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1、物理化學(xué)學(xué)~(WuliHuaxueXuebao)DecemberActa尸.-Chim.Sin.2013,29(12),2661-26662661[Article]doi:10.3866/PKU.WHXB20l3l0151www.whxb.pku.edu.cn六"r--氣氣氛,于下l’熔鹽法合成JB-FeSe楊承旭’鞠晶趙世迪徐航宇’劉孟。廖復(fù)輝’李國寶林建華(北京大學(xué)化學(xué)與分子工程學(xué)院,北京分子科學(xué)國家實驗室,稀土材料化學(xué)及應(yīng)用國家重點實驗室,北京100871北京匯文中學(xué),北京100061;溫州大學(xué)化學(xué)與材料學(xué)院,浙江溫州325027)摘要:使用傳統(tǒng)方法制備一FeS
2、e鐵基超導(dǎo)體需要隔絕空氣的真空條件,反應(yīng)溫度通常超過800。C.本文采用LiCI/NaCI/KCl熔鹽法在空氣條件下得到口一FeSe鐵基超導(dǎo)體.制備過程簡單,不需要在真空條件下封管處理,熔鹽的使用有效降低了反應(yīng)溫度,并阻止反應(yīng)物和產(chǎn)物在空氣中氧化.粉末X射線衍射和Rietveld分析結(jié)果表明產(chǎn)物純度較高.電性和磁性測試表N/3一FeSe在8K附近有超導(dǎo)性出現(xiàn).關(guān)鍵詞:口一FeSe;鐵基超導(dǎo)體;熔鹽法:空氣條件:X射線衍射中圖分類號:0646;O611.4SynthesisofJB-FeSebySalt-FluxMethodunderAirAtmosphereYANGC
3、heng.XuJUJinflZHAOShi.D-2XUHang.Yu’LlUMeng。LIAOFu.Hui’LlGuo.Bao’,LlNJian—Hua’,eStateKeyLaboratoryofRareEarthMaterialsChemistryandApplieations.BeijingNationalLaboratoryforMolecularSeiences(BNLMS),CollegeofChemistryandMolecularEngineering,PekingUniversity,Beijing100871,PR.China;2BeijingHu
4、iwenMiddleSchoolBeij'ingJ00061,PR.China;CollegeofChemistryandMaterialScience,WenzhouUniversity,Wenzhou325027,ZhejiangProvince,PR.China)Abstract:/3-FeSeistypicallypreparedundervacuumathightemperaturesexceeding800。C.HerewedevelopanewLiCI/NaelKCIfluxmethodtosuccessfullysynthesize8一FeSeunde
5、rairatmosphere.Thesyntheticprocedureissimpleandwithoutevacuationpretreatment.ThefluxefectivelydecreasesthesynthetictemperatureandprotectsthereactantsandproductsfrOmair.X-raydifractiondataandRietveldanalysisshowthattheproducthashighpurity.MagneticandelectricaImeasurementsconfirmthatallsa
6、mplesobtainedshowsuperconductivitybelow8K.KeyWords:盧一FeSe;Iron-basedsuperc0nduct0r:Salt-fluxmethod;AiratmosphereX-raydifraction1Intr0ductjoncanbeusedasastartingcompoundtoreactwithalkalimetals,Recently,一FeSe(tetragonalFeSe~一)isfoundtobeasuper—alkalineearthmetals,Yb,andEutoformsuperconduc
7、torconductorwithatransitiontemperature8Katnormalpres—AxFe2Se2(A=Li,Na,Ba,Sr,Ca,Yb,Eu)with一30to46K,sureandZ37Katpressuresofp~9GPa,Inaddition,一FeSeortoreactwithLiandNH3toformsupercOnductorsReceived:Junel8,2013;Revised:October14,2013;PublishedonWeb:Octoberl5,20l3.Correspondingauth