• Clean Technology
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• v.23 no.4
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• pp.393-400
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• 2017

In this study, we have developed a process for separating and recovering Ni and Fe in solution through a new solvent instead of TBP and Alamine336, which are solvents used in the conventional solvent extraction method. Experimental conditions were optimized through lab test and a $10L\;h^{-1}$ pilot plant was constructed for commercialization. In addition, the process data for mass production were obtained through pilot experiment and it was confirmed that there is no problem in product quality that can be used through the corrosion test of ferric chloride.

• Clean Technology
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• v.23 no.2
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• pp.158-162
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• 2017

$FeCl_3$ solution has been used as an etchant for metal etching such as Fe, Cu, Al and Ni. In the etching process, $Fe^{3+}$ is reduced to $Fe^{2+}$ and the etching efficiency is decreased. Waste $FeCl_3$ etchant has environmental, economic problems and thus the regeneration of the etching solution has been required. In this study, HCl was mixed with the $FeCl_2$ solution and then, $H_2O_2$, $NaClO_3$ were added into the mixed solution to oxidize the $Fe^{2+}$. During the oxidation process, oxidation-reduction potential (ORP) was measured and the relationship between ORP and oxidation ratio was investigated. The ORP is increased with increasing the concentration of $H_2O_2$ and $NaClO_3$, and then the ORP is decreased with oxidation progress. Such a behavior was in good agreement with Nernst's equation. Also, the oxidation efficiency was about 99% when a sufficient amount of HCl and $H_2O_2$, $NaClO_3$ were added.

• Clean Technology
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• v.14 no.2
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• pp.123-128
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• 2008

The waste solution, which was discharged from the recovery process of LCD etching solution, consists of 15 wt% nitric acid and 20 wt% acetic acid. In this study, it was conducted to separate acid individually from the mixed acid by vacuum evaporation under -760 mmHg gauge and at $40^{\circ}C$. We have investigated evaporation behavior of acid as a function of temperature. There have been problems that tiny amount of nitric acid were evaporated simultaneously above $33^{\circ}C$. Thus, efforts were conducted to recover acetic acid by vacuum evaporation with adding $H_2O$, waste mixed acid and 20 g/L NaOH for a curb on evaporation of nitric acid. By adding $H_2O$, evaporation of nitric acid was reduced from 7% to 0.78%. However, it was reduced from 7% to 0.25% by adding mixed acid. In view of the results achieved so far, we may expect to separate the etching solution individually by controlling vacuum conditions.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.22 no.6
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• pp.286-290
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• 2012

Boehmite (AlOOH) powder was synthesized using waste aluminium etching solution. In waste solution, precipitated phase was gibbsite ($Al(OH)_3$), and boehmite (AlOOH) phase was obtained at pH of 7 and 8 controlled by addition of acid. Boehmite powder was obtained by washing process to remove the Na ion in precipitated solution. Mean particle size of obtained powder was 40 nm. Boehmite phase transformed to ${\alpha}-Al_2O_3$ phase via ${\gamma}-Al_2O_3$, ${\delta}-Al_2O_3$, and ${\Theta}-Al_2O_3$.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.27 no.6
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• pp.303-308
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• 2017

The $FeCl_3$ waste solution used to etch various metals contains valuable metal such as nickel. In this study, we recovered as high purity nickel carbonate crystalline powders from nickel-containing etching waste solution after regeneration of iron chloride. Firstly we eliminated about of the iron impurities under the condition of pH 4 using 5 % NaOH aqueous solution and then removed the remaining impurities such as Ca, Mn and Zn etc. by using solvent extractant D2EHPA (Di-(2-ethylhexyl) phosphoric acid). Thereafter, nickel carbonate powder having a purity of 99.9 % or more was obtained through reaction with sodium carbonate in a nickel chloride solution.

• Proceedings of the Korean Institute of Resources Recycling Conference
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• 2004.05a
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• pp.218-226
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• 2004

Solvent extraction and stripping experiments were conducted to separate iron from a spent $FeCl_3$ etching solution containing nickel. In the extraction, PC88A, MIBK and Alamine336 were tested as an extractant in various diluents. Alamine336 salt in toluene led to the highest extraction percentage of iron. Stripping percentage of iron from the loaded organic by Alamine336 increased with decreasing HCl conentration of stripping solution and with increasing volume ratio of aqueous to organic. In the operation of bench scale mixer-settler, 7 extraction stage with 1.0M Alamine336 salt in toluene and 10 stripping stage with 0.01M HCl solution resulted in a stripped solution with 133g/L of iron and in a raffinate with most of nickel together with a small amount of iron when the flow rate ratio of organic to aqueous was 7.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2008.06a
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• pp.106-107
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• 2008

