window 132 . Such a closed return pipeline design allows the operator to directly observe the hydrofluoric acid mixture being processed in the treatment tank 100 through the return pipe 130 without opening the pipeline for manual sampling of the hydrofluoric acid mixture. Therefore, the return pipe 130 with the transparent window 132 can avoid the danger of manual sampling. In addition, the hydrofluoric acid mixture can be continuously observed through the return pipe 130, thereby improving the accuracy of monitoring the hydrofluoric acid treatment process.

在一些實施方式中,回流管130位於透明視窗132的管徑可以介於1吋至2吋之間,使得流經透明視窗132處的氫氟酸混合液足以代表整個回流管130中的氫氟酸混合液狀態。進一步而言,流經透明視窗132處的氫氟酸混合液足以代表流體管線120和處理槽100中的氫氟酸混合液狀態,從而監控處理槽100中進行處理製程的氫氟酸混合液。在一些實施方式中,透明視窗132可以包括含氟樹脂,使得透明視窗132具有足夠的透光度,且降低氫氟酸混合液對透明視窗132的侵蝕。In some embodiments, the pipe diameter of the return pipe 130 located at the transparent window 132 can be between 1 inch and 2 inches, so that the hydrofluoric acid mixture flowing through the transparent window 132 is sufficient to represent the hydrofluoric acid in the entire return pipe 130 Acid mixture state. Furthermore, the hydrofluoric acid mixture flowing through the transparent window 132 is sufficient to represent the state of the hydrofluoric acid mixture in the fluid pipeline 120 and the treatment tank 100 , so as to monitor the hydrofluoric acid mixture in the treatment tank 100 for the treatment process. In some embodiments, the transparent window 132 may include fluorine-containing resin, so that the transparent window 132 has sufficient light transmittance, and reduces the erosion of the hydrofluoric acid mixture on the transparent window 132 .

攝影機140和影像辨識單元150用於觀察回流管130中的氫氟酸混合液。具體而言,攝影機140的鏡頭對準回流管130的透明視窗132,從而拍攝透明視窗132以獲得氫氟酸混合液的影像。接著,攝影機140將影像傳遞至影像辨識單元150,使影像辨識單元150判讀影像中的氫氟酸混合液狀態。The camera 140 and the image recognition unit 150 are used to observe the hydrofluoric acid mixture in the return pipe 130 . Specifically, the lens of the camera 140 is aimed at the transparent window 132 of the return pipe 130 , so as to shoot the transparent window 132 to obtain an image of the hydrofluoric acid mixture. Next, the camera 140 transmits the image to the image recognition unit 150, so that the image recognition unit 150 interprets the state of the hydrofluoric acid mixture in the image.

更具體而言,當氫氟酸混合液包括氧化劑115時,氫氟酸混合液可以呈現非透明的顏色。例如,當氧化劑115包括高錳酸離子時,氫氟酸混合液將呈現淺綠色。此外,當氫氟酸混合液中的氧化劑115的當量上升時,氫氟酸混合液的顏色將具有更高的色彩飽和度。因此,攝影機140透過透明視窗132拍攝氫氟酸混合液的影像後,影像辨識單元150可以透過影像判讀氫氟酸混合液的色彩飽和度,從而判斷氫氟酸混合液中的氧化劑當量是否適量。More specifically, when the hydrofluoric acid mixture includes the oxidizing agent 115, the hydrofluoric acid mixture may exhibit a non-transparent color. For example, when the oxidizing agent 115 includes permanganate ions, the hydrofluoric acid mixture will appear light green. In addition, when the equivalent of the oxidizing agent 115 in the hydrofluoric acid mixed liquid increases, the color of the hydrofluoric acid mixed liquid will have higher color saturation. Therefore, after the camera 140 captures the image of the hydrofluoric acid mixture through the transparent window 132, the image recognition unit 150 can judge the color saturation of the hydrofluoric acid mixture through the image, so as to determine whether the oxidant equivalent in the hydrofluoric acid mixture is appropriate.

