우리는 전기 화학적 실험 및 계측 (LSC와 j 번째)의 지원을 위해 화학 버지니아 군사 연구소 (VMI) 부서를 인정합니다. 학부의 학장의 VMI 사무실 조브 간행물과 관련된 생산 비용을 지원했다. 우리는 UNC EFRC 인정 : 태양 연료 센터, 화합물 합성 및 재료 특성의 지원을 위해 에너지, 과학의 사무실, 수상 번호 DE-SC0001011에서 기본 에너지 과학의 사무실, 미 교육부의 재정 지원 에너지 프론티어 연구 센터 (DPH ).

1.를 합성 한 에있어서 : - (도 4; 5,5&#39;- dvbpy가 비 피리딘 -2,2&#39;- 디 비닐 -5,5&#39;- 인 터 피리딘, 2 &#39;&#39; &#39;6&#39;은 PhTpy 4&#39;- 페닐 -2,2-이다)를 합성 한 절차 이전에 설명했다. (18) 2. 전해액 (1)의 1.3 mM의 모노머 용액을 조제 <ol><li> 아세토 니트릴, 테트라의 MeCN을 N 개의 -butylammonium 헥사 플루오로 포스페이트의 0.1 M 스톡 전해액 TBAPF 6을 준비한다. <ol><li> 3 분 자체, 또는 K 2 CO 3 활성화를 통해 외래 H 2 O를 제거하기 위해 24 시간 동안, MeCN을 배치 </li><li> 부피 플라스크를 건조 25.00 ml의 불꽃 TBAPF 6 (0.969 g, 2.50 밀리몰)을 놓습니다. </li><li> 3 미립자 건조를 MeCN에서 분 자체 또는 K 2 CO 필터 및 TBAPF을 포함하는 25.00 ml의 부피 플라스크를 가져 <su볼륨 B&gt; 6. </li></ol></li><li> 1 (0.0049 g, 5.2 × 10 -6 몰) 및 건조 4 DRAM 유리 병 또는 10 ml의 둥근 바닥 플라스크를 놓고 MeCN 중 0.1 M TBAPF 6의 원액 4.00를 가하여. </li><li> 매체의 다공성 유리 분말로 분리 각 구획으로 구획 3 셀의 중앙에 하나의 구획 등색 전해액 3.5-4.0 ml의 전송. </li><li> 신속 외측 구획에 누설을 방지하기에 MeCN 중 0.1 M 나머지 건조 TBAPF (6)의 일부와, 중앙 구획 원액으로 동일한 높이로 3 구획 셀의 외측 구획을 채운다. 주의 : 다른 구획 해법 천천히 혼합 용매 높이가 동일하지 않으면 현저히 주요 구획의 농도를 변경할 수 있기 때문에 시간이 중요한 요소이다. </li></ol> 3 mm 직경의 유리 3. Electropolymerize 1Y 전극 또는 탄소 1.0 cm 2 FTO 전극 <ol><li> 질소 / 아르곤 가스 제거 튜브 및 전극에 대한 격막을 준비합니다. <ol><li> 슬릿을 통해 얇은 폴리 테트라 플루오로 에틸렌, P​​TFE, 튜브 3 고무 격막의 각각에 슬릿을 잘라 안내합니다. </li><li> , 격막 중 하나를 통해 자세 / AGNO 3 기준 전극을 밀어 외부 구획 중 하나의 기준 전극 / PTFE 튜브 / 격막을 놓고 중격하는 부분을 밀봉. </li><li> 외측 구획 중 하나 다른 격벽 뒤져 백금선 / PTFE 튜브 / 격막 백금선 / 거즈 대극 가이드, 및 격막 밀봉 구획. 슬릿 와이어를 굽힘 방지하기에 충분히 뻣뻣 충분히 큰 또는 와이어가 아닌 경우, 격막 통해 백금 와이어 대향 전극을 안내하기 위해 넓은 보아 바늘을 사용한다. </li><li> 나머지 격벽을 통해 연마 갓 3mm 유리상 탄소 전극을 안내 및 그러한 전극이 배치되어 suspended FTO 슬라이드에 대한 솔루션이나,에, 격막을 통해 악어 클립에 연결된 와이어를 안내 한 후 악어 클립 FTO 슬라이드 클램프 및 침수시 슬라이드의 도전 측이 상대 전극에 수직 있는지 확인 . <ol><li> 유리 탄소 전극 삽입하기 