拓扑绝缘体Bi2Se3的合成与表征

摘要Bi2Se3是一种典型的拓扑绝缘体，其具有独特的电子结构，可在多个前沿领域展现重要的应用潜力，其性能高度依赖于材料的微观结构，实现Bi2Se3纳米材料的可控合成是推动其实际应用的关键，但其纳米片结构的合成难以实现大面积的均匀生长和形貌控制。因此，探寻一种稳定高效的合成条件是十分重要的研究方向。本文采用一锅合成法，将Na2SeO3和Bi(NO3)3·5H2O的乙二醇溶液和添加适量PVP(聚乙烯吡咯烷酮)和AA(L-抗坏血酸)的乙二醇溶液混合反应，成功制备出拓扑绝缘体Bi2Se3。同时通过控制反应时间探究Bi2Se3六边形片状纳米结构的形成和演变过程。反应时间从20min至80min，以及120min时的反应产物进行观察。最终得到了结论：反应进行20min时形成纳米片和纳米棒；进行30min时Bi2Se3晶体初步形成六边形轮廓；进行至40min时已经有大部分晶体形成了完整六边形结构；反应进行至70min时，Bi2Se3的六边形片状纳米结构已经完全形成，再增加反应时间则可以略微提高规整六边形结构产物的占比。这个结论揭示了Bi2Se3纳米材料的生长规律，探明了反应参数与产物形貌之间的内在联系，可以为拓扑绝缘体Bi2Se3的可控合成提供理论依据，可以通过调节反应的温度梯度提高制备效率，满足众多领域的研究生产需求。关键词：拓扑绝缘体；硒化铋；一锅合成法；纳米合成

ABSTRACTBi2Se3isatypicaltopologicalinsulatorwithauniqueelectronicstructure,showingimportantapplicationpotentialinmultiplefrontierfields.Itsperformancehighlydependsonthemicrostructureofthematerial.AchievingthecontrollablesynthesisofBi2Se3nanomaterialsiscrucialtopromotetheirpracticalapplications.However,thesynthesisofnanosheetstructuresisdifficulttoachievelarge-areauniformgrowthandmorphologycontrol.Therefore,exploringstableandefficientsynthesisconditionsisaveryimportantresearchdirection.Inthispaper,aone-potsynthesismethodwasusedtomixandreactanethyleneglycolsolutionofNa2SeO3andBi(NO3)3·5H2OwithanethyleneglycolsolutioncontainingappropriateamountsofPVP(polyvinylpyrrolidone)andAA(L-ascorbicacid),successfullypreparingthetopologicalinsulatorBi2Se3.Atthesametime,theformationandevolutionprocessofhexagonalsheet-likenanostructuresofBi2Se3wereinvestigatedbycontrollingthereactiontime.Thereactionproductswereobservedatreactiontimesfrom20minto80min,aswellasat120min.Thefinalconclusionsareasfollows:nanosheetsandnanorodsformedat20minofreaction;Bi2Se3crystalsinitiallyformedhexagonaloutlinesat30min;mostcrystalsformedcompletehexagonalstructuresby40min;thehexagonalsheet-likenanostructuresofBi2Se3werecompletelyformedat70min,andincreasingthereactiontimefurthercouldslightlyincreasetheproportionofproductswithregularhexagonalstructures.ThisconclusionrevealsthegrowthlawofBi2Se3nanomaterials,clarifiestheinternalrelationshipbetweenreactionparametersandproductmorphology,andcanprovideatheoreticalbasisforthecontrollablesynthesisoftopologicalinsulatorBi2Se3.Thepreparationefficiencycanbeimprovedbyadjustingthetemperaturegradientofthereactiontomeettheresearchandproductionneedsofmanyfields.Keywords：TopologicalInsulator；Bi2Se3；One-potSynthesisMethod；Nanosynthesis

目录第1章文献综述 11.1引言 11.2拓扑绝缘体Bi2Se3的基本性质 11.2.1晶体结构与化学组成 11.2.2表面态与拓扑特性 21.3拓扑绝缘体Bi2Se3的合成机制 21.4拓扑绝缘体Bi2Se3的拓展应用 31.4.1Bi2Se3应用方向 31.4.2Bi2Se3未来展望 4第2章实验部分 52.1实验原料与设备 52.2实验过程 62.2.1拓扑绝缘体Bi2Se3的合成与表征 62.2.2拓扑绝缘体Bi2Se3的测试 7第3章实验结果与分析 73.1拓扑绝缘体Bi2Se3的形貌 73.2拓扑绝缘体Bi2Se3产物SEM图像分析 8结论 12参考文献 13第1章文献综述1.1引言拓扑绝缘体Bi2Se3的独特性质使其成为了材料科学研究的热门方向，不仅光电子、电子器件等领域高度关注其前沿发展，其在量子计算领域也有巨大应用潜力ADDINZOTERO_ITEMCSL_CITATION{"citationID":"gtRaVYFC","properties":{"formattedCitation":"\\super[1]\\nosupersub{}","plainCitation":"[1]","noteIndex":0},"citationItems":[{"id":174,"uris":["/users/local/lqtbcmXZ/items/X7N82YRL"],"itemData":{"id":174,"type":"document","title":"拓扑绝缘体Bi_2Se_3单晶体的研究进展"}}],"schema":"/citation-style-language/schema/raw/master/csl-citation.json"}[1]。随着相关研究的不断深入以及技术转化进程的加速，对拓扑绝缘体Bi2Se3的合成制备需求呈现出爆发式增长。从基础科学研究中对高质量样品的需求，到工程化应用阶段对材料量产的要求，传统合成方法在效率、成本、稳定性等方面的局限性逐渐凸显。