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Chemistry

마이크로파 합성 조건이 수산화니켈 나노시트의 구조에 미치는 영향

Published: August 18th, 2023

DOI:

10.3791/65412

1Materials Science, Engineering, and Commercialization Program, Texas State University, 2Department of Chemistry and Biochemistry, Texas State University, 3Westlake Highschool

수산화 니켈 나노 시트는 마이크로파 보조 열수 반응에 의해 합성됩니다. 이 프로토콜은 마이크로파 합성에 사용되는 반응 온도와 시간이 반응 수율, 결정 구조 및 국부 배위 환경에 영향을 미친다는 것을 보여줍니다.

약산성 조건에서 수산화니켈 나노시트의 신속한 마이크로파 보조 열수 합성을 위한 프로토콜이 제시되고 반응 온도 및 시간이 재료 구조에 미치는 영향을 조사합니다. 연구된 모든 반응 조건은 층상 α-Ni(OH)2 나노시트의 응집체를 생성합니다. 반응 온도와 시간은 재료의 구조와 제품 수율에 큰 영향을 미칩니다. 더 높은 온도에서 α-Ni(OH)2 를 합성하면 반응 수율이 증가하고, 층간 간격이 낮아지고, 결정질 도메인 크기가 증가하고, 층간 음이온 진동 모드의 주파수가 이동하고, 기공 직경이 낮아집니다. 반응 시간이 길수록 반응 수율이 증가하고 결정질 도메인 크기가 비슷해집니다. in situ 반응 압력을 모니터링하면 더 높은 반응 온도에서 더 높은 압력이 얻어진다는 것을 알 수 있습니다. 이 마이크로파 지원 합성 경로는 수많은 에너지 저장, 촉매, 센서 및 기타 응용 분야에 사용되는 다양한 전이 금속 수산화물의 합성 및 생산에 적용할 수 있는 빠르고 처리량이 많으며 확장 가능한 공정을 제공합니다.

수산화 니켈 (OH) 2는 니켈 - 아연 및 니켈 - 금속 수소화물 배터리(1,2,3,4), 연료 전지 4, 물 전해조 4,5,6,7,8,9, 슈퍼 커패시터 4, 광촉매 4, 음이온 교환기 10을 포함한 다양한 응용 분야에 사용됩니다, 및 기타 많은 분석, 전기 화학 및 센서 응용 분야 4,5. Ni(OH)2

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알림: 마이크로파 합성 공정의 개략도view 그림 1에 나와 있습니다.

1. α-Ni(OH)2 나노시트의 마이크로파 합성

  1. 전구체 용액의 제조
    1. 15mL의 초순수(≥18MΩ-cm)와 105mL의 에틸렌 글리콜을 혼합하여 전구체 용액을 준비합니다. Ni (NO3) 5.0g 첨가 2 · 6H2O와 4.1 g의 요소를 용액에 넣고 덮는다.
    2. 전구체 용?.......

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α-Ni(OH)2의 합성에 대한 반응 온도 및 시간의 영향
반응 전, 전구체 용액[Ni(NO3)2·6H2O, 요소, 에틸렌글리콜 및 물]은 pH 4.41 ± 0.10의 투명한 녹색이다(도 2A 및 표 1). 마이크로파 반응의 온도(120°C 또는 180°C)는 in situ 반응 압력과 용액의 색상에 영향을 미칩니다(그림 2B-G

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마이크로파 합성은 기존의 열수 방법(일반적인 반응 시간 4.5시간)에 비해 훨씬 빠른(13-30분 반응 시간) Ni(OH)2를 생성하는 경로를 제공합니다.38. 이 약산성 마이크로파 합성 경로를 사용하여 초박형 α-Ni(OH)2 나노시트를 생성하면 반응 시간과 온도가 결과 물질의 반응 pH, 수율, 형태, 다공성 및 구조에 영향을 미치는 것으로 관찰됩니다. 현장 반응 압력 게이?.......

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SWK와 CPR은 해군 연구실 해군 해저 연구 프로그램(보조금 번호 N00014-21-1-2072)의 지원에 감사드립니다. SWK는 해군 연구 기업 인턴십 프로그램의 지원을 인정합니다. C.P.R과 C.M.은 반응 조건 분석을 위해 미국 국립과학재단(National Science Foundation)의 PREM(Partnerships for Research and Education in Materials) Center for Intelligent Materials Assembly, Award No. 2122041의 지원을 인정합니다.

....

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NameCompanyCatalog NumberComments
ATR-FTIRBrukerTensor II FT-IR spectrometer equipped with a Harrick Scientific SplitPea ATR micro-sampling accessory
Bath sonicatorFisher Scientific15-337-409--
Ethanol VWR analyticalAC61509-0040200 proof
Ethylene GlycolVWR analyticalBDH1125-4LP99% purity
Falcon Centrifuge tubesVWR analytical21008-94050 mL
KimWipesVWR analytical21905-026--
Lab Quest 2Vernier LABQ2--
Microwave ReactorAnton Parr165741Monowave 450
Ni(NO3)2 · 6 H2OWard's Science470301-856Research lab grade
pH ProbeVernier PH-BTACalibrated vs standard pH solutions (pH= 4, 7, 11)
PorosemeterMicromeritics --ASAP 2020. Analysis software: Micromeritics, version 4.03
Powder x-ray diffactometerBrukerAXS Advanced Poweder x-ray diffractometer; d-spacing, and crystallite size analyses were performed using Highscore XRD software, and crystal structures were created using VESTA 3 software.
Reaction vialAnton Parr8272330 mL G30 wideneck, 20 mL max fill capacity
Reaction vial locking lidAnton Parr161724G30 Snap Cap
Reaction vial PTFE septumAnton Parr161728Wideneck
Scanning electron microscopeFEI--Helios Nanolab 400
UreaVWR analyticalBDH4602-500GACS grade

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