저자는 그의 영감과 기술 통찰력, Aerogel 기술에서 스티븐 스타 이너와 육군 연구 실험실-센서와 전자 장치 스파이, 군비 연구, 박사 크리스토퍼 하인즈 박사 Deryn 추 감사 개발 및 엔지니어링 센터, ARDEC-미국 육군 RDECOM, 및 그들의 지원에 대 한 미국 육군 Benet 실험실에서 박사 스티븐 Bartolucci 이 작업을 지원 했다 미국 미국 육군 사관 학교, 웨스트 포인트에서에서 교수 개발 연구 기금 교부 금에 의해.

주의: 사용 하기 전에 모든 관련 안전 데이터 시트 (SDS)를 참조 하십시오. 증기 두건 및 개인 보호 장비를 사용 하 여 포함 하도록 적절 한 안전 관행 화학 반응, 수행할 때 사용 합니다. 급속 한 수소 가스 진화 팝 캡을 일으키는 반응 튜브 및 밖으로 스프레이 솔루션에서 높은 압력을 발생할 수 있습니다. 반응 관 모자 프로토콜에 지정 된 대로 열어 확인 합니다.
1. 금속 젤 준비
<ol><li>
금속 이온 솔루션의 준비입니다.
	<ol>
<li>다음 소금의 0.1 M 솔루션의 2 개 mL를 준비: HAuCl4•3H2O와 나2PdCl4 에서 저온. 준비 2 mL의 0.1 M K2PtCl6 1:1 (v/v)에 물과 에탄올 용 매. 적극적으로 악수와 소용돌이 솔루션 소금의 해산에 도움.</li>
	</ol>
</li>
	<li>
감소 에이전트 솔루션의 준비입니다.
	<ol>
<li>다음 감소 시키는 대리인의 0.1 M 솔루션의 10 mL를 준비: dimethylamine borane (DMAB)와 NaBH4 (나트륨 borohydride).</li>
	</ol>
</li>
	<li>
Au의 준비 젤.
	<ol>
<li>1.7 mL 또는 2.0 mL microcentrifuge 관으로 0.1 m M HAuCl4•3H2O 솔루션의 0.5 mL를 플라스틱. 소금 및 감소 에이전트 솔루션의 빠른 조합을 보장 하기 위해 골드 솔루션 microcentrifuge 튜브에 DMAB의 0.5 mL를 플라스틱 강제로. 일단 솔루션은 혼합 장소 microcentrifuge 튜브 튜브 캡 튜브 랙에 수직으로 엽니다. 참고: 경우 튜브 캡 마감, 수소 가스 진화 뚜껑 팝 열기를 강제 하 고 잠재적으로 감소 혼합물 스프레이를 내부 압력을 발생 합니다.</li>
	</ol>
</li>
	<li>
Pd의 준비 젤.
	<ol>
<li>1.7 mL 또는 2.0 mL microcentrifuge 관으로 0.1 m M 나2PdCl4 솔루션의 0.5 mL를 플라스틱. 강제로 팔라듐 솔루션 microcentrifuge 튜브에 NaBH4 의 0.5 mL를 플라스틱. 장소 microcentrifuge 튜브 튜브 캡 튜브 랙에 수직으로 엽니다.</li>
	</ol>
</li>
	<li>
Pt 준비 젤.
	<ol>
<li>1.7 mL 또는 2.0 mL microcentrifuge 튜브로 0.1 M K2PtCl6 솔루션의 0.5 mL를 플라스틱. 강제로 플래티넘 솔루션 microcentrifuge 튜브에 DMAB의 0.5 mL를 플라스틱. 장소 microcentrifuge 튜브 튜브 캡 튜브 랙에 수직으로 엽니다.</li>
	</ol>
</li>
	<li>
반전 관.
	<ol>
<li>약 5 분, microcentrifuge 튜브 뚜껑과 부드럽게 3-5 시간을 반전 금속 젤의 일부가 아닌 금속 입자의 접착에 도움. 확인 튜브, 반전 후 세척제는 튜브 캡은 즉시 및 바꾸기 튜브 튜브의 수직 방향 유지 선반에.</li>
	</ol>
</li>
	<li>
재래식.<ol>
<li>동안 Au, Pd, Pt 젤 처음 몇 분 안에 형성, 금속 이온의 완전 한 감소 및 표면 자유 에너지를 최소화를 위한 3-6 h 원제 솔루션에서 초기 젤을 둡니다. 참고: 금속 젤 혼합된 금속 이온 및 환 원제 솔루션의 초기 볼륨 보다 작은 볼륨을 차지합니다. 몇 가지 추가적인 약간의 볼륨 수축 평형 시간 동안 관찰 될 수 있습니다 그리고 더 골드 젤에 대 한 발음 이며 오 스 트 발트25숙성 인 것으로.</li>
	</ol>
</li>
	<li>
젤 rinsing.<ol>
<li>재래식 기간 후 Au, Pd, Pt 젤, 초과 감소 에이전트 솔루션을 제거 하지만 금속 젤 침수 되도록 충분 한 솔루션 볼륨을 둡니다. 솔루션 초승달 모양 금속 젤 연락 오지 않는다 있는지 확인 합니다. 참고: 비록 젤은 주걱, 모 세관으로 솔루션 사이의 전송 충분히 안정적인 금속 세력 솔루션 초승달 모양 접촉으로 인해 변형 되며 젤 마지막 aerogel 밀도 증가에 따른 압축. 이 일부 감소 에이전트 솔루션 빠져들 때 전송 저온 젤 튜브에 남아 해야 합니다.</li>
		<li>천천히 반응 microcentrifuge 튜브의 상단에 이온된 물 플라스틱. 이온된 수의 전체 50 mL 원뿔 튜브에 microcentrifuge 튜브 잠수함 고 microcentrifuge 튜브 슬라이드 젤.</li>
