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APPLICATIONOFHYDROTHERMALMETHODINMATERIALSYNTHESISANDPREPARATIONPresenter:GuoYueMembersofourgroup:HeXiaodong,

GuoYue,GuanRunnan,HuangMeng,DingXiang,XiaoLina,ZhuDongyang,HuZhiqiu,LiJingshi,XuYongjian,WuHuanpeng,QiangZiyueContentsHistoryandCurrentSituationofHydrothermalProcessP1.FundamentalsExamplesofApplicationP2.P3.SupercapacitorsLithiumIonBatteriesSolarBatteriesPart1HistoryandCurrentSituation4Part.1Part.2Part.3DevelopmentofHydrothermalProcessDiscovery:1845,K.F.Eschafhautlfirstlypreparedquartzcrystalsbyusingsilicicacidasrawmaterial.By1900morethan150mineralspeciesweresynthesizedincludingdiamond.Foundation:In1900,G.W.MoreyandhiscolleaguesattheWashingtonGeophysicalLaboratoryestablishedthetheoryofhydrothermalmethod.In1940s,S.Somiyahasgiventheearlystageofhydrothermalresearch.Transition:AfterWorldWarII,hydrothermalmethodbegantobeusedinthepreparationofsyntheticchemicalmaterials.Pioneer:Commercialapplicationofthehydrothermaltechniquebeganin1908whenK.J.Bayerleachedbauxitemineralunderhydrothermalconditionstoobtainaluminium.In1940s,S.Somiyahasgiventheearlystageofhydrothermalresearch.5Part.1Part.2Part.3DevelopmentofmaterialsJournalofMaterialsScience,2008,43(7):2085-2103.6Part.1Part.2Part.3NewmethodsofHydrothermalProcessMulti-energyhydrothermalmaterialsprocessing:ResearchersattheTokyoInstituteofTechnologyfirstattemptedhydrothermalreactionswithelectrochemicalandmechanicalenergyandestablishedanewtrendinin1970sand1980s.Microwaveandsonarinthehydrothermalreactions:MaterialsResearchLaboratoryatthePennStatewellexploredthepossibilitiesofmicrowaveandsonarinthehydrothermalreactions

in1990s.Supercriticalhydrothermalsynthesis:Themethodisdevelopedfrom1990s,thesupercriticalhydrothermalapparatuscanchangethedielectricconstantandsolventdensityofwaterbychangingthetemperatureandpressure,soastochangesomechemicalreactions.7Part.1Part.2Part.3PublicationsKeywords:Hydrothermal,preparation,material,synthesisPart2Fundamentals9Part.2Part.1Part.3FundamentalsHydrothermalmethodshydrothermaloxidation/

reductionhydrothermalsynthesishydrothermalhydrolysishydrothermalcrystallizationetc.10Part.2Part.1Part.3FundamentalsHydrothermalcrystallization:Dissolution-recrystallizationrawmaterialdissolution