전에 : 패드에 수직 전극을 누른 상태에서 유체가 접촉되는 연마 패드에 알루미나 (0.5 μm의)를 배치하여 폴란드어 유리 탄소를, 다음, 8 자형 움직임에 대한 30 초에 전극을 이동 - 폴란드어로 전극의 모든면 고르게 -과를 MeCN 물총 병 린스 H 2 O 물 물총 병에 남아있는 알루미나를 씻어 낸다. </li><li> FTO 슬라이드 클램핑하기에 앞서 : 상기 슬라이드의 10 × 10mm의 부분이 노출되도록 30 X 10mm의 FTO 슬라이드의 중앙부 주위에 비 도통 캡톤 여러 층의 랩. </li><li> 멋 부리다에서 FTO 슬라이드 / 배치 잡고 FTO 슬라이드의 UV-마주 스펙트럼을 수집일관성을 확보하기 위해 소정의 한 분광계의 빔 경로에 이온. </li></ol></li></ol></li><li> 3 구획 전기 화학 셀의 솔루션을 이용하므로 디 에어레이션. <ol><li> 질소 / 아르곤 공급에 타이곤 튜브의 한쪽 끝을 연결하고를 MeCN를 포함하는 가스 세탁기에 다른 쪽 끝을 연결합니다. </li><li> , 타이곤 튜브의 또 다른 조각을 잘라 MeCN을 질소 / 아르곤 세척 유출되는 한쪽 끝을 연결하고 4 방법 스플리터에 다른 쪽 끝을 연결합니다. </li><li> 4 방법 스플리터의 3 나머지 연결에 PTFE 튜브를 연결합니다. </li><li> 구획의 각 솔루션에 PTFE 튜브 잠수함 및 솔루션의 빠른 버블이 시작 질소 / 아르곤의 흐름을 켭니다. </li><li> 이어서, 막 용액의 표면 위에 PTFE 튜브를 당겨 시스템 및 용액을 방지하기 위해 불활성 기체의 양압을 유지하기 위해 / 아르곤에 질소의 흐름을 떠나, 5-10 분 동안 용액을 포기, 드 계속 Convection 버블 링에 의해 발생. </li></ol></li><li> 전기 화학적 실험을 수행합니다. <ol><li> 3 구획 셀의 적절한 전극 텐쇼에서 전극을 연결합니다. </li><li> 순환 전압 전류 법을 수행하여, CV, 다음 매개 변수를 사용하여 실험 : 전환 전위 = 0 V와 -1.81 V; 스캔 / 소인 속도 = 100 MV / 초; 사이클 = 5 수. </li><li> CV 실험이 완료되면, 중합 용액으로부터 작업 (유리상 탄소 또는 FTO)의 전극을 제거하고 부드럽게 피펫 또는 남아있는 단량체 용액을 제거 물총 병에서의 MeCN과 전극의 표면을 헹군다. </li></ol></li></ol> 4. 표면 범위 결정 <ol><li> 대향 전극과 기준 전극 (electropolymerizatio에서 사용 바람직 같은 기준 전극을 포함하는 전기 화학 전지에 0.1 M TBAPF 6 /의 MeCN 용액에 갓 준비한 세정 작업 전극을 배치N). </li><li> 순환 전압 전류 법을 수행하여, CV, 다음 매개 변수를 사용하여 실험 : 전환 전위 = 0, +1.5 V; 스캔 / 소인 속도 = 100 MV / 초; 횟수는 =​​ 15. </li><li> , 흡착 electropolymer의 Ru (III / II) 커플의 양극과 음극 봉우리 요금을 통합 양극과 음극 피크에서 요금을 평균하고, 식 (1) 표면의 범위를 결정하는 사​​용. </li><li> FTO 슬라이드의 경우 : 장소 / 빔 경로가 컬러 필름을 통과하도록 UV-마주 샘플 홀더의 전면에 소정의 위치에있는 FTO 슬라이드를 개최합니다. FTO 슬라이드 습식 또는 건식 수 있지만, 빈 스펙트럼 하에서 수집 하였다과 같은 조건으로 비교할 수있다. </li><li> 특정 슬라이드 수거 FTO 스펙트럼 얻은 스펙트럼 빼기 전에 막 자체에 대한 흡수 스펙트럼을 생성하기 위해, 필름상의 FTO의 스펙트럼으로부터 전기 중합한다. </li></ol>