監控單元160用於監控處理槽100中的氫氟酸混合液狀態。具體而言,氫氟酸處理監控系統10中可設定色彩飽和度標準值,此標準值對應氫氟酸混合液中應具有的氧化劑115的最低當量。換而言之,當氫氟酸混合液的色彩飽和度低於所設定的色彩飽和度標準值時,即代表處理槽100中的氧化劑115的當量不足以將氫氟酸110中的不純物繼續氧化成更容易移除的化合物。此時,監控單元160將發出提示,提醒操作者或系統增加處理槽100中的氧化劑115的當量。The monitoring unit 160 is used for monitoring the state of the hydrofluoric acid mixture in the treatment tank 100 . Specifically, the standard value of color saturation can be set in the hydrofluoric acid treatment monitoring system 10 , and this standard value corresponds to the minimum equivalent of the oxidizing agent 115 that should exist in the hydrofluoric acid mixture. In other words, when the color saturation of the hydrofluoric acid mixture is lower than the set color saturation standard value, it means that the equivalent of the oxidizing agent 115 in the treatment tank 100 is not enough to continue to oxidize the impurities in the hydrofluoric acid 110 into compounds that are easier to remove. At this point, the monitoring unit 160 will issue a prompt to remind the operator or the system to increase the equivalent of the oxidizing agent 115 in the treatment tank 100 .

在一些實施方式中,氫氟酸處理監控系統10可以更包括控制單元170,例如分散式控制系統(distributed control system,DCS)。控制單元170可用於電腦化控制氫氟酸混合液的處理製程。具體而言,控制單元170可以控制氫氟酸注入口102和氧化劑注入口104的開關,從而控制注入處理槽100的氫氟酸110和氧化劑115的液體量。此外,控制單元170可以控制氫氟酸處理監控系統10中的氫氟酸混合液流向與流速,從而控制處理製程的始末點。In some embodiments, the hydrofluoric acid treatment monitoring system 10 may further include a control unit 170 such as a distributed control system (distributed control system, DCS). The control unit 170 can be used for computerized control of the treatment process of the hydrofluoric acid mixture. Specifically, the control unit 170 can control the opening and closing of the hydrofluoric acid injection port 102 and the oxidant injection port 104 , so as to control the liquid amounts of the hydrofluoric acid 110 and the oxidant 115 injected into the treatment tank 100 . In addition, the control unit 170 can control the flow direction and flow rate of the hydrofluoric acid mixture in the hydrofluoric acid treatment monitoring system 10 , so as to control the start and end points of the treatment process.

在一些實施方式中,氫氟酸處理監控系統10可以更包括管理單元180,例如即時生產管理系統(real-time production management system,RTPMS)。具體而言,管理單元180連接至影像辨識單元150、控制單元170和監控單元160,使得管理單元180可以調節氫氟酸處理監控系統10中的各個單元。舉例而言,管理單元180可以收集影像辨識單元150所判讀的色彩飽和度,並且呈現色彩飽和度隨時間的變化曲線。管理單元180也可以根據所判讀的色彩飽和度向控制單元170或監控單元160發出指令。例如,當氫氟酸混合液的色彩飽和度低於色彩飽和度標準值時,管理單元180可以向監控單元160發出指令,使監控單元160發出提示;管理單元180還可以向控制單元170發出指令,使控制單元170開啟氧化劑注入口104而增加處理槽100中的氧化劑當量。In some embodiments, the hydrofluoric acid treatment monitoring system 10 may further include a management unit 180 such as a real-time production management system (RTPMS). Specifically, the management unit 180 is connected to the image recognition unit 150 , the control unit 170 and the monitoring unit 160 , so that the management unit 180 can adjust each unit in the hydrofluoric acid treatment monitoring system 10 . For example, the management unit 180 can collect the color saturation interpreted by the image recognition unit 150 and present a curve of the color saturation over time. The management unit 180 may also issue instructions to the control unit 170 or the monitoring unit 160 according to the interpreted color saturation. For example, when the color saturation of the hydrofluoric acid mixture is lower than the color saturation standard value, the management unit 180 can send an instruction to the monitoring unit 160 to make the monitoring unit 160 issue a prompt; the management unit 180 can also send an instruction to the control unit 170 , so that the control unit 170 opens the oxidant injection port 104 to increase the oxidant equivalent in the treatment tank 100 .

依據本公開的一實施方式,第2圖繪示監控氫氟酸處理的方法200的流程圖。方法200包括步驟202至步驟212。在步驟202中,形成氫氟酸混合液。在步驟204中,回流氫氟酸混合液。在步驟206中,拍攝氫氟酸混合液以獲得的影像。在步驟208中,判讀影像的色彩飽和度。在步驟210至步驟212中,根據色彩飽和度決定是否再添加氫氟酸混合液中的氧化劑。在以下敘述中,將結合第1圖和第2圖進一步說明上述各步驟。FIG. 2 depicts a flowchart of a method 200 for monitoring hydrofluoric acid treatment, according to an embodiment of the present disclosure. Method 200 includes step 202 to step 212 . In step 202, a hydrofluoric acid mixture is formed. In step 204, the hydrofluoric acid mixture is refluxed. In step 206, the obtained image is captured by shooting the hydrofluoric acid mixture. In step 208, the color saturation of the image is judged. In step 210 to step 212, it is determined whether to add the oxidizing agent in the hydrofluoric acid mixture according to the color saturation. In the following description, the above steps will be further described in conjunction with FIG. 1 and FIG. 2 .

