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. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrocatalytic+reduction+of+nitrite+and+nitrosyl+by+iron(III)+protoporphyrin+IX+dimethyl+ester+immobilized+in+an+electropolymerized+film.">Electrocatalytic reduction of nitrite and nitrosyl by iron(III) protoporphyrin IX dimethyl ester immobilized in an electropolymerized film.</a> Inorganic Chemistry. 31, 3280-3285 (1992).</li><li>Ikeda, T., Schmehl, R., Denisevich, P., Willman, K., 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=Permeation+of+electroactive+solutes+through+ultrathin+polymeric+films+on+electrode+surfaces.">Permeation of electroactive solutes through ultrathin polymeric films on electrode surfaces.</a> Journal of the American Chemical Society. 104, 2683-2691 (1982).</li><li>Concepcion, J. 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><tbody><tr><td>Tetrabutylammonium hexafluorophosphate for electrochemical analysis, &amp;ge;99.0%</td><td>Sigma-Aldrich</td><td>86879-25G</td><td></td></tr><tr><td>Acetonitrile&amp;nbsp;(Optima LC/MS), Fisher Chemical</td><td>Fisher Scientific</td><td>A955-4</td><td></td></tr><tr><td>3 mm dia. Glassy Carbon Working Electrode</td><td>CH Instruments</td><td>CH104</td><td></td></tr><tr><td>Non-Aqueous Ag/Ag&lt;sup&gt;+&lt;/sup&gt; Reference Electrode w/ porous Teflon Tip</td><td>CH Instruments</td><td>CHI112</td><td></td></tr><tr><td>Platinum&amp;nbsp;gauze</td><td>Alfa Aesar</td><td>AA10282FF&amp;nbsp;</td><td></td></tr><tr><td>Electrode Polishing Kit</td><td>CH Instruments</td><td>CHI120</td><td></td></tr><tr><td>Cole-Parmer KAPTON TAPE 1/2&amp;nbsp;IN x 36&amp;nbsp;YD</td><td>Fisher Scientific</td><td>NC0099200</td><td></td></tr><tr><td>Fisherbrand Polypropylene Tubing 4-Way Connectors</td><td>Fisher Scientific</td><td>15-315-32B</td><td></td></tr><tr><td>500 ml Bottle, Gas Washing, Tall Form, Coarse Frit</td><td>Chemglass</td><td>CG-1114-15</td><td></td></tr><tr><td>3-compartment H-Cell for electrochemistry</td><td>Custom made H-cell with 3 compartments</td><td></td><td></td></tr></tbody></table>

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

Research

JoVE Journal

Chemistry

11.8K 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

Atom Transfer Radical Polymerization of Functionalized Vinyl Monomers Using Perylene as a Visible Light Photocatalyst

A standardized technique for atom transfer radical polymerization of vinyl monomers using perylene as a visible-light photocatalyst is presented. The procedure is performed under an inert atmosphere using air- and water-exclusion techniques. The outcome of the polymerization is affected by the ratios of monomer, initiator, and catalyst used as well as the reaction concentration, solvent, and nature of the light source. Temporal control over the polymerization can be exercised by turning the visible light source off and on. Low dispersities of the resultant polymers as well as the ability to chain-extend to form block copolymers suggest control over the polymerization, while chain end-group analysis provides evidence supporting an atom-transfer radical polymerization mechanism.

A method for the atom transfer radical polymerization of functionalized vinyl monomers using perylene as a visible-light photocatalyst is described.

가시광 광촉매 페 릴렌 사용 관능 비닐 모노머의 원자 이동 라디칼 중합

A standardized technique for atom transfer radical polymerization of vinyl monomers using perylene as a visible-light photocatalyst is presented. The ...

연구

화학

Electroactive Polymer Nanoparticles Exhibiting Photothermal Properties

A method for the synthesis of electroactive polymers is demonstrated, starting with the synthesis of extended conjugation monomers using a three-step process that finishes with Negishi coupling. Negishi coupling is a cross-coupling process in which a chemical precursor is first lithiated, followed by transmetallation with ZnCl2. The resultant organozinc compound can be coupled to a dibrominated aromatic precursor to give the conjugated monomer. Polymer films can be prepared via electropolymerization of the monomer and characterized using cyclic voltammetry and ultraviolet-visible-near infrared (UV-Vis-NIR) spectroscopy. Nanoparticles (NPs) are prepared via emulsion polymerization of the monomer using a two-surfactant system to yield an aqueous dispersion of the polymer NPs. The NPs are characterized using dynamic light scattering, electron microscopy, and UV-Vis-NIR-spectroscopy. Cytocompatibility of NPs is investigated using the cell viability assay. Finally, the NP suspensions are irradiated with a NIR laser to determine their effectiveness as potential materials for photothermal therapy (PTT).