ions/microclustertransportionhightemperature/pressureconvectionsupersaturated

solutionnucleationtargetcrystalgrowthPart3ExamplesofApplication12Part.3Part.1Part.2SupercapacitorACSAppliedMaterials&Interfaces,2013,5(21):11427-11433.13Part.3Part.1Part.2Supercapacitor14Part.3Part.1Part.2SupercapacitorAhighestcapacitanceof350F/gisobtainedforWS2/RGOhybridsatascanrateof2mV/s,whereasRGOandWS2sheetsshowacapacitanceof130and70F/g.Hence,thecapacitancevalueofWS2/RGOhybridsatascanrateof2mV/sisabout5and2.6timeshigherthanWS2andRGOsheets.15Part.3Part.1Part.2Supercapacitorself-assembledgraphenehydrogel(SGH)mechanicallystronghighspecificcapacitanceinherentbiocompatibility16Part.3Part.1Part.2SupercapacitorSynthesisaconvenientone-stephydrothermalmethodThetypicalSGHcanbeeasilypreparedbyheating2mg/mLofhomogeneousgrapheneoxide(GO)aqueousdispersionSealedinaTeflon-linedautoclaveat180℃for12hThreeSGHcolumnswithadiameteraround0.8cmeachcansupport100gweightwithlittledeformationmechanicallystrongProperties17Part.3Part.1Part.2Supercapacitorhighspecificcapacitance(b)cyclicvoltammogramsoftheSGH-basedsupercapacitorattwodifferentscanrates(c)galvanostaticcharge/dischargecurvesoftheSGH-basedsupercapacitorataconstantcurrentof1A/g18Part.3Part.1Part.2LithiumIonBatteriesNovelthree-dimensionalflower-likeporousAl2O3nanosheetsanchoringhollowNiOnanoparticlesforhigh-efficiencylithiumionbatteriesAunique3Dflower-likeporousAl2O3nanosheetsanchoringhollowNiOnanoparticles(FH-NiO@Al2O3)aredesignedandpreparedviaacontrollablehydrothermalmethod.TheFH-NiO@Al2O3demonstratessuperiorLi-storageperformances(1217mAh/gat500mA/g,97%retentionafter300cycles)JournalofMaterialsChemistryA,2016,4(29):11507-11515.19Part.3Part.1Part.2LithiumIonBatteries10mlEG5ml2MNi(NO3)22ml2MAl2(NO3)37ml1MNa2CO315mlNH3·H2Ostir20minsolutionFlower-likeNi2Al(CO3)2(OH)3nanoplates

50mLTeon-linedstainless-steelautoclave180℃,18hwash,dry750℃,200minH2350℃,300minO2Flower-likeNiO@Al2O36wt%NH3·H2O2hwash,dryFH-NiO@Al2O3Electrochemicaltesting:FH-NiO@Al2O3:CB:PVDF=8:1:1Electrolyte:1MLiPF6(EC/DEC=1:1)Voltagerange:0.01-3VCountereclertrode:LifoilSeparator:polypropylenemicroporousfilmTheoreticalcapacity:717mAh/g20Part.3Part.1Part.2LithiumIonBatteries①Numerousnanoparticlesareuniformlyconfinedandanchoredtothinnanosheets.②itshowsaspecificsurfaceareaof215.058m2/g.③itshowsremarkablerateperformanceandcyclicstability.21Part.3Part.1Part.2LithiumIonBatteriesHigh-ratelayeredlithium-richcathodenanomaterialsforlithium-ionbatteriessynthesizedwiththeassistofcarbonspherestemplatesJournalofPowerSources,2016,331:247-257.22Part.3Part.1Part.2LithiumIonBatteriesSEMimagesofcarbonspheresobtainedfromvariousconcentrationsofglucosesolution:(a)0.1M;(b)0.2M;(c)0.3M;(d)0.4M;(e)0.5M;and(f)0.6M.23Part.3Part.1Part.2LithiumIonBatteries0%Cs5%Cs10%Cs15%Cs24Part.3Part.1Part.2LithiumIonBatteries25Part.3Part.1Part.2LithiumIonBatteriesSolvothermalsynthesizedLiMn1?xFexPO4@Cnanopowderswithexcellenthighrateandlowtemperatureperformancesforlithium-ionbatteriesRSCAdvances,2016,6(57):52271-52278.EG:ethyleneglycol26Part.3Part.1Part.2LithiumIonBatteriesWiththedecreaseofMn/Feratio(Fig.4b-d),thenanosheetsgraduallychangeintoshortnanorodswithasizeof30-50nmindiameterand100-150nminlength.27Part.3Part.1Part.2LithiumIonBatteries28Part.3Part.1Part.2LithiumIonBatteriesAfter100cycles,D8-LiFePO4retainaspecificdischargecapacityof153mAh/g(99.2%)20Cretainaspecificdischargecapacityof140.2mAh/g29Part.3Part.1Part.2SolarBatteriesJournaloftheAmericanChemicalSociety,2014,136(43):15310-15318.30Part.3Part.1Part.2SolarBatteriesSynthesis31Part.3Part.1Part.2SolarBatterieshydrolysisoftitaniumalkoxidepolycondensationofhydroxyalkoxides

32Part.3Part.1Pa

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