现有合成技术，如分子束外延法虽然能够实现原子级精度的薄膜生长ADDINZOTERO_ITEMCSL_CITATION{"citationID":"JQQv6Rpx","properties":{"formattedCitation":"\\super[2]\\nosupersub{}","plainCitation":"[2]","noteIndex":0},"citationItems":[{"id":209,"uris":["/users/local/lqtbcmXZ/items/NC223B47"],"itemData":{"id":209,"type":"article-journal","container-title":"合肥工业大学学报（自然科学版）","issue":"1","note":"publisher:合肥工业大学","page":"60-63","title":"掺Mn拓扑绝缘体Bi2Se3薄膜的制备及其电磁特性研究","volume":"41","author":[{"literal":"杜洪洋"},{"literal":"徐伟"},{"literal":"宋玲玲"},{"literal":"仇怀利"},{"literal":"李中军"},{"literal":"黄荣俊"}],"issued":{"date-parts":[["2018",1]]}}}],"schema":"/citation-style-language/schema/raw/master/csl-citation.json"}[2]，但设备昂贵、操作复杂且生长速率缓慢；化学气相沉积法虽可制备大面积样品，但工艺参数调控严苛，产物质量参差不齐ADDINZOTERO_ITEMCSL_CITATION{"citationID":"kY9DQCS3","properties":{"formattedCitation":"\\super[3]\\nosupersub{}","plainCitation":"[3]","noteIndex":0},"citationItems":[{"id":197,"uris":["/users/local/lqtbcmXZ/items/ENV3JPNV"],"itemData":{"id":197,"type":"article-journal","abstract":"Topologicalinsulator(TI),apromisingquantumandsemiconductormaterial,hasgaplesssurfacestateandnarrowbulkbandgap.Firstly,theproperties,classificationsandcompoundsofTIareintroduced.Secondly,thepreparationanddopingofTIareassessed.Someresultsarelisted.(1)AlthoughvariouspreparationmethodsareusedtoimprovethecrystalqualityoftheTI,itcannotreachtheindustrialization.Fermilevelregulationstillfaceschallenges;(2)ThecarriertypeandlatticeofTIareaffectedbynon-magneticimpurities.Themostpromisingpropertyisthesuperconductivityatlowtemperature;(3)Magneticimpuritiescandestroythetime-reversalsymmetryoftheTIsurface,whichopensthebandgapontheTIsurfaceresultinginsomenovelphysicaleffectssuchasquantumanomalousHalleffect(QAHE).Thirdly,thispapersummarizesvariousapplicationsofTIincludingphotodetector,magneticdevice,field-effecttransistor(FET),laser,andsoon.Furthermore,manyoftheirparametersarecomparedbasedonTIandsomecommonmaterials.ItisfoundthatTI-baseddevicesexhibitexcellentperformance,butsomeparameterssuchassignaltonoiseratio(S/N)arestilllowerthanothermaterials.Finally,itsadvantages,challengesandfutureprospectsarediscussed.Overall,thispaperprovidesanopportunitytoimprovecrystalquality,dopingregulationandapplicationofTI.","container-title":"Materials","DOI":"10.3390/ma10070814","ISSN":"1996-1944","issue":"7","journalAbbreviation":"Materials","language":"en","license":"/licenses/by/4.0/","page":"814","source":"DOI.org(Crossref)","title":"TheProperty,PreparationandApplicationofTopologicalInsulators:AReview","title-short":"TheProperty,PreparationandApplicationofTopologicalInsulators","volume":"10","author":[{"family":"Tian","given":"Wenchao"},{"family":"Yu","given":"Wenbo"},{"family":"Shi","given":"Jing"},{"family":"Wang","given":"Yongkun"}],"issued":{"date-parts":[["2017",7,17]]}}}],"schema":"/citation-style-language/schema/raw/master/csl-citation.json"}[3]。鉴于拓扑绝缘体Bi2Se3的巨大应用价值，对其的合成制备也将产生不小的需求，为了后续的应用拓展，迫切需要一种简洁快速、稳定有效的合成方法以满足拓扑绝缘体Bi2Se3的研究应用需求。目前的拓扑绝缘体Bi2Se3制备方法普遍采用如水热共还原法ADDINZOTERO_ITEMCSL_CITATION{"citationID":"6WaqiBLa","properties":{"formattedCitation":"\\super[4]\\nosupersub{}","plainCitation":"[4]","noteIndex":0},"citationItems":[{"id":187,"uris":["/users/local/lqtbcmXZ/items/4WYD332E"],"itemData":{"id":187,"type":"article-journal","abstract":"WereportanenvironmentallyfriendlyhydrothermalapproachtothesynthesisofBi\n2\nSe\n3\nnanosheetsbyusinggallicacidasareductantinacontrollablemanner.