<ol>
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C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polypyrrole+films+containing+metal+complexes:+syntheses+and+applications.">Polypyrrole films containing metal complexes: syntheses and applications.</a> Coordination Chemistry Reviews. 147, 339-371 (1996).</li><li>Sabouraud, G., Sadki, S., Brodie, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+mechanisms+of+pyrrole+electropolymerization.">The mechanisms of pyrrole electropolymerization.</a> Chemical Society Review. 29, 283-293 (2000).</li><li>Denisevich, P., Abru&#241;a, H. D., Leidner, C. R., Meyer, T. J., Murray, R. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electropolymerization+of+vinylpyridine+and+vinylbipyridine+complexes+of+iron+and+ruthenium:+homopolymers,+copolymers,+reactive+polymers.">Electropolymerization of vinylpyridine and vinylbipyridine complexes of iron and ruthenium: homopolymers, copolymers, reactive polymers.</a> Inorganic Chemistry. 21, 2153-2161 (1982).</li><li>Younathan, J. N., Wood, K. S., Meyer, T. 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J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Making+Oxygen+with+Ruthenium+Complexes.">Making Oxygen with Ruthenium Complexes.</a> Accounts of Chemical Research. 42, 1954-1965 (2009).</li><li>Chen, Z., Concepcion, J. J., Jurss, J. W., Meyer, T. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Single-Site,+Catalytic+Water+Oxidation+on+Oxide+Surfaces.">Single-Site, Catalytic Water Oxidation on Oxide Surfaces.</a> Journal of the American Chemical Society. 131, 15580-15581 (2009).</li><li>Lapides, A. M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Stabilization+of+a+Ruthenium(II)+Polypyridyl+Dye+on+Nanocrystalline+TiO2+by+an+Electropolymerized+Overlayer.">Stabilization of a Ruthenium(II) Polypyridyl Dye on Nanocrystalline TiO2 by an Electropolymerized Overlayer.</a> Journal of the American Chemical Society. 135, 15450-15458 (2013).</li><li>Paulson, S. C., Sapp, S. A., Elliott, C. 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Electroanal. Chem. Interfacial Electrochem. 115, 65-74 (1980).</li><li>Laviron, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=General+expression+of+the+linear+potential+sweep+voltammogram+in+the+case+of+diffusionless+electrochemical+systems.">General expression of the linear potential sweep voltammogram in the case of diffusionless electrochemical systems.</a> J. Electroanal. Chem. 101, 19-28 (1979).</li><li>Ratcliff, E. L., Jenkins, J. L., Nebesny, K., Armstrong, N. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrodeposited,+&#34;Textured&#34;+Poly(3-hexyl-thiophene)+(e-P3HT)+Films+for+Photovoltaic+Applications.">Electrodeposited, &#34;Textured&#34; Poly(3-hexyl-thiophene) (e-P3HT) Films for Photovoltaic Applications.</a> Chemistry of Materials. 20, 5796-5806 (2008).</li></ol>

No conflicts of interest declared.

전기 중합은 다른 기술에 공통없는 제어 변수의 큰 범위를 제공합니다. 등 시약 (단량체) 농도, 온도, 용매, 반응 같은 표준 변수 이외에, 전기 중합 추가적으로 전기 화학적 방법에 공통 전기 화학적 실험 매개 변수에 의해 제어 될 수있다. CV 스캔 속도, 스위칭 잠재력 및 횟수는 electropolymers의 증착에 영향을 미칩니다. 예를 들면, 리간드의 환원 전파를 통해 사이클의 수가 증가함에 따라, 또...

