A close-looped process based on the membrane separation and electrolysis is proposed to regenerate the copper etchant in-situ, recover copper on-site and reuse it. It is characterized by selective separation of copper...A close-looped process based on the membrane separation and electrolysis is proposed to regenerate the copper etchant in-situ, recover copper on-site and reuse it. It is characterized by selective separation of copper from the spent etchant, which is accomplished by the ion exchange membrane-electrowinning, and at the same time the other components useful for etching are reclaimed. The experiments show that at least 90 % of electricity efficiency for copper removal can be maintained and the optimum condition for membrane-electrowinning is: cell voltage 2 -2.5 V, operating temperature 40 - 50 ℃ and current density 500 - 1 500 A/m2. The regenerated etchant can be suc cessfully reused to etch copper after adjusting its composition to the normal range, and its recycling property is as good as that of the fresh etchant after 50 times of use-disposal-regeneration cycles.展开更多
The solvent extraction of copper from simulated ammoniacal spent etchant with 1-（4＇-dodecyl）-phenyl-3-tertiary butyl-1,3-octadione（HR） was studied,and a model of extraction isotherm was proposed and verified with...The solvent extraction of copper from simulated ammoniacal spent etchant with 1-（4＇-dodecyl）-phenyl-3-tertiary butyl-1,3-octadione（HR） was studied,and a model of extraction isotherm was proposed and verified with equilibrium extraction constant.The influence of equilibration time,extractant concentration and phase ratio on the extraction of copper was studied at（298±0.5） K.For the spent etching solutions containing 112.98 g/L Cu,6 mol/L NH3 and 1 mol/L NH4＋,the optimal solvent extraction condition of copper was obtained in one-stage solvent extraction at phase ratio of 5：4 with 40% HR in sulphonated kerosene for 5 min.The copper concentration in the raffinate decreased to 63.24 g/L and raffinate can be favorably recycled to the etching solution.The stripping studies were carried out with the simulated copper spent electrolyte containing 30 g/L Cu and 180 g/L H2SO4.The stripping ratio is 98.27% from the loaded organic phase after one-stage stripping at phase ratio of 1：2 at（298±0.5） K.展开更多
In order to protect the finished structures on the front side during deep silicon wet etching processes, the wax coating for double-sided etching process on the wafer is studied to separate the aforementioned structur...In order to protect the finished structures on the front side during deep silicon wet etching processes, the wax coating for double-sided etching process on the wafer is studied to separate the aforementioned structures from the strong aqueous bases. By way of heating and vacuumization, the air bubbles are expelled from the coating to extend the protection duration. The air pressure in the sealed chamber is 0.026 7 Pa, and the temperature of the heated wafer is 300℃. Two kinds of the wax are used, and the corresponding photos of the etched wafer and the protection times are given. In 75 ℃ 10 % KOH solution, the protection duration is more than 8 h.展开更多
Electrochemical technologies for the on-site treatment of spent acid etchant have received great attention due their ease of operation and economic benefits. On the other hand, a large amount of Cl2 is generated durin...Electrochemical technologies for the on-site treatment of spent acid etchant have received great attention due their ease of operation and economic benefits. On the other hand, a large amount of Cl2 is generated during the electrolysis process, which leads to potential environmental risks. In the present work, a novel threecompartment ceramic membrane flow reactor, including a cathode chamber, an anode chamber, and a gas absorption chamber was developed. The three chambers were divided by an Al2O3 ceramic membrane and a breathable hydrophobic anode diffusion electrode(ADE). The Cl2 evolution onset potential of the ADE was increased to 1.19 V from 1.05 V of the graphite felt, effectively inhibiting the chlorine evolution reaction(CER).The anode-generated Cl2 diffused into the gas absorption chamber through the ADE and was eventually consumed by the H2O2 adsorbent. Cu could be recovered without emitting chlorine due to the special structure of reactor. The current efficiency of copper precipitation and cathode reduction from Cu2+to Cu+reached 97.7%at a working current of 150 m A. These results indicated that the novel membrane reactor had high potential for application in the copper recovery industry.展开更多
采用光学显微镜和扫描电子显微镜对不同腐蚀剂腐蚀后的Mg-Nd-Zn-Zr镁合金铸态显微组织进行观察。结果表明,Mg-NdZn-Zr合金的铸态组织主要由α-Mg和晶界处的Mg_(12)(Nd,Zn)两相组成,另外还有小块状Mg12(Nd,Zn)相及近圆形的富Zr相区域。1...采用光学显微镜和扫描电子显微镜对不同腐蚀剂腐蚀后的Mg-Nd-Zn-Zr镁合金铸态显微组织进行观察。结果表明,Mg-NdZn-Zr合金的铸态组织主要由α-Mg和晶界处的Mg_(12)(Nd,Zn)两相组成,另外还有小块状Mg12(Nd,Zn)相及近圆形的富Zr相区域。1号传统腐蚀剂(4 m L硝酸+96 m L乙醇)可较好显示组织;经2号腐蚀剂(12 g苦味酸+80 m L乙酸+80 m L蒸馏水+350 m L乙醇)腐蚀5 s和10 s后,组织发黑,晶界不明显,但可部分显示出富Zr相区,延长腐蚀时间到20 s,晶粒显现出来,发黑现象得到缓解,富Zr区域明显,但晶界附近出现大量气泡;3号腐蚀剂(60 m L乙二醇+20 m L乙酸+19 m L蒸馏水+1 m L硝酸)腐蚀组织表明,其对晶粒的显示效果明显好于2号,然而很难观察到富Zr区域。展开更多
文摘A close-looped process based on the membrane separation and electrolysis is proposed to regenerate the copper etchant in-situ, recover copper on-site and reuse it. It is characterized by selective separation of copper from the spent etchant, which is accomplished by the ion exchange membrane-electrowinning, and at the same time the other components useful for etching are reclaimed. The experiments show that at least 90 % of electricity efficiency for copper removal can be maintained and the optimum condition for membrane-electrowinning is: cell voltage 2 -2.5 V, operating temperature 40 - 50 ℃ and current density 500 - 1 500 A/m2. The regenerated etchant can be suc cessfully reused to etch copper after adjusting its composition to the normal range, and its recycling property is as good as that of the fresh etchant after 50 times of use-disposal-regeneration cycles.