A protocol is presented for the synthesis and preparation of nanoparticles consisting of electroactive polymers.

전기 활성 고분자 나노 입자 출전 광열 등록

A method for the synthesis of electroactive polymers is demonstrated, starting with the synthesis of extended conjugation monomers using a three-step ...

공학

A Simple and Efficient Protocol for the Catalytic Insertion Polymerization of Functional Norbornenes

Norbornene can be polymerized by a variety of mechanisms, including insertion polymerization whereby the double bond is polymerized and the bicyclic nature of the monomer is conserved. The resulting polymer, polynorbornene, has a very high glass transition temperature, Tg, and interesting optical and electrical properties. However, the polymerization of functional norbornenes by this mechanism is complicated by the fact that the endo substituted norbornene monomer has, in general, a very low reactivity. Furthermore, the separation of the endo substituted monomer from the exo monomer is a tedious task. Here, we present a simple protocol for the polymerization of substituted norbornenes (endo:exo ca. 80:20) bearing either a carboxylic acid or a pendant double bond. The process does not require that both isomers be separated, and proceeds with low catalyst loadings (0.01 to 0.02 mol%). The polymer bearing pendant double bonds can be further transformed in high yield, to afford a polymer bearing pendant epoxy groups. These simple procedures can be applied to prepare polynorbornenes with a variety of functional groups, such as esters, alcohols, imides, double bonds, carboxylic acids, bromo-alkyls, aldehydes and anhydrides.

We describe the catalytic insertion polymerization of 5-norbornene-2-carboxylic acid and 5-vinyl-2-norbornene to form functional polymers with a very high glass transition temperature.

기능 노보 넨의 촉매 삽입 중합을위한 간단하고 효율적인 프로토콜

Norbornene can be polymerized by a variety of mechanisms, including insertion polymerization whereby the double bond is polymerized and the bicyclic ...

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). ...

Raman and IR Spectroelectrochemical Methods as Tools to Analyze Conjugated Organic Compounds

In the presented work, two spectroelectrochemical techniques are discussed as tools for the analysis of the structural changes occurring in the molecule on the vibrational level of energy. Raman and IR spectroelectrochemistry can be used for advanced characterization of the structural changes in the organic electroactive compounds. Here, the step-by-step analysis by means of Raman and IR spectroelectrochemistry is shown. Raman and IR spectroelectrochemical techniques provide complementary information about structural changes occurring during an electrochemical process, i.e. allows for the investigation of redox processes and their products. The examples of IR and Raman spectroelectrochemical analysis are presented, in which the products of the redox reactions, both in solution and solid state, are identified.

A protocol of step-by-step Raman and IR spectroelectrochemical analysis is presented.

In the presented work, two spectroelectrochemical techniques are discussed as tools for the analysis of the structural changes occurring in the molecule ...

Using Cyclic Voltammetry, UV-Vis-NIR, and EPR Spectroelectrochemistry to Analyze Organic Compounds

Cyclic voltammetry (CV) is a technique used in the analysis of organic compounds. When this technique is combined with electron paramagnetic resonance (EPR) or ultraviolet-visible and near-infrared (UV-Vis-NIR) spectroscopies, we obtain useful information such as electron affinity, ionization potential, band-gap energies, the type of charge carriers, and degradation information that can be used to synthesize stable organic electronic devices. In this study, we present electrochemical and spectroelectrochemical methods to analyze the processes occurring in active layers of an organic device as well as the generated charge carriers.

In this article, we describe electrochemical, electron paramagnetic resonance, and ultraviolet-visible and near-infrared spectroelectrochemical methods to analyze organic compounds for application in organic electronics.