전기 중합 직접 전극 표면에서 단량체 성 전구 물질의 중합을 개시하기 위해인가 된 전위를 이용하고 Electrocatalysis 화학적 얇은 전기 및 / 또는 전극과 반도체 표면에 활성 폴리 피리 필름. 1-4을 생성 시키는데 이용 된 중합 기법 전자 전달 5-10, 11, 12 광화학, 통전 변색 성 13-16, 17 및 18은 배위 화학 electropolymerized 필름에서 조사되었다. 이 기술이 처음 비닐 3, 5, 7, 8, 11 ~ 15, 19, 20 및 피롤 6, 9의 전기 중합을위한 마이어 - 머레이 협력 노스 캐롤라이나 대학에서 개발 된, 21 ~ 24 절 유도기판을 행하는 각종 착체에 탈. 1 금속 착체에 배위하면, electropolymers를 생산 공통 딜 리간드 계의 번호를 표시도. 피롤 관능 리간드, 전기 중합은 (그림 2) 산화 적 전기 중합 결과, 피롤 잔기의 산화에 의해 개시되는 동안 환원 전기 중합에서 비닐 함유 화합물의 전기 중합은 비닐 기 접합 딜 리간드의 감소에 따라 발생한다. 전기 중합 기술은 직접 전극에 거의 모든 전이 금속 착물을 부착하기위한 일반화 된 방법을 제공하기위한 목적으로 개발되었다. 이 방법의 다양성은 electropolymer 수정 전극의 수많은 조사에 문을 엽니 다. 전극에 직접 접합을 포함하는 다른 접속 전략, 대조적으로, 전기 중합은 ADV을 구비전극면 수정 전 없어도 사용할 ANTAGE. . 따라서 상관없이 표면 형태 또는 조성물 (4), 10, 25, 전도성 기판의 임의의 수에 적용 할 수있는, 범용성이 26 중합체 길이가 성장함에 따라 물성 변화의 결과이고; 모노머는 전해액에 가용성이지만, 중합이 발생하고, 가교는 전극 표면이 발생 필름, 침전 및 물리적 흡착 (도 3) rigidifies. 27 일반적으로 태양 전지 연료 연구에 사용되는 고가의 pH의,에 불안정한 산화물 물 표면, 또는 포스 포 네이트 유도체 화 착체에 불안정한 산화물 표면 - 결합 된 카르 복실 레이트에 비해, 이들 계면 전극 중합체 필름 구조는 안정성의 이점도 제공 넓은 pH 범위 (0-14)을 통해 유기 용매 및 물을 포함하여 다양한 미디어.28-30 전기 중합은 서브 단층에서 카르 복실 레이트 또는 포스 - 유도 단지 인터페이스 구조가 단층 표면 적용 범위가 제한되는 반면 수십 또는 동등 단일 층의 수백에 명백한 표면 커버리지의 큰 범위와 필름을 증착 할 수 있습니다. 비닐 피롤 함유 딜과 폴리 피리 임의의 여러 화합물이 중합 할 수 있지만, [Ru로 II (PhTpy)는 (5,5&#39;- dvbpy ()을 MeCN) (PF 6) 2 (1; PhTpy 4&#39;- 페닐이며 -2,2- &#39;6&#39;, 2 &#39;&#39;- 터 피리딘, 5,5&#39;- dvbpy는 디 비닐 -2,2&#39;- 5,5&#39;- 비 피리딘; 그림 4) 환원 전기 중합을 입증하는 모델 단지로 활용 될 것입니다 유리상 탄소와 불소 도핑 된 산화 주석에서, FTO,이 보고서의 전극. 1 인해 금속 - 대 Li, 전위에 전기 응용 례를 가지고 현대 electropolymer 전구체의 예이고GAND 충전 전송, MLCT은 빛 스펙트럼의 가시 영역에 누워 흡수 스펙트럼은, UV-마주 광. 18, 30 일에 대한 여기에 제시된 어떤 결과가 이미 약간 수정 된 형태로 발표되었다주의하시기 바랍니다. (18)을 조사 할 수있다

<table border="0" cellpadding="0" cellspacing="0" width="652">
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			<td height="21" style="height:21px;width:384px;">Name of Reagent/ Equipment</td>
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			<td height="20" style="height:20px;">Tetrabutylammonium hexafluorophosphate for electrochemical analysis, &#8805;99.0%,&#160;</td>
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			<td height="20" style="height:20px;width:384px;">Acetonitrile&#160;(Optima LC/MS), Fisher Chemical</td>
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			<td height="20" style="height:20px;">3 mm dia. Glassy Carbon Working Electrode</td>
			<td>CH Instruments</td>
			<td>CH104</td>
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			<td height="20" style="height:20px;">Non-Aqueous Ag/Ag+ Reference Electrode w/ porous Teflon Tip</td>
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			<td colspan="2">Custom made H-cell with 3 compartments</td>
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reductive electropolymerization of a vinyl-containing poly-pyridyl complex on glassy carbon and fluorine-doped tin oxide electrodes

