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Chemistry

Effet des conditions de synthèse par micro-ondes sur la structure des nanofeuilles d’hydroxyde de nickel

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

Les nanofeuilles d’hydroxyde de nickel sont synthétisées par une réaction hydrothermale assistée par micro-ondes. Ce protocole démontre que la température et le temps de réaction utilisés pour la synthèse par micro-ondes affectent le rendement de la réaction, la structure cristalline et l’environnement de coordination locale.

Un protocole de synthèse hydrothermale rapide, assistée par micro-ondes, de nanofeuilles d’hydroxyde de nickel dans des conditions légèrement acides est présenté, et l’effet de la température et du temps de réaction sur la structure du matériau est examiné. Toutes les conditions de réaction étudiées aboutissent à des agrégats de nanofeuillets de α-Ni(OH)2 stratifiés. La température et le temps de réaction influencent fortement la structure du matériau et le rendement du produit. La synthèse de α-Ni(OH)2 à des températures plus élevées augmente le rendement de la réaction, réduit l’espacement entre les couches, augmente la taille du domaine cristallin, déplace les fréquences des modes vibratoires des anions intercalaires et abaisse le diamètre des pores. Des temps de réaction plus longs augmentent les rendements de réaction et permettent d’obtenir des tailles de domaine cristallin similaires. La surveillance de la pression de réaction in situ montre que des pressions plus élevées sont obtenues à des températures de réaction plus élevées. Cette voie de synthèse assistée par micro-ondes fournit un processus rapide, à haut débit et évolutif qui peut être appliqué à la synthèse et à la production d’une variété d’hydroxydes de métaux de transition utilisés pour de nombreuses applications de stockage d’énergie, de catalyse, de capteurs et autres.

L’hydroxyde de nickel, Ni(OH)2, est utilisé pour de nombreuses applications, notamment les batteries nickel-zinc et nickel-hydrure métallique 1,2,3,4, les piles à combustible4, les électrolyseurs d’eau 4,5,6,7,8,9, les supercondensateurs4, les photocatalyseurs 4, les échangeurs d’anions

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NOTE : La figure 1 présente un aperçu schématique du procédé de synthèse par micro-ondes.

1. Synthèse par micro-ondes de nanofeuillets de α-Ni(OH)2

  1. Préparation de la solution de précurseur
    1. Préparer la solution de précurseur en mélangeant 15 mL d’eau ultrapure (≥18 MΩ-cm) et 105 mL d’éthylène glycol. Ajouter 5,0 g de Ni(NO3)2 · 6 H2O et 4,1 g d’urée dans la solut.......

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Influence de la température et du temps de réaction sur la synthèse du α-Ni(OH)2
Avant la réaction, la solution de précurseur [Ni(NO3)2 · 6 H2O, urée, éthylène glycol et eau] est de couleur verte transparente avec un pH de 4,41 ± 0,10 (Figure 2A et Tableau 1). La température de la réaction micro-ondes (120 °C ou 180 °C) influence la pression de réaction in situ et la couleur de la soluti.......

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La synthèse par micro-ondes fournit une voie pour générer du Ni(OH)2 qui est nettement plus rapide (temps de réaction de 13 à 30 minutes) par rapport aux méthodes hydrothermales conventionnelles (temps de réaction typiques de 4,5 h)38. En utilisant cette voie de synthèse par micro-ondes légèrement acide pour produire des nanofeuilles de α-Ni(OH)2 ultraminces, on observe que le temps de réaction et la température influencent le pH de la réaction, les rendements, .......

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S.W.K. et le C.P.R. remercient chaleureusement l’Office of Naval Research Ship Research Program (subvention n° N00014-21-1-2072). S.W.K. remercie le Naval Research Enterprise Internship Program pour son soutien. Le C.P.R et le C.M. reconnaissent le soutien du Centre pour l’assemblage intelligent des matériaux (PREM) de la National Science Foundation (PREM), prix n° 2122041, pour l’analyse des conditions de réaction.

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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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