在步驟202中,將氫氟酸和第一劑量的氧化劑注入處理槽中,以形成氫氟酸混合液。具體而言,藉由控制單元170開啟處理槽100的氫氟酸注入口102和氧化劑注入口104,使得單批次的氫氟酸110和第一劑量的氧化劑115注入處理槽100中以進行處理製程。在一些實施方式中,處理製程包括令氧化劑115氧化氫氟酸110中的不純物,例如含砷的化合物。此被氧化的含砷的化合物可以在後續精餾製程中被移除,使得經過處理製程和後續精餾製程的氫氟酸110可以達到電子級的標準。舉例而言,氧化劑115可以包括高錳酸離子。在上述實施方式中,包括氧化劑115的氫氟酸混合液可以呈現淺綠色。In step 202, hydrofluoric acid and a first dose of oxidant are injected into the treatment tank to form a hydrofluoric acid mixture. Specifically, the hydrofluoric acid injection port 102 and the oxidant injection port 104 of the treatment tank 100 are opened by the control unit 170, so that a single batch of hydrofluoric acid 110 and a first dose of oxidant 115 are injected into the treatment tank 100 for processing Process. In some embodiments, the treatment process includes causing the oxidizing agent 115 to oxidize impurities in the hydrofluoric acid 110 , such as arsenic-containing compounds. The oxidized arsenic-containing compounds can be removed in the subsequent rectification process, so that the hydrofluoric acid 110 after the treatment process and the subsequent rectification process can reach the standard of electronic grade. For example, the oxidizing agent 115 may include permanganate ions. In the above embodiments, the hydrofluoric acid mixture including the oxidizing agent 115 may appear light green.

在步驟204中,使氫氟酸混合液經由回流管回流至處理槽中。具體而言,未完成處理製程的氫氟酸混合液離開處理槽100後會進入流體管線120,且進一步經由回流管130回流至處理槽100中以繼續進行處理製程。In step 204, the hydrofluoric acid mixture is returned to the treatment tank through the return pipe. Specifically, the hydrofluoric acid mixture that has not completed the treatment process will enter the fluid pipeline 120 after leaving the treatment tank 100 , and further flow back into the treatment tank 100 through the return pipe 130 to continue the treatment process.

在步驟206中,拍攝回流管的透明視窗,以獲得氫氟酸混合液的影像。具體而言,回流管130包括透明視窗132,從而可以從回流管130外部直接觀察回流管130中的氫氟酸混合液。因此,攝影機140可以透過拍攝回流管130的透明視窗132而獲得氫氟酸混合液的影像。由於攝影機140透過透明視窗132拍攝氫氟酸混合液,氫氟酸處理監控系統10可以透過攝影機140持續拍攝氫氟酸混合液,進而連續性監控氫氟酸混合液的狀態。In step 206, the transparent window of the return pipe is photographed to obtain an image of the hydrofluoric acid mixture. Specifically, the return pipe 130 includes a transparent window 132 , so that the hydrofluoric acid mixture in the return pipe 130 can be directly observed from the outside of the return pipe 130 . Therefore, the camera 140 can capture the image of the hydrofluoric acid mixture through the transparent window 132 of the return pipe 130 . Since the camera 140 takes pictures of the hydrofluoric acid mixture through the transparent window 132, the hydrofluoric acid treatment monitoring system 10 can continuously take pictures of the hydrofluoric acid mixture through the camera 140, thereby continuously monitoring the state of the hydrofluoric acid mixture.