		<li>24 h에 대 한 이온된 수에 젤 두고 12 h 물 대체. 젤과 접촉 하는 액체 초승달을 허용 하지 마십시오.</li>
	</ol>
</li>
</ol>2. 전기 화학 표면 영역 (ECSA) 젖은 금속 젤의 특성
참고: 전기 화학 특성 젖은 금속 젤 동결 건조를 실시 이전에 수행 됩니다. 결과 ECSA 다음 최종 aerogel 구조의 표면의 예상 시간입니다. 질소 흡착 측정 말린된 aerogels의 노출 영역을 추정 하는 데 사용 됩니다.
<ol><li>
용 매 교환.<ol>
<li>Au에서 이온된 수의 제거, Pd, 및 태평양 표준시 가능한 솔루션 린스 액체 초승달 모양 젤 연락 오지 않는 확인 하십시오.</li>
		<li>50 mL, 0.5 M KCl 지원 젤 모 공 내의 전해질 이온된 수를 교환 하려면 원뿔 관에 추가 합니다. 24 h를 위한 KCl 해결책에 있는 젤을 둡니다.</li>
	</ol>
</li>
	<li>
작업 전극 준비입니다.
	<ol>
<li>좋은 브러쉬 또는 노출 하는 와이어 끝의 4-5 m m 길이 떠나 다른 응용 프로그램 장치를 사용 하 여 비 반응성 래커로 플래티넘 1 m m 와이어 전극 코트.</li>
		<li>건조 래커에 대 일 분을 허용 합니다.</li>
		<li>옻 칠의 적어도 2 개의 외 투를 적용 하십시오.</li>
	</ol>
</li>
	<li>
3 전극 셀 설정 했다입니다.
	<ol>
<li>3 전극 셀 설정 Ag/AgCl (3m 포화)와 함께 사용 하 여 참조 전극는 0.5 m m 직경 Pt 와이어 보조/카운터 전극 및 래커 코팅된 작업 전극.</li>
		<li>플라스틱 50 mL 원뿔 튜브 반으로 잘라 고 전기 유리병으로 사용 합니다.</li>
		<li>두 가지 방법 중 하나로 작업 전극과 젤 문의: 1) 찔 려 젤, 또는 2) 연락처 모드.<ol>
<li>
작업 전극-찔 려 젤.<ol>
<li>수정 된 50 mL 원뿔 튜브의 하단에 젤으로 부드럽게 삽입 래커 코팅된 전극 젤. 반면 Pd 및 Pt 젤 전극 삽입 시 더 자주 골절 참고: 찔 젤 방법 Au 젤, 더 효과적인 증명 한다.</li>
			</ol>
</li>
			<li>
작업 전극-모드 문의입니다.<ol>
<li>래커 코팅된 작업 전극 내부 표면 따라 원뿔 관으로 삽입 하 고 나머지 작업 전극의 노출된 Pt 와이어 위에 금속 젤.</li>
			</ol>
</li>
		</ol>
</li>
	</ol>
</li>
	<li>
전기 화학 임피던스 분광학 (EIS)입니다.<ol>
<li>Potentiostatic EIS 100 MHz와 10 mV 진폭 사인파를 사용 하 여 1 mHz 사이의 주파수를 사용 하 여 검색을 수행 합니다. 현재 오버플로 경우 동일한 주파수 범위는 100-200 mA 진폭 사인파와 galvanostatic EIS를 사용 합니다.</li>
	</ol>
</li>
	<li>
EIS 데이터에서 전기 화학 표면 영역 (ECSA)의 결정.<ol>
<li>대 한 Z ", 1mhz, 그리고 샘플 질량, m, 분할의 최저 EIS 주파수 f 에서 임피던스의 허수부 다음 방정식 결정 특정 커패시턴스, Csp를 사용 하 여: C sp = 1 / (2 πfZ "m) (1) 참고: 아래 3 단계에서에서 건조 동결 하는 ECSA 젖은 젤 사전에서 결정을 모든 솔루션에서 금속 이온의 젤을 형성 하기 위하여 감소 된다 가정 하 여 질량을 결정 합니다. 이 가정에 따라, 100% 미만 어떤 실제 수익률 발생 합니다 Csp를 과소 평가.</li>
	</ol>
</li>
	<li>
주기적 voltammetry (CV)입니다.<ol>
<li>100, 75, 50, 25, 10, 5, 및 1 mV/s의 스캔 속도 사용 하 여 CV 측정. Au 젤에 대 한 (vs Ag/AgCl)-0.2 0.2 V의 전압 범위를 사용 하 고 0.4에 0.1 V 수소 흡착 및 탈 착, 및 금속의 oxidation-reduction을 피하기 위해 Pd 및 Pt 젤에 대 한 선택.</li>
	</ol>
</li>
	<li>
이력서 데이터에서 전기 화학 표면 영역 (ECSA)의 결정.<ol>
<li>1 mV/s의 느린 이력서 스캔 속도 사용 하 고 특정 커패시턴스는 방정식을 계산: C sp = (∫ivdv) / (2μmΔV) (2) 참고: 여기 i 와 v 는 전류와 잠재력 (A와 V) 이력서 검색, 스캔 속도 μ (V/s), 젤의 질량은 m (g) 이며 δ 는 방전 (vs Ag/AgCl)의 잠재적인 창입니다.</li>
	</ol>
</li>
</ol>3. Aerogel 준비와 특성입니다.
<ol><li>단계 1.8에서 Au, Pd, Pt 젤에 대 한 이온된 린스 물을 제거 하 고 물 초승달 모양 금속 젤 연락 오지 않는다 합니다.</li>
	<li>이상 30 분 전송 냉동된 금속 4의 세트 포인트 압력으로 건조 기 동결으로 젤은 젤-80 ° C 냉동 고에 장소 Pa 또는 낮은.</li>
</ol>