사용 하 여 순환 Voltammetry, UV-Vi-NIR, EPR Spectroelectrochemistry 유기 화합물 분석

Cyclic voltammetry (CV) is a technique used in the analysis of organic compounds. When this technique is combined with electron paramagnetic resonance ...

Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. Conductive polymers, poly(3,4-ethylenedioxythiophene) (PEDOT) and poly(3,4-propylenedioxythiophene) (PProDOT), and a semiconducting polymer, poly(thieno[3,2-b]thiophene) (PTT), were deposited on unconventional highly-disordered and textured substrates with high surface areas, such as paper, towels and fabrics. This reported deposition chamber is an improvement of previous vapor reactors because our system can accommodate both volatile and nonvolatile monomers, such as 3,4-propylenedioxythiophene and thieno[3,2-b]thiophene. Utilization of both solid and liquid oxidants are also demonstrated. One limitation of this method is that it lacks sophisticated in situ thickness monitors. Polymer coatings made by the commonly used solution-based coating methods, such as spin-coating and surface grafting, are often not uniform or susceptible to mechanical degradation. This reported vapor phase deposition method overcomes those drawbacks and is a strong alternative to common solution-based coating methods. Notably, polymer films coated by the reported method are uniform and conformal on rough surfaces, even at a micrometer scale. This feature allows for future application of vapor deposited polymers in electronics devices on flexible and highly textured substrates.

This paper presents a protocol for reactive vapor deposition of poly(3,4-ethylenedioxythiophene), poly(3,4-propylenedioxythiophene), and poly(thieno[3,2-b]thiophene) films on glass slides and rough substrates, such as textiles and paper.

임의 기판에 활용 된 고분자 필름의 반응성 증 착

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. ...

Fabricating Degradable Thermoresponsive Hydrogels on Multiple Length Scales via Reactive Extrusion, Microfluidics, Self-assembly, and Electrospinning

While various smart materials have been explored for a variety of biomedical applications (e.g., drug delivery, tissue engineering, bioimaging, etc.), their ultimate clinical use has been hampered by the lack of biologically-relevant degradation observed for most smart materials. This is particularly true for temperature-responsive hydrogels, which are almost uniformly based on polymers that are functionally non-degradable (e.g., poly(N-isopropylacrylamide) (PNIPAM) or poly(oligoethylene glycol methacrylate) (POEGMA)). As such, to effectively translate the potential of thermoresponsive hydrogels to the challenges of remote-controlled or metabolism-regulated drug delivery, cell scaffolds with tunable cell-material interactions, theranostic materials with the potential for both imaging and drug delivery, and other such applications, a method is required to render the hydrogels (if not fully degradable) at least capable of renal clearance following the required lifetime of the material. To that end, this protocol describes the preparation of hydrolytically-degradable hydrazone-crosslinked hydrogels on multiple length scales based on the reaction between hydrazide and aldehyde-functionalized PNIPAM or POEGMA oligomers with molecular weights below the renal filtration limit. Specifically, methods to fabricate degradable thermoresponsive bulk hydrogels (using a double barrel syringe technique), hydrogel particles (on both the microscale through the use of a microfluidics platform facilitating simultaneous mixing and emulsification of the precursor polymers and the nanoscale through the use of a thermally-driven self-assembly and cross-linking method), and hydrogel nanofibers (using a reactive electrospinning strategy) are described. In each case, hydrogels with temperature-responsive properties similar to those achieved via conventional free radical cross-linking processes can be achieved, but the hydrazone cross-linked network can be degraded over time to re-form the oligomeric precursor polymers and enable clearance. As such, we anticipate these methods (which may be generically applied to any synthetic water-soluble polymer, not just smart materials) will enable easier translation of synthetic smart materials to clinical applications.

Protocols are described for the fabrication of degradable thermoresponsive hydrogels based on hydrazone cross-linking of polymeric oligomers on the bulk scale, microscale, and nanoscale, the latter for preparation of both gel nanoparticles and nanofibers.

자기 조립, 분해 Thermoresponsive Hydrogels 반응 압출, 마이크로, 통해 여러 길이 가늠 자에를 조작 하 고 전기

While various smart materials have been explored for a variety of biomedical applications (e.g., drug delivery, tissue engineering, bioimaging, etc.), ...