在步驟208中,藉由影像辨識單元判讀影像的色彩飽和度。具體而言,攝影機140拍攝影像之後,影像辨識單元150可以判讀影像中的氫氟酸混合液的色彩飽和度。氫氟酸混合液的色彩飽和度對應於氫氟酸混合液中的氧化劑當量,從而為氫氟酸處理監控系統10提供是否添加氧化劑的判斷依據。In step 208, the color saturation of the image is judged by the image recognition unit. Specifically, after the camera 140 captures the image, the image recognition unit 150 can judge the color saturation of the hydrofluoric acid mixture in the image. The color saturation of the hydrofluoric acid mixed liquid corresponds to the oxidant equivalent in the hydrofluoric acid mixed liquid, thereby providing the hydrofluoric acid treatment monitoring system 10 with a basis for judging whether to add an oxidant.

在一些實施方式中,影像辨識單元150判讀影像的色彩飽和度可以包括先判讀影像的三原色紅綠藍(red-green-blue,RGB)參數。接著,影像辨識單元150將RGB參數轉換成色相-飽和度-明度(hue-saturation-value,HSV)參數,並且將飽和度參數進行標準化而獲得影像的色彩飽和度。舉例而言,標準化後的色彩飽和度可以介於0至255之間。In some implementations, the image recognition unit 150 judging the color saturation of the image may include first judging three primary colors red-green-blue (RGB) parameters of the image. Next, the image recognition unit 150 converts the RGB parameters into hue-saturation-value (HSV) parameters, and normalizes the saturation parameters to obtain the color saturation of the image. For example, the normalized color saturation can be between 0 and 255.

在一些實施方式中,判讀影像的色彩飽和度可以更包括隨時間連續判讀影像的色彩飽和度,且將連續判讀的色彩飽和度繪製成時間變化曲線。第3圖依據本公開的依實施方式繪示影像的色彩飽和度隨時間變化的曲線圖。如第3圖所示,當氫氟酸和第一劑量的氧化劑混合後,氫氟酸混合液中的氧化劑的當量最高,此時氫氟酸混合液的色彩飽和度上升成最大值,即對應第一波峰310的位置。隨著處理製程的進行,氫氟酸混合液中的氧化劑的當量逐漸降低,因此氫氟酸混合液的色彩飽和度也逐漸下降。In some embodiments, judging the color saturation of the image may further include continuously judging the color saturation of the image over time, and plotting the continuously judging color saturation as a time-varying curve. FIG. 3 is a graph showing color saturation of an image as a function of time according to an embodiment of the present disclosure. As shown in Figure 3, when hydrofluoric acid is mixed with the first dose of oxidizing agent, the equivalent of the oxidizing agent in the hydrofluoric acid mixed solution is the highest, and the color saturation of the hydrofluoric acid mixed solution rises to the maximum value at this time, that is, the corresponding The position of the first peak 310. With the progress of the treatment process, the equivalent of the oxidizing agent in the hydrofluoric acid mixed solution gradually decreases, so the color saturation of the hydrofluoric acid mixed solution also gradually decreases.

在步驟210中,比較影像的色彩飽和度和色彩飽和度標準值,以判斷色彩飽和度是否低於色彩飽和度標準值。具體而言,先在氫氟酸處理監控系統10中設定色彩飽和度標準值,此標準值對應氧化氫氟酸混合液中的不純物所應有的氧化劑115的最低當量。In step 210, the color saturation of the image is compared with the color saturation standard value to determine whether the color saturation is lower than the color saturation standard value. Specifically, a standard value of color saturation is firstly set in the hydrofluoric acid treatment monitoring system 10, and this standard value corresponds to the minimum equivalent of the oxidizing agent 115 for oxidizing impurities in the hydrofluoric acid mixed solution.

在一些實施方式中,色彩飽和度標準值可以來自於使用氫氟酸處理監控系統10之前的實驗結果。具體而言,在氫氟酸中加入不同當量的氧化劑,接著取出部分的氫氟酸混合液並加入水以形成氫氟酸混合液樣品。當氫氟酸混合液中具有過量的氧化劑時,加水後的氫氟酸混合液樣品將呈現深色。當氫氟酸混合液中具有適量的氧化劑時,加水後的氫氟酸混合液樣品將呈現淺色。當氫氟酸混合液中具有不足的氧化劑時,加水後的氫氟酸混合液樣品將呈現無色。將具有過量、適量和不足的氧化劑當量的氫氟酸混合液放入氫氟酸處理監控系統10,並使用攝影機140和影像辨識單元150判讀不同狀態下的氫氟酸混合液的色彩飽和度。結果而言,具有適量氧化劑當量的氫氟酸混合液的色彩飽和度可作為色彩飽和度標準值。In some embodiments, the color saturation standard value can be obtained from the experimental results before treating the monitoring system 10 with hydrofluoric acid. Specifically, different equivalents of oxidizing agents are added to hydrofluoric acid, and then part of the hydrofluoric acid mixture is taken out and water is added to form a sample of the hydrofluoric acid mixture. When there is excessive oxidizing agent in the hydrofluoric acid mixed solution, the hydrofluoric acid mixed solution sample after adding water will present dark color. When there is an appropriate amount of oxidant in the hydrofluoric acid mixture, the hydrofluoric acid mixture sample after adding water will appear light-colored. When there is insufficient oxidizing agent in the hydrofluoric acid mixed solution, the hydrofluoric acid mixed solution sample after adding water will appear colorless. Put the hydrofluoric acid mixture with excessive, proper and insufficient oxidant equivalents into the hydrofluoric acid treatment monitoring system 10, and use the camera 140 and the image recognition unit 150 to interpret the color saturation of the hydrofluoric acid mixture in different states. As a result, the color saturation of the hydrofluoric acid mixture with an appropriate amount of oxidant equivalent can be used as the standard value of color saturation.