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I. Computations from Nitrogen Isotherms.</a> Journal of the American Chemical Society. 73, 373-380 (1951).</li><li>Brunauer, B., Emmett, P., Teller, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Adsorption+of+Gases+in+Multimolecular+Layers.">Adsorption of Gases in Multimolecular Layers.</a> Journal of the American Chemical Society. 60, 309-319 (1938).</li><li>Herrmann, A., 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=Multimetallic+Aerogels+by+Template-Free+Self-Assembly+of+Au,+Ag,+Pt,+and+Pd+Nanoparticles.">Multimetallic Aerogels by Template-Free Self-Assembly of Au, Ag, Pt, and Pd Nanoparticles.</a> Chemistry of Materials. 26, 1074-1083 (2014).</li><li>Kornyshev, A., Irbakh, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Double-layer+capacitance+on+a+rough+metal+surface.">Double-layer capacitance on a rough metal surface.</a> Physical Review E. 53, 6192-6199 (1996).</li><li>Bisquert, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Influence+of+the+boundaries+in+the+impedance+of+porous+film+electrodes.">Influence of the boundaries in the impedance of porous film electrodes.</a> Physical Chemistry Chemical Physics. 2, 4185-4192 (2000).</li><li>Bisquert, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Theory+of+the+Impedance+of+Electron+Diffusion+and+Recombination+in+a+Thin+Layer.">Theory of the Impedance of Electron Diffusion and Recombination in a Thin Layer.</a> Journal of Physical Chemistry B. 106, 325-333 (2002).</li><li>Lu, K., Yuan, L., Xin, X., Xu, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hybridization+of+graphene+oxide+with+commercial+graphene+for+constructing+3D+metal-free+aerogel+with+enhanced+photocatalysis.">Hybridization of graphene oxide with commercial graphene for constructing 3D metal-free aerogel with enhanced photocatalysis.</a> Applied Catalysis B. 226, 16-22 (2018).</li><li>Nystron, G., Roder, L., Fernandez-Ronco, M., Mezzenga, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Amyloid+Templated+Organic+Inorganic+Hybrid+Aerogels.">Amyloid Templated Organic Inorganic Hybrid Aerogels.</a> Advanced Functional Materials. , 1703609-1703620 (2017).</li></ol>

저자는 공개 없다.

고귀한 금속 aerogel 합성 방법 느린 합성 기법에 버금가 다공성, 높은 표면적 monoliths의 급속 한 형성에 결과 여기 발표. 감소 에이전트 솔루션 비율을 1:1 (v/v) 금속 이온 솔루션 제안된 젤 형성 모델을 용이 하 게 중요 하다. 금속 이온의 전기 화학 감소의 결과로 급속 한 수소 가스 진화 보조 원제 역할 densification, 그리고 젤 형성 동안 성장 하는 나노 입자의 융합을 촉진 한다. 표 1 에 표?...