생체공학

Electrochemical Preparation of Poly(3,4-Ethylenedioxythiophene) Layers on Gold Microelectrodes for Uric Acid-Sensing Applications

Two different methods for the synthesis of poly(3,4-ethylenedioxythiophene) (PEDOT) on gold electrodes are described, using electropolymerization of 3,4-ethylenedioxythiophene (EDOT) monomer in an aqueous and an organic solution. Cyclic voltammetry (CV) was used in the synthesis of PEDOT thin layers. Lithium perchlorate (LiClO4) was used as a dopant in both aqueous (aqueous/acetonitrile (ACN)) and organic (propylene carbonate (PC)) solvent systems. After the PEDOT layer was created in the organic system, the electrode surface was acclimatized by successive cycling in an aqueous solution for use as a sensor for aqueous samples. 
The use of an aqueous-based electropolymerization method has the potential benefit of removing the acclimatization step to have a shorter sensor preparation time. Although the aqueous method is more economical and environmentally friendly than the organic solvent method, superior PEDOT formation is obtained in the organic solution. The resulting PEDOT electrode surfaces were characterized by scanning electron microscopy (SEM), which showed the constant growth of PEDOT during electropolymerization from the organic PC solution, with rapid fractal-type growth on gold (Au) microelectrodes.

Electrochemical Preparation of Poly3,4-Ethylenedioxythiophene Layers on Gold Microelectrodes for Uric Acid-Sensing Applications

We describe aqueous and organic solvent systems for the electropolymerization of poly(3,4-ethylenedioxythiophene) to create thin layers on the surface of gold microelectrodes, which are used for sensing low molecular weight analytes.

요산 감지 응용 분야를 위한 금 미세전극 위에 폴리(3,4-에틸렌디옥시티오펜) 층의 전기화학적 제조

Two different methods for the synthesis of poly(3,4-ethylenedioxythiophene) (PEDOT) on gold electrodes are described, using electropolymerization of ...

Vapor Phase Deposition of Electroactive Poly(3,4-ethylenedioxythiophene) onto Electrospun Commodity Polymer Nanofibers

This study investigates the preparation of polyacrylonitrile (PAN) nanofibers through electrospinning to create highly porous and strong materials for applications in water purification, electrocatalysis, and biomedicine. The uniformly white PAN nanofiber mats were cut into 2 cm x 2 cm coupons to ensure consistency. After electrospinning, these nanofibers were coated with an electroactive polymer (EAP) using chemical vapor deposition, with iron (III) chloride (FeCl3) serving as an oxidant for polymerizing 3,4-ethylenedioxythiophene (EDOT) into poly(3,4-ethylenedioxythiophene) (PEDOT). The study examined the impact of different FeCl3 concentrations on PEDOT deposition on the PAN coupons. PEDOT deposition led to an increase in coupon weight. Scanning electron microscopy (SEM) revealed increases in the diameter of the nanofibers treated with increasing FeCl3 oxidant concentration, although higher FeCl3&#160;concentrations caused inter-fiber bridging, implying a concomitant decrease in inter-fiber spacing. Energy dispersive X-ray spectroscopy (EDS) was used to confirm the presence of Fe, Cl, and S in the nanofibers, with sulfur content rising with FeCl3&#160;concentration used, suggesting increased PEDOT deposition efficiency with increasing oxidant concentration. Mechanical testing showed that PEDOT-coated PAN fibers had improved tensile strength and toughness in the hydrated state compared to pure PAN nanofibers. These results highlight the crucial role of FeCl3&#160;concentration in influencing the morphology and properties of PAN-PEDOT composites, enhancing their suitability for applications such as water purification, tissue engineering, biosensing, catalysis, and energy storage.

This paper describes a simple technique for coating electrospun PAN nanofibers with electroactive polymers using vapor deposition. The effects of the oxidant FeCl&#8323; on the deposition of poly(3,4-ethylenedioxythiophene) coatings on PAN were investigated to understand and optimize polymer growth, fiber diameter, and overall mechanical strength of the nanofiber mats.

전기 방사 상품 고분자 나노 섬유에 전기 활성 폴리 (3,4- 에틸렌 디옥시 티오펜)의 기상 증착

This study investigates the preparation of polyacrylonitrile (PAN) nanofibers through electrospinning to create highly porous and strong materials for ...