值得說明的是,在較佳的實施方式中,監控氫氟酸混合液的目標可以是將氫氟酸混合液的色彩飽和度維持在稍微高於色彩飽和度標準值,例如將氫氟酸混合液的色彩飽和度維持在比色彩飽和度標準值大於約5%至10%。此時的氫氟酸混合液中具有適當過量的氧化劑當量,使得氫氟酸混合液中的氧化劑當量足以對氫氟酸進行處理製程,同時避免過量的氧化劑影響產品品質。It is worth noting that, in a preferred embodiment, the goal of monitoring the hydrofluoric acid mixture can be to maintain the color saturation of the hydrofluoric acid mixture at slightly higher than the color saturation standard value, such as mixing the hydrofluoric acid The color saturation of the liquid is maintained at about 5% to 10% greater than the color saturation standard value. At this time, the hydrofluoric acid mixed solution has an appropriate excess oxidant equivalent, so that the oxidant equivalent in the hydrofluoric acid mixed solution is sufficient to process the hydrofluoric acid, while avoiding the excessive oxidant from affecting product quality.

在一些實施方式中,色彩飽和度標準值可以介於影像辨識單元可判讀的最大色彩飽和度的約25%至30%之間。舉例而言,當影像辨識單元可判讀的色彩飽和度範圍介於0至255之間時,色彩飽和度標準值可以在約60至75的範圍內。在一些實施方式中,當氫氟酸混合液具有不足的氧化劑當量時,氫氟酸混合液的色彩飽和度可以介於影像辨識單元可判讀的最大色彩飽和度的約20%至24%之間。In some embodiments, the color saturation standard value may be between about 25% and 30% of the maximum color saturation that can be interpreted by the image recognition unit. For example, when the range of color saturation that can be judged by the image recognition unit is between 0 and 255, the standard value of color saturation may be in the range of about 60 to 75. In some embodiments, when the hydrofluoric acid mixed solution has insufficient oxidant equivalent, the color saturation of the hydrofluoric acid mixed solution can be between about 20% and 24% of the maximum color saturation that can be interpreted by the image recognition unit .

若影像的色彩飽和度低於色彩飽和度標準值時,則前進至步驟212,使監控單元發出提示,並且將第二劑量的氧化劑注入處理槽中。具體而言,當影像的色彩飽和度低於色彩飽和度標準值時,監控單元160將發出提示,提醒操作者或氫氟酸處理監控系統10應增加氧化劑當量。同時,控制單元170可開啟處理槽100的氧化劑注入口104,使得第二劑量的氧化劑115注入處理槽100中。在第二劑量的氧化劑115注入處理槽100後,回到方法200的步驟206而繼續監控氫氟酸混合液的色彩飽和度直到氫氟酸處理製程結束。If the color saturation of the image is lower than the color saturation standard value, the process proceeds to step 212 , the monitoring unit issues a prompt, and a second dose of oxidant is injected into the processing tank. Specifically, when the color saturation of the image is lower than the color saturation standard value, the monitoring unit 160 will issue a prompt to remind the operator or the hydrofluoric acid treatment monitoring system 10 to increase the oxidant equivalent. At the same time, the control unit 170 may open the oxidant injection port 104 of the treatment tank 100 , so that the second dose of oxidant 115 is injected into the treatment tank 100 . After the second dose of oxidant 115 is injected into the treatment tank 100 , return to step 206 of the method 200 and continue to monitor the color saturation of the hydrofluoric acid mixture until the hydrofluoric acid treatment process is completed.