에너지 저장 및 변환, 촉매, 센서 응용 프로그램의 다양 한 화학 반응성, 및 대량 전송 속성1,2,제어를 제공 하는 3 차원 금속 nanostructures에서 혜택 3,,45. 이러한 3 차원 금속 nanostructures 추가 향상 전도도, 연 성가 단성, 그리고 강도8,9. 장치에 통합 자료 무료 서 또는 지원 자료와 결합 된 것 필요로 한다. 지원 구조에 나노 재료의 활성 소재, 최소화 하는 수단을 제공 하지만 약한 흡착 및 장치 작업10,11동안 궁극적인 덩어리에서 고통을 수 있습니다.
다양 한 합성 방법 개별 나노 입자 크기와 모양을 제어 하는, 몇 가지 접근 연속 3 차원 나노 소재12,,1314제어 가능 고귀한 금속 3 차원 nanostructures의 단 분산 나노 입자, 졸-겔 형성, 나노 접착, 복합 재료, 나노, 체인과 biotemplating15,16 dithiol 결합을 통해 형성 된 , 17 , 18. 이러한 방법의 많은 합성 시간 일 원하는 자료를 주 순서 필요. 선구자 소금 솔루션의 직접적인 감소에서 합성 하는 고귀한 금속 nanofoams 길이, 마이크로미터의 수백의 단거리 순서와 빠른 합성 날짜 표시줄 함께 준비 된 하지만 기계 장치 통합을 위한 눌러 필요 19 , 20.
Kistler에 의해 처음 보고, aerogels 높은 특정 표면 영역 크기 순서 그들의 대량 소재 대응21,,2223 보다 적게 조밀한과 다공성 구조를 달성 하기 위해 합성 경로 제공 . 벌크 재료의 거시적인 길이 규모에 3 차원 구조를 확장 나노 집계 또는 지원 자료 또는 기계 가공을 필요로 하는 nanofoams에 이점을 제공 합니다. 그러나 Aerogels 제공 다공성 및 입자 기능 크기,, 제어 합성 경로 확장 합성 시간, 그리고 일부 경우 대리인 또는 링커 분자, 증가 전반적인 처리 단계 및 시간 상한의 사용.
여기 금, 팔라듐, 그리고 신속 하 고 직접적인 솔루션 기반 감소를 통해 플래티넘 aerogels를 합성 하는 방법24를제공 됩니다. 1: 1에서 감소 시키는 대리인으로 다양 한 전조 고귀한 금속 이온을 결합 분 초 이내 금속 젤의 형성에 (v/v) 비 결과 비교 솔-젤 같은 다른 기술에 대 한 합성 시간이 훨씬 더 오래. Microcentrifuge 튜브 또는 작은 볼륨 원뿔 튜브의 사용 감소 단계 촉진 제안된 nucleation, 성장, densification, 퓨전, 젤 형성에 대 한 평형 모델의 부산물로 서 활발 한 수소 가스 진화를 활용 합니다. Aerogel nanostructure 기능 크기에 가까운 상관 전자 현미경 이미지 분석, x 선 diffractometry, 질소 가스 흡착, 전기 화학 임피던스 분광학, 및 순환 voltammetry 스캔으로 결정 됩니다. 솔벤트 액세스할 수 특정 표면 영역 전기 화학 임피던스 분광학 및 주기적 voltammetry 결정 됩니다. 이 합성 방법 고귀한 금속 aerogels monoliths는 신속 하 고 직접적인 감소 방식으로 얻을 수 있습니다 그 높은 특정 표면 영역을 보여 줍니다.