제어 전극 표면 개질이 필드, 태양 연료 애플리케이션 특히 사람들의 수가 중요하다. 전기 중합은 헬름홀츠 층 기판의 중합을 개시하기 위해인가 된 전위를 이용하여, 전극의 표면에 폴리머 필름을 electrodeposits 한 표면 개질 기술이다. 이 유용한 기술은 먼저 1980 년대 초 채플 힐 노스 캐롤라이나 대학의 머레이 - 마이어의 협력에 의해 설립 단량체 기판 등의 무기 복합체를 포함하는 필름의 다양한 물리적 현상을 연구하기 위해 사용 하였다. 여기서는 유리상 탄소와 불소 도핑 된 산화 주석 코팅 된 전극 상에 함유 된 폴리 비닐 피리 딜 착체의 환원 전기 중합을 수행함으로써 무기 복합체로 피복 전극 용 절차를 강조. 전기 화학 전지의 구성 및 문제 해결 절차에 대한 권장 사항이 포함되어 있습니다. 하지 전자 있지만xplicitly 여기에 설명, 피롤 함유 화합물의 산화 전기 중합은 비닐 계 환원 전기 중합 유사한 절차를 따르지만 훨씬 덜 민감한 산소와 물이다.

규정 CV 실험 (프로토콜 텍스트 STEP 3.3.2)의 진행을 관찰 할 때 Electropolymer 성장은 가장 쉽게 인식된다. (5) 0.071 cm 2 (3 mm 직경)에 electropolymer 성장 1 유리 탄소 전극을 예시 그림. 실험의 첫 번째 사이클은 전압 전류가 대략 1 차 및 2 차 리간드를 중심으로 감소 전파를 통해 연속적인 사이클에 따라 유사한 농도 (그림 5, 블랙 추...

Watch this Scientific Journal Video about Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes at JoVE.com

Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization.

유리 탄소와 불소 도핑 된 주석 산화물 전극에 비닐 함유 폴리 피리 딜 단지의 환원 적 전기 중합

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is ...

reductive-electropolymerization-vinyl-containing-poly-pyridyl-complex

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JoVE Journal

Chemistry

11.7K 조회수.  Virginia Military Institute. A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization. 

비디오: Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

Improved In-gel Reductive &#946;-Elimination for Comprehensive O-linked and Sulfo-glycomics by Mass Spectrometry

Separation of proteins by SDS-PAGE followed by in-gel proteolytic digestion of resolved protein bands has produced high-resolution proteomic analysis of biological samples. Similar approaches, that would allow in-depth analysis of the glycans carried by glycoproteins resolved by SDS-PAGE, require special considerations in order to maximize recovery and sensitivity when using mass spectrometry (MS) as the detection method. A major hurdle to be overcome in achieving high-quality data is the removal of gel-derived contaminants that interfere with MS analysis. The sample workflow presented here is robust, efficient, and eliminates the need for in-line HPLC clean-up prior to MS. Gel pieces containing target proteins are washed in acetonitrile, water, and ethyl acetate to remove contaminants, including polymeric acrylamide fragments. O-linked glycans are released from target proteins by in-gel reductive &#946;-elimination and recovered through robust, simple clean-up procedures. An advantage of this workflow is that it improves sensitivity for detecting and characterizing sulfated glycans. These procedures produce an efficient separation of sulfated permethylated glycans from non-sulfated (sialylated and neutral) permethylated glycans by a rapid phase-partition prior to MS analysis, and thereby enhance glycomic and sulfoglycomic analyses of glycoproteins resolved by SDS-PAGE.

Improved In-gel Reductive &amp;#946;-Elimination for Comprehensive O-linked and Sulfo-glycomics by Mass Spectrometry

In order to comprehensively explore the diversity of O-linked glycans, a new procedure for in-gel reductive &#946;-elimination, combined with permethylation and a rapid phase-partition method, is applied to the analysis of O-linked glycans directly released from glycoproteins resolved by SDS-PAGE and amenable to subsequent glycomic analysis by mass spectrometry.