在一些實施方式中,第二劑量的氧化劑115實質上是補足第一劑量的氧化劑115的不足,因此氧化劑115的第二劑量可以小於第一劑量。舉例而言,參考第3圖,在時間t1時,氫氟酸中加入第一劑量的氧化劑後,氫氟酸混合液的色彩飽和度上升至第一波峰310。隨著反應持續進行,氫氟酸混合液的色彩飽和度隨時間逐漸降低,其中的氧化劑成分也隨之消耗。在時間t2時,色彩飽和度低於色彩飽和度標準值(在此示例中為影像辨識單元可判讀的最大色彩飽和度的25%)時,表示氧化劑已消耗至不足以讓反應繼續進行,故氫氟酸處理監控系統將第二劑量的氧化劑加入氫氟酸混合液中,使得在時間t3時的色彩飽和度上升至第二波峰320。由於氧化劑的第二劑量可以小於第一劑量,第二波峰320的高度低於第一波峰310的高度。In some embodiments, the second dose of oxidizing agent 115 substantially complements the deficiency of the first dose of oxidizing agent 115, so the second dose of oxidizing agent 115 may be less than the first dose. For example, referring to FIG. 3 , at time t1, after the first dose of oxidant is added to the hydrofluoric acid, the color saturation of the hydrofluoric acid mixture rises to a first peak 310 . As the reaction continues, the color saturation of the hydrofluoric acid mixture gradually decreases with time, and the oxidizing agent therein is also consumed. At time t2, when the color saturation is lower than the color saturation standard value (in this example, 25% of the maximum color saturation that can be interpreted by the image recognition unit), it means that the oxidant has been consumed enough to allow the reaction to continue, so The hydrofluoric acid treatment monitoring system adds a second dose of oxidant into the hydrofluoric acid mixture, so that the color saturation at time t3 rises to the second peak 320 . Since the second dose of oxidant may be smaller than the first dose, the height of the second peak 320 is lower than the height of the first peak 310 .

若影像的色彩飽和度未低於色彩飽和度標準值,則回到步驟206,使氫氟酸處理監控系統持續監控影像的色彩飽和度直到氫氟酸處理製程結束。一旦影像的色彩飽和度低於色彩飽和度標準值,則再次前進至步驟212,即在處理槽中再次注入氧化劑。If the color saturation of the image is not lower than the color saturation standard value, then return to step 206, so that the hydrofluoric acid treatment monitoring system continuously monitors the color saturation of the image until the hydrofluoric acid treatment process is completed. Once the color saturation of the image is lower than the color saturation standard value, proceed to step 212 again, that is, inject the oxidant into the processing tank again.

根據本公開上述實施方式,本公開的氫氟酸處理監控系統包括形成封閉流體路徑的處理槽、流體管線和回流管,其中回流管包括透明視窗。氫氟酸處理監控系統還包括拍攝透明視窗中的氫氟酸混合液的攝影機,並藉由影像辨識單元判讀氫氟酸混合液影像的色彩飽和度值,以判斷氫氟酸混合液中的氧化劑當量是否適量。由於本公開的氫氟酸處理監控系統包括封閉的流體路徑和可以連續監控色彩飽和度變化的單元,從而可以避免人工取樣的危險性,並且透過連續性監控而增加對處理製程的控制精確性。According to the above-mentioned embodiments of the present disclosure, the hydrofluoric acid treatment monitoring system of the present disclosure includes a treatment tank forming a closed fluid path, a fluid pipeline and a return pipe, wherein the return pipe includes a transparent window. The hydrofluoric acid treatment monitoring system also includes a camera that shoots the hydrofluoric acid mixture in the transparent window, and uses the image recognition unit to interpret the color saturation value of the hydrofluoric acid mixture image to determine the oxidant in the hydrofluoric acid mixture Whether the equivalent is appropriate. Since the hydrofluoric acid treatment monitoring system of the present disclosure includes a closed fluid path and a unit capable of continuously monitoring changes in color saturation, the danger of manual sampling can be avoided, and the control accuracy of the treatment process can be increased through continuous monitoring.