<table border="0" cellpadding="0" cellspacing="0" width="691">
	<tbody>
		<tr height="25">
			<td height="25" style="height:25px;width:215px;">HAuCl4&#376;&#8226;3H2O&#160;</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">16961-25-4</td>
			<td style="width:229px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:215px;">Na2PdCl4</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">13820-40-1</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:215px;">K2PtCl6</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">16921-30-5</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Pd(NH3)4Cl2</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">13933-31-8</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">K2PtCl4</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">10025-99-7</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Pt(NH3)4Cl2&#376;&#8226;H2O</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">13933-31-8</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">dimethylamine borane (DMAB)</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">74-94-2</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:215px;">NaBH4</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">16940-66-2</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:215px;">NaH2PO2&#376;&#8226;H2O</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td style="width:119px;">10039-56-2</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Ethanol</td>
			<td style="width:128px;">Sigma-Aldrich</td>
			<td>792780</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:215px;">Snap Cap Microcentrifuge Tubes, 2.0 mL</td>
			<td style="width:128px;">Cole Parmer</td>
			<td>UX-06333-70</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:215px;">Snap Cap Microcentrifuge Tubes, 1.7 mL</td>
			<td style="width:128px;">Cole Parmer</td>
			<td>UX-06333-60</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Conical Centrifuge Tubes 15mL</td>
			<td style="width:128px;">Stellar Scientific</td>
			<td>T15-101&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Ag/AgCl Reference Electrode</td>
			<td style="width:128px;">BASi</td>
			<td style="width:119px;">MF-2052</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Pt wire electrode</td>
			<td style="width:128px;">BASi</td>
			<td style="width:119px;">MF-4130</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:215px;">Miccrostop Lacquer</td>
			<td style="width:128px;">Tober Chemical Division</td>
			<td style="width:119px;">NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Potentiostat</td>
			<td style="width:128px;">Biologic-USA</td>
			<td style="width:119px;">VMP-3</td>
			<td>Electrochemical analysis-EIS, CV</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:215px;">Freeze Dryer</td>
			<td style="width:128px;">Labconco</td>
			<td style="width:119px;">Freezone 2.5 Liter</td>
			<td>Aerogel freeze drying</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">XRD</td>
			<td style="width:128px;">PanAlytical</td>
			<td style="width:119px;">Empyrean</td>
			<td>X-ray diffractometry</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:215px;">Surface and Pore Analyzer</td>
			<td style="width:128px;">Quantachrome</td>
			<td style="width:119px;">NOVA 4000e</td>
			<td>Nitrogen gas adsorption</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:215px;">ImageJ, Image analysis software</td>
			<td style="width:128px;">National Institute of Health</td>
			<td style="width:119px;">NA</td>
			<td>SEM image analysis</td>
		</tr>
	</tbody>
</table>

a rapid synthesis method for au, pd, and pt aerogels via direct solution-based reduction

여기, 금, 팔라듐, 그리고 신속 하 고 직접적인 솔루션 기반 감소를 통해 플래티넘 aerogels를 합성 하는 방법을 제시 합니다. 감소 시키는 대리인 분 초 이내 금속 젤의 형성에서 1:1 (v/v) 비율 결과에 다양 한 전조 고귀한 금속 이온의 조합에 비해 솔-젤 같은 다른 기술에 대 한 합성 시간이 훨씬 더 오래. microcentrifuge에서 감소 단계를 실시 튜브 또는 작은 볼륨 원뿔 튜브 용이 제안된 nucleation, 성장, densification, 퓨전, 젤 형성, 초기 반응 볼륨 보다 작은 마지막 젤 형상에 대 한 평형 모델. 이 메서드는 부산물로 감소 단계, 그리고 시 약 농도 결과로 서 활발 한 수소 가스의 활용. 솔벤트 액세스할 수 특정 표면 영역 전기 화학 임피던스 분광학 및 주기적 voltammetry 결정 됩니다. 헹 구 고 동결 건조, 후 스캐닝 전자 현미경, x 선 diffractometry, 및 질소 가스 흡착과 결과 aerogel 구조를 검사 합니다. 합성 방법 및 특성화 기술 결과에 가까운 통신 aerogel 인 대 크기의. 이 합성 방법 고귀한 금속 aerogels monoliths는 신속 하 고 직접적인 감소 방식으로 얻을 수 있습니다 그 높은 특정 표면 영역을 보여 줍니다.

금속 이온과 환 원제 솔루션 함께 결과의 즉시 격렬 한 가스 발전으로 어두운 블랙 색상을 선회 하는 솔루션에 추가. 반응 진행의 그림 1에 표시 된 제안 된 젤 형성 메커니즘을 제안 합니다. 젤 대형 1) 나노 nucleation, 2) 성장, 3) densification, 4) 융합, 및 5) 평형의 5 단계까지 진행합니다. 처음 네 단계는 반응, 평형 젤 원제 솔루션에 남아 하 고 이온된 수 ?...

Watch this Scientific Journal Video about A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction at JoVE.com

A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction

Au, Pd, Pt Aerogels 직접 솔루션 기반 감소를 통해 빠른 합성 방법

Au, Pd, Pt aerogels를 신속 하 고 직접적인 솔루션 기반 감소 합성 방법은 제공 됩니다.

Here, a method to synthesize gold, palladium, and platinum aerogels via a rapid, direct solution-based reduction is presented. The combination of various ...

a-rapid-synthesis-method-for-au-pd-pt-aerogels-via-direct-solution

Research

JoVE Journal

Chemistry

8.6K 조회수.  United States Military Academy, West Point. Au, Pd, Pt aerogels를 신속 하 고 직접적인 솔루션 기반 감소 합성 방법은 제공 됩니다.