질량 분석에 의해 - 겔 개선 환원 적 β-제거 포괄적 인 O가 연결된과에 대한 설포 글라 이코믹스

Separation of proteins by SDS-PAGE followed by in-gel proteolytic digestion of resolved protein bands has produced high-resolution proteomic analysis of ...

연구

화학

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

복합 산화물 박막의 에피 택셜 성장을위한 원자 적으로 정의 된 템플릿

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

Transport of Surface-modified Carbon Nanotubes through a Soil Column

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, electronics and biomedical applications. Due to their accelerating production and use, CNTs constitute a potential environmental risk if they are released to soil and groundwater systems. It is therefore essential to improve the current understanding of environmental fate and transport of CNTs. The transport and retention of CNTs in both natural and artificial media have been reported in literature, but the findings widely vary and are thus not conclusive. There are a number of physical and chemical parameters responsible for variation in retention and transport. In this study, a complete procedure of selected multiwalled carbon nanotubes (MWCNTs) is presented starting from their surface modification to a complete set of laboratory column experiments at critical physical and chemical scenarios. Results indicate that the stability of the commercially available MWCNTs are critical with their attached surface functional group which can also influence the transport and retention of MWCNT through the surrounding medium.

Surface properties of a nanoparticle are important for their interaction with the surrounding medium. Therefore the surface modification of carbon nanotubes can be critical for their transport and retention through porous media. Here, lab scale column experiments are used to understand the possible transport and retention of these nanoparticles.

토양 칼럼을 통해 표면 개질 된 카본 나노 튜브의 운송

Carbon nanotubes (CNTs) are widely manufactured nanoparticles, which are being utilized in a number of consumer products, such as sporting goods, ...

Photochemical Oxidative Growth of Iridium Oxide Nanoparticles on CdSe@CdS Nanorods

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide (CdSe@CdS) nanorod photocatalysts. Seeded rods are grown using a colloidal hot-injection method and then moved to an aqueous medium by ligand exchange. CdSe@CdS nanorods, an iridium precursor and other salts are mixed and illuminated. The deposition process is initiated by absorption of photons by the semiconductor particle, which results with formation of charge carriers that are used to promote redox reactions. To insure photochemical oxidative growth we used an electron scavenger. The photogenerated holes oxidize the iridium precursor, apparently in a mediated oxidative pathway. This results in the growth of high quality crystalline iridium oxide particles, ranging from 0.5 nm to about 3 nm, along the surface of the rod. Iridium oxide grown on CdSe@CdS heterostructures was studied by a variety of characterization methods, in order to evaluate its characteristics and quality. We explored means for control over particle size, crystallinity, deposition location on the CdS rod, and composition. Illumination time and excitation wavelength were found to be key parameters for such control. The influence of different growth conditions and the characterization of these heterostructures are described alongside a detailed description of their synthesis. Of significance is the fact that the addition of iridium oxide afforded the rods astounding photochemical stability under prolonged illumination in pure water (alleviating the requirement for hole scavengers).

A protocol for the photochemical oxidative growth of small crystalline iridium oxide nanoparticles on the surface of CdSe@CdS seeded rod nanoparticles is presented.

의 CdSe @ CdS와 나노 막대에 이리듐 산화물 나노 입자의 광 화학적 산화 성장

We demonstrate a procedure for the photochemical oxidative growth of iridium oxide catalysts on the surface of seeded cadmium selenide-cadmium sulfide ...

