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Materials

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Chemistry

Effekt av mikrobølgesyntesebetingelser på strukturen av nikkelhydroksid nanoark

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

Nikkelhydroksid nanoark syntetiseres ved en mikrobølgeassistert hydrotermisk reaksjon. Denne protokollen demonstrerer at reaksjonstemperaturen og tiden som brukes til mikrobølgesyntese påvirker reaksjonsutbyttet, krystallstrukturen og det lokale koordinasjonsmiljøet.

En protokoll for rask, mikrobølgeassistert hydrotermisk syntese av nikkelhydroksid nanoark under mildt sure forhold presenteres, og effekten av reaksjonstemperatur og tid på materialets struktur undersøkes. Alle undersøkte reaksjonsbetingelser resulterer i aggregater av lagdelte α-Ni (OH) 2 nanoark. Reaksjonstemperaturen og tiden påvirker sterkt strukturen til materialet og produktutbyttet. Syntetisering av α-Ni(OH)2 ved høyere temperaturer øker reaksjonsutbyttet, senker mellomlagsavstanden, øker krystallinsk domenestørrelse, forskyver frekvensene til mellomlags anionvibrasjonsmoduser og senker porediameteren. Lengre reaksjonstider øker reaksjonsutbyttet og resulterer i lignende krystallinske domenestørrelser. Overvåking av reaksjonstrykket in situ viser at høyere trykk oppnås ved høyere reaksjonstemperaturer. Denne mikrobølgeassisterte synteseruten gir en rask, høy gjennomstrømning, skalerbar prosess som kan brukes til syntese og produksjon av en rekke overgangsmetallhydroksider som brukes til en rekke energilagring, katalyse, sensor og andre applikasjoner.

Nikkelhydroksid, Ni(OH)2, brukes til en rekke bruksområder, inkludert nikkel-sink og nikkel-metallhydridbatterier 1,2,3,4, brenselceller4, vannelektrolysatorer 4,5,6,7,8,9, superkondensatorer4, fotokatalysatorer 4, anionbyttere10, og mange a....

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MERK: Den skjematiske oversikten over mikrobølgesynteseprosessen er presentert i figur 1.

1. Mikrobølgesyntese av α-Ni (OH) 2 nanoark

  1. Fremstilling av forløperløsning
    1. Forbered forløperoppløsningen ved å blande 15 ml ultrarent vann (≥18 MΩ-cm) og 105 ml etylenglykol. Tilsett 5,0 g Ni(NO3)2 · 6 H2O og 4, 1 g urea til løsningen og dekselet.
    2. Plasser forløperløsningen.......

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Påvirkning av reaksjonstemperatur og tid på syntesen av α-Ni(OH)2
Før reaksjonen er forløperløsningen [Ni (NO3) 2 · 6 H2O, urea, etylenglykol og vann] en gjennomsiktig grønn farge med en pH på 4,41 ± 0,10 (figur 2A og tabell 1). Temperaturen i mikrobølgereaksjonen (enten 120 °C eller 180 °C) påvirker reaksjonstrykket og fargen på løsningen (figur 2B-G

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Mikrobølgesyntese gir en rute for å generere Ni (OH) 2 som er betydelig raskere (13-30 min reaksjonstid) i forhold til konvensjonelle hydrotermale metoder (typiske reaksjonstider på 4,5 timer) 38. Ved å bruke denne mildt sure mikrobølgesynteseruten for å produsere ultratynne α-Ni (OH) 2 nanoark, observeres det at reaksjonstid og temperatur påvirker reaksjonens pH, utbytte, morfologi, porøsitet og struktur av de resulterende materialene. Ved bruk av en in situ rea.......

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S.W.K. og C.P.R. takker for støtte fra Office of Naval Research Navy Undersea Research Program (Grant No. N00014-21-1-2072). S.W.K. anerkjenner støtte fra Naval Research Enterprise Internship Program. CPR og CM anerkjenner støtte fra National Science Foundation Partnerships for Research and Education in Materials (PREM) Center for Intelligent Materials Assembly, Award No. 2122041, for analyse av reaksjonsbetingelsene.

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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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