비디오: A Rapid Synthesis Method for Au, Pd, and Pt Aerogels Via Direct Solution-Based Reduction

Preparing Silica Aerogel Monoliths via a Rapid Supercritical Extraction Method

A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The procedure requires 15-20 min of preparation time, during which a liquid precursor mixture is prepared and poured into wells of a metal mold that is placed between the platens of a hydraulic hot press, followed by several hours of processing within the hot press. The precursor solution consists of a 1.0:12.0:3.6:3.5 x 10-3 molar ratio of tetramethylorthosilicate (TMOS):methanol:water:ammonia. In each well of the mold, a porous silica sol-gel matrix forms. As the temperature of the mold and its contents is increased, the pressure within the mold rises. After the temperature/pressure conditions surpass the supercritical point for the solvent within the pores of the matrix (in this case, a methanol/water mixture), the supercritical fluid is released, and monolithic aerogel remains within the wells of the mold. With the mold used in this procedure, cylindrical monoliths of 2.2 cm diameter and 1.9 cm height are produced. Aerogels formed by this rapid method have comparable properties (low bulk and skeletal density, high surface area, mesoporous morphology) to those prepared by other methods that involve either additional reaction steps or solvent extractions (lengthier processes that generate more chemical waste).The rapid supercritical extraction method can also be applied to the fabrication of aerogels based on other precursor recipes.

This article describes a rapid supercritical extraction method for fabricating silica aerogels. By utilizing a confined mold and hydraulic hot press, monolithic aerogels can be made in eight hours or less.

빠른 초 임계 추출 방법을 통해 실리카 에어로젤, 모노 리드 (monolith)를 준비

A procedure for the fabrication of monolithic silica aerogels in eight hours or less via a rapid supercritical extraction process is described. The ...

연구

화학

Synthesis, Characterization, and Functionalization of Hybrid Au/CdS and Au/ZnS Core/Shell Nanoparticles

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large extinction coefficients which can be tuned across the visible spectrum. Research into the plasmonic enhancement of optical transitions has become popular, due to the possibility of altering and in some cases improving photo-absorption or emission properties of nearby chromophores such as molecular dyes or quantum dots. The electric field of the plasmon can couple with the excitation dipole of a chromophore, perturbing the electronic states involved in the transition and leading to increased absorption and emission rates. These enhancements can also be negated at close distances by energy transfer mechanism, making the spatial arrangement of the two species critical. Ultimately, enhancement of light harvesting efficiency in plasmonic solar cells could lead to thinner and, therefore, lower cost devices. The development of hybrid core/shell particles could offer a solution to this issue. The addition of a dielectric spacer between a gold nanoparticles and a chromophore is the proposed method to control the exciton plasmon coupling strength and thereby balance losses with the plasmonic gains. A detailed procedure for the coating of gold nanoparticles with CdS and ZnS semiconductor shells is presented. The nanoparticles show high uniformity with size control in both the core gold particles and shell species allowing for a more accurate investigation into the plasmonic enhancement of external chromophores.

The synthesis of uniform gold nanoparticles coated with semiconductor shells of CdS or ZnS is performed. The semiconductor coating is conducted by first depositing a silver sulfide shell and exchanging the silver cations for zinc or cadmium cations.

합성, 특성 및 하이브리드 금 / CD 및 금 /은 ZnS 코어 / 쉘 나노 입자의 작용 화

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large ...

A Method to Manipulate Surface Tension of a Liquid Metal via Surface Oxidation and Reduction

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where interfacial tension is a dominant force. A variety of methods exist for controlling the interfacial tension of aqueous and organic liquids on this scale; however, these techniques have limited utility for liquid metals due to their large interfacial tension.
Liquid metals can form soft, stretchable, and shape-reconfigurable components in electronic and electromagnetic devices. Although it is possible to manipulate these fluids via mechanical methods (e.g., pumping), electrical methods are easier to miniaturize, control, and implement. However, most electrical techniques have their own constraints: electrowetting-on-dielectric requires large (kV) potentials for modest actuation, electrocapillarity can affect relatively small changes in the interfacial tension, and continuous electrowetting is limited to plugs of the liquid metal in capillaries.
Here, we present a method for actuating gallium and gallium-based liquid metal alloys via an electrochemical surface reaction. Controlling the electrochemical potential on the surface of the liquid metal in electrolyte rapidly and reversibly changes the interfacial tension by over two orders of magnitude ( &#820;500 mN/m to near zero). Furthermore, this method requires only a very modest potential (&#60; 1 V) applied relative to a counter electrode. The resulting change in tension is due primarily to the electrochemical deposition of a surface oxide layer, which acts as a surfactant; removal of the oxide increases the interfacial tension, and vice versa. This technique can be applied in a wide variety of electrolytes and is independent of the substrate on which it rests.

We present a method to control the interfacial energy of a liquid metal in an electrolyte via electrochemical deposition (or removal) of a surface oxide layer. This simple method can control the capillary behavior of gallium-based liquid metals by tuning the interfacial energy rapidly, significantly, and reversibly using modest voltages.

