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논문 기본 정보

자료유형
학위논문
저자정보

한슬기 (충남대학교, 忠南大學校 大學院)

지도교수
이종현
발행연도
2017
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충남대학교 논문은 저작권에 의해 보호받습니다.

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이 논문의 연구 히스토리 (2)

2017

핵연료 피복관 산세 폐액으로부터 침전 반응 및 불화물 용융염 전해제련을 통한 지르코늄 회수.
한슬기 2017.01 학위논문

2016

BaF<sub>2</sub> 침전 및 불화물 용융염 전해 제련을 통한 폐 산세액 내 지르코늄 회수
한슬기 ,  이영준 ,  최정훈 외 1명 한국재료학회지 2016.01 학술저널

초록· 키워드

오류제보하기
Zirconium(Zr) nuclear fuel cladding tube is made by three times pilgering and annealing process. In order to remove oxidized layer and impurity on the surface of the tube, the pickling process is required. Zirconium(Zr) is dissolved in HF and HNO3 mixed acid during the process and pickling acid including dissolved Zr is totally discarded after being neutralized. In the study, Na5Zr2F13 was precipitated by adding NaF at low temperature(-10℃) with stirring. In addtion, BaF2 was also added into waste acid and Ba2ZrF8 was recovered. It was investigated how dispersiveness, reaction time and particle size of BaF2 affect precipitation reaction, and they were compared in terms of residue concentration in the solution. As a result, when BaF₂was dispersed and the particle size was less than 1 μm, the residual Ba2+ and Zr4+ concentration in the solution decreased to 169 ppm and 11.47 ppm respectively. It is very difficult to extract the zirconium from the as recovered Ba2ZrF8 because the melting temperature is 1031˚C. Hence, we tried to recover Zr by electrowinning process using low temperature molten salt compound which was fabricated by adding ZrF4 into Ba2ZrF8 to decrease the melting point. Change of the Zr redox potential was observed by using cyclic voltammetry and the voltage change of the cell was observed by using polarization and chronopotentiometry. The structure of electro deposited Zr was analyzed and electro deposition characteristics were also evaluated. Zr ingot was fabricated by arc melting and the purity of Zr was measured to 99.99 wt. % by GDMS.

목차

목차 ·········································································Ⅰ
List of Figures ···························································Ⅲ
List of Table ······························································Ⅵ
1. 서론 ····································································1
2. 이론적 배경 ···························································4
2. 1. 지르코늄(Zirconium) ·········································4
2. 2. 침전 반응 ····················································5
2. 2. 1. 결정 핵 생성 ···········································5
2. 2. 2. 결정 핵 생성 시 에너지 변화 ··························7
2. 2. 2. 1. 균일 핵생성(Homogeneous nucleation) ··········7
2. 2. 2. 2. 불균일 핵생성(Heterogeneous nucleation) ·······11
2. 2. 3. 결정 핵 생성 속도 ·······································14
2. 2. 4. 결정 성장 ·················································16
2. 2. 5. 화학 평형 상수 ··········································19
2. 3. 전기 화학 반응················································21
2. 3. 1. 산화(Oxidation)와 환원(Reduction) 반응 ·············21
2. 3. 2. Butler-Volmer 식·········································24
2. 3. 3. 물질전달 지배방정식 ···································26
2. 3. 4. 순환전압전류법(Cyclic voltammetry, CV)·············29
2. 3. 5. 전기화학반응의 가역성 ·································32
2. 3. 6. 정전류법(Chronopotentionmetry, CP) ·················34
2. 3. 7. 패러데이 법칙(전기화학당량) ··························36
3. 재료 및 실험 방법 ·····················································38
3. 1. 재료 ····························································38
3. 2. NaF 침전 실험 ···············································38
3. 3. BaF2 침전 실험 ···············································40
3. 4. 지르코늄 전해 제련···········································42
3. 4. 1. 순환전압전류(Cyclic voltammetry, CV) 실험·········42
3. 4. 2. 정전류(Chronopotentionmetry, CP) 실험··············44
3. 5. 특성분석························································46
4. 결과 및 고찰 ···························································47
4. 1. NaF 침전 실험················································47
4. 1. 1. NaF 첨가량에 따른 침전 실험 ························47
4. 1. 2. NaF 첨가 후 교반 시간에 따른 침전 실험···········56
4. 1. 3. NaF 첨가 후 저온 시간에 따른 침전 실험···········59
4. 1. 4. NaF 첨가 후 저온 및 교반 시간에 따른 침전 실험·63
4. 2. BaF2 침전 실험················································66
4. 2. 1. BaF2 분산유무에 따른 침전 실험·······················66
4. 2. 2. BaF2 반응 시간에 따른 침전 실험·····················72
4. 2. 3. BaF2 입자 크기에 따른 침전 실험·····················77
4. 3. Zr 전해 제련 실험············································85
4. 3. 1. 순환전압전류(Cyclic voltammetry, CV) 실험·········85
4. 3. 2. 정전류(Chronopotentionmetry, CP) 실험··············88
4. 3. 3. 전해 제련을 통한 Zr 전착 및 전착물 특성 평가·····90
5. 결론 ·····································································97
Reference ··································································99
Abstract ··································································104

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