과거 PCB 제조 공정의 주된 관심사는 한정된 시간안에 다량의 제품을 생산하기 위한 것에 초점이 맞추어져 있었으나, 최근 중국의 전자산업 시장진출에 따른 PCB 가격 하락 및 원자제 가격 상승으로 인하여 생산 단가를 낮출 수 있는 방법으로 시선을 돌리고 있다. 특히, PCB 제조 공정에서, 생산 가격을 낮출 수 있는 방법중 가장 큰 비중을 차지하고 있는 것은, 습식 에칭 시 사용되는 용액(에칭액)의 사용 양을 제어함으로써, 화학 약품의 구입에 따른 비용 및 사용된 약품을 처리하는 비용을 줄일 수 있는 방법을 찾으려 노력하고 있다. 그러나, 애칭액을 효율적으로 제어하기 위해서는 여러 센서에서 나오는 데이터를 통합하여 진단할 수 있는 시스템이 필요하다. 그러나, 센서에 의한 데이터가 다양함에 제어 알고리듬이 복잡함에 따라 효율적인 제어 시스템이 개발되기 힘들다는 문제점이 있다. 본 논문에서는 이점에 착안하여, 인공지능 알고리듬을 이용한 애칭액 신액 투입조건을 실시간으로 제어 할 수 있는 시스템을 제안한다. 제안된 시스템을 사용하여, 애칭액을 균일하게 유지함에 따라 애칭액의 사용량을 줄일 수 있을 뿐 아니라, 폐액을 일정하게 관리할 수 있음을 확인하였다.

• Resources Recycling
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• v.26 no.2
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• pp.18-24
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• 2017

The $FeCl_3$ solution has been used as an etchant for etching of metal. It is necessary to reuse the etching solution because waste $FeCl_3$ etchant generated after use has provided environmental and economic problems. In this study, HCl was mixed with the $FeCl_2$ solution and then $H_2O_2$ was added into the mixed solution to oxidize the $Fe^{2+}$. During the oxidation process, oxidation-reduction potential (ORP) was measured and the relationship between ORP and oxidation ratio was investigated. As a result, this study found that the ORP was increased with increasing the concentration of HCl and $H_2O_2$, while the ORP is decreased with oxidation progress. Such a behavior was in good agreement with Nernst's equation. Also, the oxidation efficiency reached about 99% when a sufficient amount of HCl and $H_2O_2$ were added.

• Clean Technology
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• v.27 no.3
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• pp.240-246
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• 2021

The waste etching solution for chip on film (COF) contained about 3.5% copper, and it was recovered through cementation using iron samples. The effect of cementation with plate, chip, and powder iron samples was investigated. The molar ratio (m/r) of iron to copper was used as a variable in order to increase the recovery rate of copper. As the molar ratio increased, the copper content in the solution rapidly decreased at the beginning of the cementation reaction. Before and after the reaction, the copper content of the solution was determined by Inductively Coupled Plasma (ICP) using copper concentration according to time. After cementation at room temperature for 1 hour, the recovery rate of copper had increased the most in the iron powder sample, having the largest specific surface area of the samples, followed by the chip and plate samples. The recovered copper powder was characterized for its crystalline phase, morphology, and elemental composition by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Energy-dispersive X-ray spectroscopy (EDS), respectively. Copper and unreacted iron were present together in the iron powder samples. The optimum condition for recovering copper was obtained using iron chips with a molar ratio of iron to copper of 4 giving a recovery rate of about 98.4%.

• Resources Recycling
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• v.15 no.5 s.73
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• pp.26-32
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• 2006

The waste solution discharged from the LCD manufacturing process contains acids like nitric, acetic and phosphoric acid and metal ions such as Al, Mo and other impurities. It is important to remove impurities less than 1 ppm in phosphoric acid to reuse as an etchant because the residual impurities even in sub-ppm concentration in semiconductor materials play a major role on the electronic properties. In this study, a mixed system of solvent extraction, diffusion dialysis and ion-exchange was developed to commercialize in an efficient system fur recovering the high-purity phosphoric acid. By vacuum evaporation, almost 99% of nitric and acetic acid was removed. And by solvent extraction method with tri-octyl phosphate (TOP) as an extractant, the removal of acetic and nitric acid from the acid mixture was achieved effectively at the ratio A/O=1/3 with 4th stage of extraction stage. About 97.5% of Al and 36.7% of Mo were removed by diffusion dialysis. Essentially almost complete removal of metal ions and purification of high-purity phosphoric acid could be obtained by using ion exchange.