방법은 표면 산화와 환원을 통해 액체 금속의 표면 장력을 조작

Controlling interfacial tension is an effective method for manipulating the shape, position, and flow of fluids at sub-millimeter length scales, where ...

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the development of antibody drug conjugates (ADCs) and nanomedicine, fluorescent microscopy and systems chemistry. For many of these applications, specificity of the bioconjugation method used is of prime concern. The Michael addition of maleimides with cysteine(s) on the target proteins is highly selective and proceeds rapidly under mild conditions, making it one of the most popular methods for protein bioconjugation.
We demonstrate here the modification of the only surface-accessible cysteine residue on yeast cytochrome c with a ruthenium(II) bisterpyridine maleimide. The protein bioconjugation is verified by gel electrophoresis and purified by aqueous-based fast protein liquid chromatography in 27% yield of isolated protein material. Structural characterization with MALDI-TOF MS and UV-Vis is then used to verify that the bioconjugation is successful. The protocol shown here is easily applicable to other cysteine - maleimide coupling of proteins to other proteins, dyes, drugs or polymers.

Synthesis of Protein Bioconjugates via Cysteine-maleimide Chemistry

This protocol details the important steps required for the bioconjugation of a cysteine containing protein to a maleimide, including reagent purification, reaction conditions, bioconjugate purification and bioconjugate characterization.

The chemical linking or bioconjugation of proteins to fluorescent dyes, drugs, polymers and other proteins has a broad range of applications, such as the ...

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of Chalcogenidoplumbates(II or IV)

The phases of &#34;PbCh2&#34; (Ch = Se, Te) are obtained from solid-state syntheses (i.e., by the fusion of the elements under inert conditions in silica glass ampules). Reduction of such phases by elemental alkaline metals in amines affords crystalline chalcogenidoplumbate(II) salts comprised of [PbTe3]2- or [Pb2Ch3]2- anions, depending upon which sequestering agent for the cations is present: crown ethers, like 18-crown-6, or cryptands, like [2.2.2]crypt. Reactions of solutions of such anions with transition-metal compounds yield (poly-)chalcogenide anions or transition-metal chalcogenide clusters, including one with a &#181;-PbSe ligand (i.e., the heaviest-known CO homolog).
In contrast, the solid-state synthesis of a phase of the nominal composition &#34;K2PbSe2&#34; by successive reactions of the elements and by the subsequent solvothermal treatment in amines yields the first non-oxide/halide inorganic lead(IV) compound: a salt of the ortho-selenidoplumbate(IV) anion [PbSe4]4-. This was unexpected due to the redox potentials of Pb(IV) and Se(-II). Such methods can further be applied to other elemental combinations, leading to the formation of solutions with binary [HgTe2]2- or [BiSe3]3- anions, or to large-scale syntheses of K2Hg2Se3 or K3BiSe3 via the solid-state route.
All compounds are characterized by single-crystal X-ray diffraction and elemental analysis; solutions of plumbate salts can be investigated by 205Pb and 77Se or 127Te NMR techniques. Quantum chemical calculations using density functional theory methods enable energy comparisons. They further allow for insights into the electronic configuration and thus, the bonding situation. Molecular Rh-containing Chevrel-type compounds were found to exhibit delocalized mixed valence, whereas similar telluridopalladate anions are electron-precise; the cluster with the &#181;-PbSe ligand is energetically favored over a hypothetical CO analog, in line with the unsuccessful attempt at its synthesis. The stability of formal Pb(IV) within the [PbSe4]4- anion is mainly due to a suitable stabilization within the crystal lattice.

Combining Solid-state and Solution-based Techniques: Synthesis and Reactivity of ChalcogenidoplumbatesII or IV

The synthesis of chalcogenidoplumbates(II,IV) via the in situ reduction of nominal "PbCh2" (Ch = Chalcogen) and via a solid-state reaction and subsequent solvothermal reactions is presented. Additionally, reactivities of plumbate(II) solutions are portrayed, which yield the heaviest-known CO homolog known to date: the &#181;-PbSe ligand.

고체 및 솔루션 기반의 기술 결합 : 합성 및 Chalcogenidoplumbates의 반응성 (II 또는 IV)

The phases of &#34;PbCh2&#34; (Ch = Se, Te) are obtained from solid-state syntheses (i.e., by the fusion of the elements under inert conditions in silica ...

Synthesis and Testing of Supported Pt-Cu Solid Solution Nanoparticle Catalysts for Propane Dehydrogenation

A convenient method for the synthesis of bimetallic Pt-Cu catalysts and performance tests for propane dehydrogenation and characterization are demonstrated here. The catalyst forms a substitutional solid solution structure, with a small and uniform particle size around 2 nm. This is realized by careful control over the impregnation, calcination, and reduction steps during catalyst preparation and is identified by advanced in situ synchrotron techniques. The catalyst propane dehydrogenation performance continuously improves with increasing Cu:Pt atomic ratio.

