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1、利用聚電解質加強電聚浮除法與超過濾處理化學機械研磨廢水之研究Treatment of Chemical Mechanical Polishing Wastewater by Polyelectrolyte Enhanced Electro-Coagulation-Flotation and Ultrafiltration Process 研究生：陳育婷Chen, Yu-Tin指導教授：黃益助Huang, Yi-Chu 【摘要 】在台灣高科技產業如半導體化學機械研磨(CMP) 製程，節約用水和廢水處理回收使用已成為一重要議題。在晶片平坦化過程中需要大量的超純水來去除CMP 研磨液與晶片上的粒狀物
2、質。這些從半導體產業所排放之含有奈米粒徑之CMP 廢水，若未經妥善處理將危害人體健康及環境。本研究目的主要在探討添加聚電解質(聚苯乙烯硫酸順丁烯二酸鈉鹽, PSSM)結合電聚浮除與超過濾程序處理 CMP 廢水之處理效率，試期有效降低CMP 廢水之濁度與金屬含量。本研究欲處理之廢水為金屬層化學機械研磨廢水（Cu-Chemical Mechanical Polishing Wastewater） ，其來源為台南科學園區某半導體工廠之實廠廢水。電聚浮除系統之電極板材質為鋁金屬，尺寸為 180 mm 80 m 1 mm ，有效極板面積為0.062 m2，以間距 15 mm固定四面鋁片於夾板上，反應槽置
3、入1.5 L 待處理水樣。在超過濾系統，所使用之薄膜材質為再生纖維，有效面積為 0.0045m2，分子量截斷點為10,000。以電聚浮除程序處理CMP 廢水，操作電壓10 V/cm 、導電度625 S/cm 、PSSM=0 mg/L 、電聚時間60 分鐘時，Cu 去除率可達96 %，Al 去除率為66.7 %，Si 去除率則可達99 %以上， 濁度去除率為80.3 %。未添加 PSSM之廢水經電聚浮除程序後所產生之膠羽，往往過於鬆散，導致其膠羽很容易因擾動而再度分離。在操作電壓10 V/cm 、 導電度489 S/cm，添加 PSSM 2 mg/L 、 電聚時間60 分鐘時， Cu 去除率可達
4、98.5 %， Al 去除率為93.4 %，Si 去除率將近100 %，濁度去除率為94.3 %。在電聚浮除程序當中添加PSSM，可藉架橋作用與水中懸浮膠羽結合，在電聚時間較短時，即可達較佳去除效率。由掃描式電子顯微鏡(SEM) 觀察經電聚浮除程序後所產生之污泥，可發現有添加PSSM 比未添加之廢水所產生之污泥，其膠羽體積較大且結構較為緊緻。在超過濾程序提升經電聚浮除處理(未添加 PSSM)後之滲透液中，當體積濃縮因子(VCF)=7 時，其 Cu 殘留濃度為 0.10 mg/L 左右， 濁度為 0.50 NTU ；而 Al 殘留濃度在電聚時間60 分鐘者較佳， 其殘留濃度為7.24 mg/L
5、；而在電聚時間45 分鐘再經超過濾處理後之Al 殘留濃度為16.0 mg/L 。 Si 殘留濃度則在經電聚浮除程序後皆低於儀器偵測極限值(MDL=0.5 mg/L)。在超過濾提升經添加PSSM 2mg/L 加強電聚浮除後之滲透液中，在VCF=7 ，其 Cu 平均殘留濃度為0.07-0.18 mg/L ，濁度為 0.45 NTU ，而 Al 平均殘留濃度為13.0 mg/L ；Si 殘留濃度在電聚浮除程序後已低於儀器偵測極限值(MDL=0.5 mg/L) 。本研究結合電聚浮除和超過濾程序可有效移除CMP 廢水中之濁度和金屬物質，可供CMP 廢水處理及回收再使用技術選擇之參考。關鍵字：化學機械研磨
6、廢水（Cu-CMP Wastewater ） 、聚苯乙烯硫酸順丁烯二酸鈉鹽(PSSM) 、電聚浮除、超過濾【Abstract 】Water conservation and wastewater reclamation have been an important issue of various hi-tech industries such as chemical mechanical polishing (CMP) process in semi-conductor industry in Taiwan. In smoothening processes of wafers, huge
7、amount of ultra-pure water is consumed to remove the CMP slurry and particles on wafers. Discharge of wastewater containing nano-particles from the semiconductor industry without proper treatments would have a great impact to human health and the environment. The objective of this research is to stu
8、dy the treatment efficiency of the addition of polyelectrolyte, poly (styrenesulfonic acid-co maleic acid) sodium (PSSM), coupled with the electro-coagulation-flotation (ECF) and ultrafiltration process to reduce the turbidity and metals from CMP wastewater. The Cu-CMP wastewater used in this study
9、was collected from a CMP process of a semiconductor factory in the Tainan Science Park located in southern Taiwan. The bench reactor contained 1.5 L wastewater in concern and four pieces of aluminum electrodes with 15 mm intervals between each plate. The size of each plate was 180 mm 8 mm 1 mm with
10、effective area of 0.062 m2. In the ultrafiltration system, the type of membrane used was regenerated cellulose with an effective area of 0.0045 m2and molecular weight cut-off of 10,000 daltons. In the absence of PSSM, the respective removal ratios of copper, aluminum, silicon, and turbidity were 96.
11、0 %, 66.7 %, 99.0 % and 80.3 % under the operation conditions of voltage 10 V/cm, conductivity 625 S/cm and time 60 minutes. Without PSSM addition, the flocs aggregated after ECF processes were loose and easily separated due to agitation. In the experiments of addition of PSSM 2 mg/L, the respective
12、 removal ratios of copper, aluminum, silicon, and turbidity were 98.5 %, 93.4 %, 100 % and 94.3 % under the operation conditions of voltage 10 V/cm, conductivity 489 S/cm and time 60 minutes. In ECF processes, PSSM addition enhanced the coagulation of polyelectrolyte and colloids by bridging mechani
13、sm that increased the removal efficiency under lower operation time. The settled sediments after ECF processes were observed via scanning electron microscope (SEM) indicated the volume and density of flocs with PSSM addition were higher than those without PSSM addition. In the experiments of ultrafi
14、ltration coupled with the ECF processes without PSSM addition, the copper, turbidity, and silicon concentration in permeate at volumetric concentration factor (VCF) 7 were around 0.10 mg/L, 0.5 NTU and below detection limit 0.5mg/L, respectively. Aluminum concentrations in the permeate at VCF of 7 w
15、ere 7.24 mg/L under operation time 60 minutes and 16.0 mg/L under operation time 45 minutes. However in the experiments of ultrafiltration coupled with the ECF processes with 2 mg/L PSSM addition, the copper, turbidity, aluminum, and silicon concentration in permeate at volumetric concentration fact
16、or (VCF) 7 were around 0.070.18 mg/L, 0.45 NTU, 13.0 mg/L, and below detection limit 0.5 mg/L, respectively. ECF coupled with ultrafiltration processes can effectively remove the turbidity and metals from the CMP wastewater and the results of this study can be referred as an alternative for treatment of CMP wastewater and possible reclamation as well as reuse of treated water. Keywords: chemical mechanical polishing, Poly (styrenesulfonic acid-co maleic acid) sodium (PSSM), elect
