반도체 제조공정에서 발생하는 혼산폐액으로부터 고순도 인산 회수

Recovery of phosphoric acid from the waste acids in semiconductor manufacturing process

액정(LCD)과 반도체 제조공정에서 발생하는 인산, 질산, 초산, Al, Mo 등이 혼재하고 있는 인산계 혼산폐액을 액정제조공정에서 사용할 수 있는 고순도 에칭액으로 재활용하기 위해서 용매추출법, 진공 증발법, 확산투석법 및 이온교환법의 각각의 기술적 특성을 살린 혼합 처리공정을 이용하여 고순도 인산 회수 기술을 확립하고 상용화 시스템을 개발하고자 하였다. 시험 결과 진공증발에 의해 질산과 초산을 100% 제거할 수 있었고, TOP를 사용한 용매추출에서도 추출 4단, 탈거 6단, 상비 1/3으로 완벽하게 제거할 수 있었다. 이온교환의 전단계로 적용한 확산투석에서 Al 97%, Mo 75% 제거할 수 있었고 이온교환공정에서 Al 및 Mo를 각각 1ppm 이하로 정제할 수 있었다.

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 removal of impurities to tess than 1ppm 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, we have been clearly established that a mixed system of solvent extraction, diffusion dialysis and ion-exchange technique, which made individually the most of characteristics is developed to commercialize in an efficient system for recovering the high-purity phosphoric acid. By applying vacuum evaporation, the yield of the process are almost 99% removal of nitric acid and acetic acid was achieved. And by applying the 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 O/A=1/3 with four stages and the stripping of nitric acid from organic phase is attained at a ration of O/A=1 with six stages by distilled water. About 97% and 76% removal of Al and Mo were achieved by diffusion dialysis. Essentially complete less than 1ppm removal of Al, Mo by using ion exchange ion resin and purification of the phosphoric acid was obtain.