前面概述一些實施例的特徵,使得本領域技術人員可更好地理解本公開的觀點。本領域技術人員應該理解,他們可以容易地使用本公開作為設計或修改其他製程和結構的基礎,以實現相同的目的和/或實現與本文介紹之實施例相同的優點。本領域技術人員還應該理解,這樣的等同構造不脫離本公開的精神和範圍,並且在不脫離本公開的精神和範圍的情況下,可以進行各種改變、替換和變更。The foregoing outlines features of some embodiments so that those skilled in the art may better understand the aspects of the present disclosure. Those skilled in the art should appreciate that they may readily use the present disclosure as a basis for designing or modifying other processes and structures for carrying out the same purposes and/or achieving the same advantages as the embodiments described herein. Those skilled in the art should also understand that such equivalent constructions do not depart from the spirit and scope of the present disclosure, and that they can make various changes, substitutions and alterations without departing from the spirit and scope of the present disclosure.

10:氫氟酸處理監控系統 100:處理槽 102:氫氟酸注入口 104:氧化劑注入口 106:回流注入口 108:出口處 110:氫氟酸 115:氧化劑 120:流體管線 125:泵浦 130:回流管 132:透明視窗 140:攝影機 150:影像辨識單元 160:監控單元 170:控制單元 180:管理單元 190:精餾系統 200:方法 202,204,206,208,210,212:步驟 310:第一波峰 320:第二波峰 t1,t2,t3:時間10: Hydrofluoric acid treatment monitoring system 100: processing tank 102: Hydrofluoric acid injection port 104: Oxidizer injection port 106: Backflow inlet 108: Exit 110: hydrofluoric acid 115: Oxidizing agent 120: Fluid pipeline 125: pump 130: return pipe 132: transparent window 140: camera 150: Image recognition unit 160: Monitoring unit 170: control unit 180: Snap-in 190: Distillation system 200: method 202, 204, 206, 208, 210, 212: steps 310: The first crest 320:Second crest t1, t2, t3: time

當結合附圖閱讀時,從以下詳細描述中可以最好地理解本公開的各方面。應注意,根據工業中的標準方法,各種特徵未按比例繪製。實際上,為了清楚地討論,可任意增加或減少各種特徵的尺寸。 第1圖依據本公開的一實施方式繪示氫氟酸處理監控系統的示意圖。 第2圖依據本公開的一實施方式繪示監控氫氟酸處理的方法流程圖。 第3圖依據本公開的一實施方式繪示色彩飽和度的時間變化曲線圖。 Aspects of the disclosure are best understood from the following detailed description when read with the accompanying figures. It should be noted that, according to the standard practice in the industry, various features are not drawn to scale. In fact, the dimensions of the various features may be arbitrarily increased or decreased for clarity of discussion. FIG. 1 is a schematic diagram of a hydrofluoric acid treatment monitoring system according to an embodiment of the present disclosure. FIG. 2 is a flowchart illustrating a method for monitoring hydrofluoric acid treatment according to an embodiment of the present disclosure. FIG. 3 shows a time-varying graph of color saturation according to an embodiment of the present disclosure.

國內寄存資訊(請依寄存機構、日期、號碼順序註記) 無 國外寄存資訊(請依寄存國家、機構、日期、號碼順序註記) 無 Domestic deposit information (please note in order of depositor, date, and number) none Overseas storage information (please note in order of storage country, institution, date, and number) none

10:氫氟酸處理監控系統 10: Hydrofluoric acid treatment monitoring system

100:處理槽 100: processing tank

102:氫氟酸注入口 102: Hydrofluoric acid injection port

104:氧化劑注入口 104: Oxidizer injection port

106:回流注入口 106: Backflow inlet

108:出口處 108: Exit

110:氫氟酸 110: hydrofluoric acid

115:氧化劑 115: Oxidizing agent

120:流體管線 120: Fluid pipeline

125:泵浦 125: pump

130:回流管 130: return pipe

132:透明視窗 132: transparent window

140:攝影機 140: camera

150:影像辨識單元 150: Image recognition unit

160:監控單元 160: Monitoring unit

170:控制單元 170: control unit

180:管理單元 180: Snap-in

190:精餾系統 190: Distillation system

Claims (10)