On-line Analysis of Nitrogen Containing Compounds in Complex Hydrocarbon Matrixes

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The composition of heavy crude oils and shale oils varies substantially depending on the origin of the mixture. In particular they contain an increased amount of nitrogen containing compounds compared to the conventionally used sweet crude oils. As nitrogen compounds have an influence on the operation of thermal processes occurring in coker units and steam crackers, and as some species are considered as environmentally hazardous, a detailed analysis of the reactions involving nitrogen containing compounds under pyrolysis conditions provides valuable information. Therefore a novel method has been developed and validated with a feedstock containing a high nitrogen content, i.e., a shale oil. First, the feed was characterized offline by comprehensive two-dimensional gas chromatography (GC &#215; GC) coupled with a nitrogen chemiluminescence detector (NCD). In a second step the on-line analysis method was developed and tested on a steam cracking pilot plant by feeding pyridine dissolved in heptane. The former being a representative compound for one of the most abundant classes of compounds present in shale oil. The composition of the reactor effluent was determined via an in-house developed automated sampling system followed by immediate injection of the sample on a GC &#215; GC coupled with a time-of-flight mass spectrometer (TOF-MS), flame ionization detector (FID) and NCD. A novel method for quantitative analysis of nitrogen containing compounds using NCD and 2-chloropyridine as an internal standard has been developed and demonstrated.

A method combining comprehensive two-dimensional gas chromatography with nitrogen chemiluminescence detection has been developed and applied to on-line analysis of nitrogen containing compounds in a complex hydrocarbon matrix.

복잡한 탄화수소 행렬에 질소 함유 화합물의 온라인 분석

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The ...

Investigations on the Ga(III) Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

We demonstrate a method for the isolation of EOB-DTPA (3,6,9-triaza-3,6,9-tris(carboxymethyl)-4-(ethoxybenzyl)-undecanedioic acid) from its Gd(III) complex and protocols for the preparation of its novel non-radioactive, i.e., natural Ga(III) as well as radioactive 68Ga complex. The ligand as well as the Ga(III) complex were characterized by nuclear magnetic resonance (NMR) spectroscopy, mass spectrometry and elemental analysis. 68Ga was obtained by a standard elution method from a 68Ge/68Ga generator. Experiments to evaluate the 68Ga-labeling efficiency of EOB-DTPA at pH 3.8&#8211;4.0 were performed. Established analysis techniques radio TLC (thin layer chromatography) and radio HPLC (high performance liquid chromatography) were used to determine the radiochemical purity of the tracer. As a first investigation of the 68Ga tracers&#39; lipophilicity the n-octanol/water distribution coefficient of 68Ga species present in a pH 7.4 solution was determined by an extraction method. In vitro stability measurements of the tracer in various media at physiological pH were performed, revealing different rates of decomposition.

Investigations on the GaIII Complex of EOB-DTPA and Its 68Ga Radiolabeled Analogue

A procedure for the isolation of EOB-DTPA and subsequent complexation with natural Ga(III) and 68Ga is presented herein, as well as a thorough analysis of all compounds and investigations on labeling efficiency, in vitro stability and the n-octanol/water distribution coefficient of the radiolabeled complex.

EOB-DTPA와의 조지아 (III) 단지에 대한 조사 그것<sup&gt; (68)</sup&gt; 조지아 방사성 표지 된 아날로그

We demonstrate a method for the isolation of EOB-DTPA (3,6,9-triaza-3,6,9-tris(carboxymethyl)-4-(ethoxybenzyl)-undecanedioic acid) from its Gd(III) ...

Grafting Multiwalled Carbon Nanotubes with Polystyrene to Enable Self-Assembly and Anisotropic Patchiness

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a free-radical polymerization strategy to enable the modulation of the nanotube surface properties and produce supramolecular self-assembly of the nanostructures. First, a selective hydroxylation of the pristine nanotubes through a biphasic catalytically mediated oxidation reaction creates superficially distributed reactive sites at the sidewalls. The latter reactive sites are subsequently modified with methacrylic moieties using a silylated methacrylic precursor to create polymerizable sites. Those polymerizable groups can address further polymerization of styrene to produce a hybrid nanomaterial containing PS chains grafted to the nanotube sidewalls. The polymer-graft content, amount of silylated methacrylic moieties introduced and hydroxylation modification of the nanotubes are identified and quantified by Thermogravimetric Analysis (TGA). The presence of reactive functional groups hydroxyl and silylated methacrylate are confirmed by Fourier Transform Infrared Spectroscopy (FT-IR). Polystyrene-grafted carbon nanotube solutions in tetrahydrofuran (THF) provide wall-to-wall collinearly self-assembled nanotubes when cast samples are analyzed by transmission electron microscopy (TEM). Those self-assemblies are not obtained when suitable blanks are similarly cast from analogous solutions containing non-grafted counterparts. Therefore, this method enables the modification of the nanotube anisotropic patchiness at the sidewalls which results into spontaneous auto-organization at the nanoscale.