基金Project (2007CB613601) supported by the National Basic Research Program of China
文摘The solvent extraction of copper from simulated ammoniacal spent etchant with 1-（4＇-dodecyl）-phenyl-3-tertiary butyl-1,3-octadione（HR） was studied,and a model of extraction isotherm was proposed and verified with equilibrium extraction constant.The influence of equilibration time,extractant concentration and phase ratio on the extraction of copper was studied at（298±0.5） K.For the spent etching solutions containing 112.98 g/L Cu,6 mol/L NH3 and 1 mol/L NH4＋,the optimal solvent extraction condition of copper was obtained in one-stage solvent extraction at phase ratio of 5：4 with 40% HR in sulphonated kerosene for 5 min.The copper concentration in the raffinate decreased to 63.24 g/L and raffinate can be favorably recycled to the etching solution.The stripping studies were carried out with the simulated copper spent electrolyte containing 30 g/L Cu and 180 g/L H2SO4.The stripping ratio is 98.27% from the loaded organic phase after one-stage stripping at phase ratio of 1：2 at（298±0.5） K.
文摘In order to protect the finished structures on the front side during deep silicon wet etching processes, the wax coating for double-sided etching process on the wafer is studied to separate the aforementioned structures from the strong aqueous bases. By way of heating and vacuumization, the air bubbles are expelled from the coating to extend the protection duration. The air pressure in the sealed chamber is 0.026 7 Pa, and the temperature of the heated wafer is 300℃. Two kinds of the wax are used, and the corresponding photos of the etched wafer and the protection times are given. In 75 ℃ 10 % KOH solution, the protection duration is more than 8 h.
基金Supported by the National Natural Science Foundation of China(21838005,21676139)the Higher Education Natural Science Foundation of Jiangsu Province(15KJA530001)+1 种基金the Key Scientific Research and Development Projects of Jiangsu Province(BE201800901)Research Fund of State Key Laboratory of MaterialsOriented Chemical Engineering(ZK201604).
文摘Electrochemical technologies for the on-site treatment of spent acid etchant have received great attention due their ease of operation and economic benefits. On the other hand, a large amount of Cl2 is generated during the electrolysis process, which leads to potential environmental risks. In the present work, a novel threecompartment ceramic membrane flow reactor, including a cathode chamber, an anode chamber, and a gas absorption chamber was developed. The three chambers were divided by an Al2O3 ceramic membrane and a breathable hydrophobic anode diffusion electrode(ADE). The Cl2 evolution onset potential of the ADE was increased to 1.19 V from 1.05 V of the graphite felt, effectively inhibiting the chlorine evolution reaction(CER).The anode-generated Cl2 diffused into the gas absorption chamber through the ADE and was eventually consumed by the H2O2 adsorbent. Cu could be recovered without emitting chlorine due to the special structure of reactor. The current efficiency of copper precipitation and cathode reduction from Cu2+to Cu+reached 97.7%at a working current of 150 m A. These results indicated that the novel membrane reactor had high potential for application in the copper recovery industry.
文摘采用光学显微镜和扫描电子显微镜对不同腐蚀剂腐蚀后的Mg-Nd-Zn-Zr镁合金铸态显微组织进行观察。结果表明,Mg-NdZn-Zr合金的铸态组织主要由α-Mg和晶界处的Mg_(12)(Nd,Zn)两相组成,另外还有小块状Mg12(Nd,Zn)相及近圆形的富Zr相区域。1号传统腐蚀剂(4 m L硝酸+96 m L乙醇)可较好显示组织;经2号腐蚀剂(12 g苦味酸+80 m L乙酸+80 m L蒸馏水+350 m L乙醇)腐蚀5 s和10 s后,组织发黑,晶界不明显,但可部分显示出富Zr相区,延长腐蚀时间到20 s,晶粒显现出来,发黑现象得到缓解,富Zr区域明显,但晶界附近出现大量气泡;3号腐蚀剂(60 m L乙二醇+20 m L乙酸+19 m L蒸馏水+1 m L硝酸)腐蚀组织表明,其对晶粒的显示效果明显好于2号,然而很难观察到富Zr区域。