一種氫氟酸處理監控系統,包括: 一處理槽,包括一氫氟酸注入口、一氧化劑注入口、一回流注入口和一出口處; 一流體管線,連接至該處理槽的該出口處; 一回流管,連接該流體管線和該處理槽的該回流注入口,其中該回流管包括一透明視窗; 一攝影機,用以拍攝該回流管的該透明視窗以獲得一影像; 一影像辨識單元,用以判讀該影像的一色彩飽和度;以及 一監控單元,用以在該色彩飽和度低於一色彩飽和度標準值時發出提示。 A hydrofluoric acid treatment monitoring system, comprising: A treatment tank, including a hydrofluoric acid injection port, an oxidant injection port, a backflow injection port and an outlet; a fluid line connected to the outlet of the treatment tank; a return pipe, connecting the fluid line and the return inlet of the treatment tank, wherein the return pipe includes a transparent window; a camera, used to photograph the transparent window of the return pipe to obtain an image; an image recognition unit for judging a color saturation of the image; and A monitoring unit is used for sending a prompt when the color saturation is lower than a standard value of color saturation. 如請求項1所述之氫氟酸處理監控系統,進一步包括一控制單元,用以控制該氫氟酸注入口和該氧化劑注入口。The hydrofluoric acid treatment monitoring system as described in claim 1 further includes a control unit for controlling the hydrofluoric acid injection port and the oxidant injection port. 如請求項2所述之氫氟酸處理監控系統,進一步包括一管理單元,連接至該影像辨識單元、該控制單元和該監控單元,其中該管理單元用以根據該影像的該色彩飽和度向該控制單元和該監控單元發出指令。The hydrofluoric acid treatment monitoring system as described in claim 2, further comprising a management unit connected to the image recognition unit, the control unit and the monitoring unit, wherein the management unit is used to report to the user according to the color saturation of the image The control unit and the monitoring unit issue commands. 如請求項1所述之氫氟酸處理監控系統,其中該回流管位於該透明視窗的一管徑介於1吋至2吋之間。The hydrofluoric acid treatment monitoring system as described in Claim 1, wherein a pipe diameter of the return pipe located at the transparent window is between 1 inch and 2 inches. 如請求項1所述之氫氟酸處理監控系統,其中該透明視窗包括含氟樹脂。The hydrofluoric acid treatment monitoring system as described in Claim 1, wherein the transparent window includes fluorine-containing resin. 一種監控氫氟酸處理的方法,包括: 將一氫氟酸和一第一劑量的一氧化劑注入一處理槽中,以形成一氫氟酸混合液; 使該氫氟酸混合液經由一回流管回流至該處理槽中,其中該回流管包括一透明視窗; 拍攝該回流管的該透明視窗,以獲得該氫氟酸混合液的一影像; 藉由一影像辨識單元判讀該影像的一色彩飽和度,且比較該色彩飽和度和一色彩飽和度標準值;以及 當該影像的該色彩飽和度低於該色彩飽和度標準值時,一監控單元發出提示,且將一第二劑量的該氧化劑注入該處理槽中。 A method of monitoring hydrofluoric acid treatment comprising: injecting hydrofluoric acid and a first dose of an oxidizing agent into a treatment tank to form a hydrofluoric acid mixture; return the hydrofluoric acid mixture to the treatment tank through a return pipe, wherein the return pipe includes a transparent window; photographing the transparent window of the return pipe to obtain an image of the hydrofluoric acid mixture; Judging a color saturation of the image by an image recognition unit, and comparing the color saturation with a color saturation standard value; and When the color saturation of the image is lower than the color saturation standard value, a monitoring unit issues a prompt, and injects a second dose of the oxidant into the processing tank. 如請求項6所述之方法,其中藉由該影像辨識單元判讀該影像的該色彩飽和度包括: 藉由該影像辨識單元判讀該影像的一RGB參數;以及 將該RGB參數轉換成一HSV參數,以獲得該色彩飽和度。 The method according to claim 6, wherein judging the color saturation of the image by the image recognition unit includes: Deciphering an RGB parameter of the image by the image recognition unit; and Convert the RGB parameter to an HSV parameter to obtain the color saturation. 如請求項6所述之方法,其中該色彩飽和度標準值介於該影像辨識單元可判讀的一最大色彩飽和度的25%至30%之間。The method as claimed in claim 6, wherein the color saturation standard value is between 25% and 30% of a maximum color saturation that can be interpreted by the image recognition unit. 如請求項6所述之方法,其中藉由該影像辨識單元判讀該影像的該色彩飽和度進一步包括隨時間連續判讀該影像的該色彩飽和度,且將連續判讀的該色彩飽和度繪製成一時間變化曲線。The method as claimed in claim 6, wherein judging the color saturation of the image by the image recognition unit further comprises continuously judging the color saturation of the image over time, and plotting the continuously judging color saturation as a time Curve. 如請求項6所述之方法,其中該氧化劑包括高錳酸離子。The method of claim 6, wherein the oxidizing agent comprises permanganate ions.
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