A convenient method for the synthesis of 2 nm supported bimetallic nanoparticle Pt-Cu catalysts for propane dehydrogenation is reported here. In situ synchrotron X-ray techniques allow for the determination of the catalyst structure, which is typically unobtainable using laboratory instruments.

프로판 탈수 소화를위한 Pt-Cu 고용체 나노 입자 촉매 합성 및 시험

A convenient method for the synthesis of bimetallic Pt-Cu catalysts and performance tests for propane dehydrogenation and characterization are ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

백 금-니켈 나노 와이어 및 산소 감소 성능 최적화의 합성

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Fabrication and Testing of Catalytic Aerogels Prepared Via Rapid Supercritical Extraction

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three preparation methods are described: (a) the incorporation of metal salts into silica or alumina wet gels using an impregnation method; (b) the incorporation of metal salts into alumina wet gels using a co-precursor method; and (c) the addition of metal nanoparticles directly into a silica aerogel precursor mixture. The methods utilize a hydraulic hot press, which allows for rapid (&#60;6 h) supercritical extraction and results in aerogels of low density (0.10 g/mL) and high surface area (200-800 m2/g). While the work presented here focuses on the use of copper salts and copper nanoparticles, the approach can be implemented using other metal salts and nanoparticles. A protocol for testing the three-way catalytic ability of these aerogels for automotive pollution mitigation is also presented. This technique uses custom-built equipment, the Union Catalytic Testbed (UCAT), in which a simulated exhaust mixture is passed over an aerogel sample at a controlled temperature and flow rate. The system is capable of measuring the ability of the catalytic aerogels, under both oxidizing and reducing conditions, to convert CO, NO and unburned hydrocarbons (HCs) to less harmful species (CO2, H2O and N2). Example catalytic results are presented for the aerogels described.

Here we present protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms. Methods for preparing materials using copper salts and copper-containing nanoparticles are featured. Catalytic testing protocols demonstrate the effectiveness of these aerogels for three-way catalysis applications.

제조 및 급속 한 초 임계 추출 통해 준비 촉매 Aerogels의 테스트

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three ...

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity in aqueous CO2 reduction. Different from traditional metal nanocrystals, the synthesis of metal single atoms involves a matrix material that can confine those single atoms and prevent them from aggregation. We report an electrospinning and thermal annealing method to prepare Ni single atoms dispersed and coordinated in a graphene shell, as active centers for CO2 reduction to CO. During the synthesis, N dopants play a critical role in generating graphene vacancies to trap Ni atoms. Aberration-corrected scanning transmission electron microscopy and three-dimensional atom probe tomography were employed to identify the single Ni atomic sites in graphene vacancies. Detailed setup of electrochemical CO2 reduction apparatus coupled with an on-line gas chromatography is also demonstrated. Compared to metallic Ni, Ni single atom catalyst exhibit dramatically improved CO2 reduction and suppressed H2 evolution side reaction.

Synthesis and Performance Characterizations of Transition Metal Single Atom Catalyst for Electrochemical CO2 Reduction

Here, we present a protocol for the synthesis and electrochemical testing of transition metal single atoms coordinated in graphene vacancies as active centers for selective carbon dioxide reduction to carbon monoxide in aqueous solutions.

합성 및 전기 화학적 CO2 감소를 위한 전이 금속 단일 원자 촉매의 성능 Characterizations

This protocol presents both the synthesis method of the Ni single atom catalyst, and the electrochemical testing of its catalytic activity and selectivity ...

Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a challenge, as it requires asymmetric growth of symmetric crystals. Here, we report a distinctive synthesis of substrate-bound Au nanowires. This template-free synthesis employs thiolated ligands and substrate adsorption to achieve the continuous asymmetric deposition of Au in solution at ambient conditions. The thiolated ligand prevented the Au deposition on the exposed surface of the seeds, so the Au deposition only occurs at the interface between the Au seeds and the substrate. The side of the newly deposited Au nanowires is immediately covered with the thiolated ligand, while the bottom facing the substrate remains ligand-free and active for the next round of Au deposition. We further demonstrate that this Au nanowire growth can be induced on various substrates, and different thiolated ligands can be used to regulate the surface chemistry of the nanowires. The diameter of the nanowires can also be controlled with mixed ligands, in which another &#34;bad&#34; ligand could turn on the lateral growth. With the understanding of the mechanism, Au nanowire-based nanostructures can be designed and synthesized.

We report a solution-based method to synthesize substrate-bound Au nanowires. By tuning the molecular ligands used during the synthesis, the Au nanowires can be grown from various substrates with different surface properties. Au nanowire-based nanostructures can also be synthesized by adjusting the reaction parameters.