A procedure for the synthesis of polystyrene-grafted multiwalled carbon nanotubes using successive chemical modification steps to selectively introduce the polymer chains to the sidewalls and their self-assembly via anisotropic patchiness is presented.

자기 집합에 있도록 폴리스 티 렌과 이방성 Patchiness Multiwalled 탄소 나노튜브를 접목

We demonstrate a straightforward protocol to graft pristine multiwalled carbon nanotubes (MWCNTs) with polystyrene (PS) chains at the sidewalls through a ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

전기 화학 임피던스 분 광 전기 화학 속도 상수 추정을 위한 도구로

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven effective in gas adsorption, separations, and catalysis. MOFs are most commonly synthesized as bulk powder, requiring additional processes to adhere them to functional devices and fabrics that risk decreasing the powder porosity and adsorption capacity. Here, we demonstrate a method of first coating fabrics with metal oxide films using atomic layer deposition (ALD). This process creates conformal films of controllable thickness on each fiber, while providing a more reactive surface for MOF nucleation. By submerging the ALD coated fabric in solution during solvothermal MOF synthesis, the MOFs create a conformal, well-adhered coating on the fibers, resulting in a MOF-functionalized fabric, without additional adhesion materials that may block MOF pores and functional sites. Here we demonstrate two solvothermal synthesis methods. First, we form a MIL-96(Al) layer on polypropylene fibers using synthetic conditions that convert the metal oxide to MOF. Using initial inorganic films of varying thicknesses, diffusion of the organic linker into the inorganic allows us to control the extent of MOF loading on the fabric. Second, we perform a solvothermal synthesis of UiO-66-NH2 in which the MOF nucleates on the conformal metal oxide coating on polyamide-6 (PA-6) fibers, thereby producing a uniform and conformal thin film of MOF on the fabric. The resulting materials can be directly incorporated into filter devices or protective clothing and eliminate the maladroit qualities of loose powder.

Solvothermal Synthesis of MIL-96 and UiO-66-NH2 on Atomic Layer Deposited Metal Oxide Coatings on Fiber Mats

Metal-organic frameworks are effective in gas storage and heterogeneous catalysis, but typical synthesis methods result in loose powders that are difficult to incorporate into smart materials. We demonstrate a method of first coating fabrics with ALD metal oxides, resulting in conformal films of MOF on the fabrics during solvothermal synthesis.

밀-96와 UiO-66-NH2 원자 층 Solvothermal 합성 섬유 매트에 금속 산화물 코팅을 입금

Metal-organic frameworks (MOFs), which contain reactive metal clusters and organic ligands allowing for large porosities and surface areas, have proven ...

Negative Additive Manufacturing of Complex Shaped Boron Carbides

Boron carbide (B4C) is one of the hardest materials in existence. However, this attractive property also limits its machineability into complex shapes for high wear, high hardness, and lightweight material applications such as armors. To overcome this challenge, negative additive manufacturing (AM) is employed to produce complex geometries of boron carbides at various length scales. Negative AM first involves gelcasting a suspension into a 3D-printed plastic mold. The mold is then dissolved away, leaving behind a green body as a negative copy. Resorcinol-formaldehyde (RF) is used as a novel gelling agent because unlike traditional hydrogels, there is little to no shrinkage, which allows for extremely complex molds to be used. Furthermore, this gelling agent can be pyrolyzed to leave behind ~50 wt% carbon, which is a highly effective sintering aid for B4C. Due to this highly homogenous distribution of in situ carbon within the B4C matrix, less than 2% porosity can be achieved after sintering. This protocol highlights in detail the methodology for creating near fully dense boron carbide parts with highly complex geometries.

A method called negative additive manufacturing is used to produce near fully dense complex shaped boron carbide parts of various length scales. This technique is possible via the formulation of a novel suspension involving resorcinol-formaldehyde as a unique gelling agent that leaves behind a homogenous carbon sintering aid after pyrolysis.

복잡 한 모양의 붕 소 합금의 첨가제 제조 제외

Boron carbide (B4C) is one of the hardest materials in existence. However, this attractive property also limits its machineability into complex shapes for ...