过渡金属硫化物的微波水热合成及其性能研究

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Microwave hydrothermal synthesis and properties of transition metal sulfides

LI Xue ⋅1，2，3，4* ，XU Zhihan’，LI Pengcheng1，LI Guowei 1 ，WU Yuhao 1 ， ZHAO Wenhao' （1.Luoyang Institute of Science and Technology，Luoyang 471023; 2.Henan Key Laboratory of Green Building Materials Manufacturing and Intelligent Equipment，Luoyang471023； 3. Zheng Zhou Research Institute for Abrasives & Grinding Co.，Ltd， Zhengzhou 450001; 4. Zheng Zhou University， Zhengzhou 450001）

Abstract：Transition metal sulfides havedemonstratedconsiderable potential in electrocatalyticaplications，rendering theoptimizationof theirsynthesisandtheregulationoftheirperformanceasubjectof intenseresearchinterest.Inthis study，transitionmetalsulfide-nickel composites were synthesizedusing atwo-step microwave-hydrothermal method.To systematicallyinvestigatetheinfluenceofvarioussynthesisparametersonthestructureandpropertiesoftheresultingproducts，the following experimental strategywas designed：aseriesofsamples were prepared bycontrolling keyvariables，including metal salt concentration （0.01，0.015，0.03，and 0.045 mol·L-1 ），ammonium fluoride concentration （O.oo9，0.019， 0.03，0.076，and 0.114mol⋅L-1 ），as well as the type （thioacetamide and thiourea） and concentration （O.o5， O.1，and 0.15 mol·L -1 ）of sulfur sources.The electrochemical performance of the as-prepared samples was evaluatedusing an electrochemical workstationequippedwith linearsweepvoltammetry （LSV），cyclicvoltammetry（CV），chronopotentiometry（CP）， andelectrochemical impedance spectroscopy（EIS）.Keyparameters such as the Tafel slope，double-layer capacitance（Cdl）， electrochemical activesurfacearea （ECSA），and charge transferresistance （Rct）were furtheranalyzed to systematicalyassess the electrocatalyticperformanceandtherebyoptimizethecompositeformulation.Finally，thesampleexhibitingthebest performance was characterized by X-raydifraction （XRD）and scaning electron microscopy（SEM） to analyze its phase composition，crystal structure，andmicroscopic morphology.Theseresults wereused toelucidate theunderlying mechanisms responsible for the observed electrochemical behavior.

Keywords：microwave hydrothermal method; metal salt concentration; ammonium fluoride;sulfur source; composite

1引言

催化剂是高效绿色化学反应的核心，在能源转化与存储领域意义重大[1-6]。（剩余6171字）