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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