\n\n,\n\nInthiswork,asimpleandreproduciblehydrothermalsynthesiswasemployedtosynthesizetwo-dimensionalBi\n2\nSe\n3\nnanosheetsbyusinggallicacidasareductant.Meanwhile,theeffectsoftheamountsofgallicacidandsodiumhydroxideandthesurfactantTritonX-100onphasecompositionandmorphologyoftheobtainedBi\n2\nSe\n3\nwerealsostudied.TheresultsrevealthatgallicacidcouldeffectivelyreduceSe\n4+\ntoSe\n2−\nandgaverisetotheformationofBi\n2\nSe\n3\n.Additionally,keepingthereactionconditionsofmolarratioofgallicacidtotheprecursorelements(Bi+Se)at1to1(orhigher)andusingstrongalkalinesolutionswerethekeyfactorstosynthesizehighpuritycrystallineBi\n2\nSe\n3\nnanosheets.Furthermore,flower-likeBi\n2\nSe\n3\ncomposedofnanosheetswithadozennanometerthicknesscouldbeeasilyfabricatedbyaddingappropriateamountsofTritonX-100.Thisworkprovidesanovelapproachforsynthesisofultra-thinBi\n2\nSe\n3\nnanosheetsinacontrollablemanner.","container-title":"RSCAdvances","DOI":"10.1039/D2RA01129H","ISSN":"2046-2069","issue":"24","journalAbbreviation":"RSCAdv.","language":"en","page":"15150-15157","source":"DOI.org(Crossref)","title":"HydrothermalsynthesisofBi₂Se₃nanosheetsbyusinggallicacidasareductant","volume":"12","author":[{"family":"Huo","given":"Di"},{"family":"Lin","given":"Gongge"},{"family":"Lv","given":"Mengfan"}],"issued":{"date-parts":[["2022"]]}}}],"schema":"/citation-style-language/schema/raw/master/csl-citation.json"}[4]、溶剂热法ADDINZOTERO_ITEMCSL_CITATION{"citationID":"uE6cK3eT","properties":{"formattedCitation":"\\super[3,5]\\nosupersub{}","plainCitation":"[3,5]","noteIndex":0},"citationItems":[{"id":197,"uris":["/users/local/lqtbcmXZ/items/ENV3JPNV"],"itemData":{"id":197,"type":"article-journal","abstract":"Topologicalinsulator(TI),apromisingquantumandsemiconductormaterial,hasgaplesssurfacestateandnarrowbulkbandgap.Firstly,theproperties,classificationsandcompoundsofTIareintroduced.Secondly,thepreparationanddopingofTIareassessed.Someresultsarelisted.(1)AlthoughvariouspreparationmethodsareusedtoimprovethecrystalqualityoftheTI,itcannotreachtheindustrialization.Fermilevelregulationstillfaceschallenges;(2)ThecarriertypeandlatticeofTIareaffectedbynon-magneticimpurities.Themostpromisingpropertyisthesuperconductivityatlowtemperature;(3)Magneticimpuritiescandestroythetime-reversalsymmetryoftheTIsurface,whichopensthebandgapontheTIsurfaceresultinginsomenovelphysicaleffectssuchasquantumanomalousHalleffect(QAHE).Thirdly,thispapersummarizesvariousapplicationsofTIincludingphotodetector,magneticdevice,field-effecttransistor(FET),laser,andsoon.Furthermore,manyoftheirparametersarecomparedbasedonTIandsomecommonmaterials.ItisfoundthatTI-baseddevicesexhibitexcellentperformance,butsomeparameterssuchassignaltonoiseratio(S/N)arestilllowerthanothermaterials.Finally,itsadvantages,challengesandfutureprospectsarediscussed.Overall,thispaperprovidesanopportunitytoimprovecrystalquality,dopingregulationandapplicationofTI.","container-title":"Materials","DOI":"10.3390/ma10070814","ISSN":"1996-1944","issue":"7","journalAbbreviation":"Materials","language":"en","license":"/licenses/by/4.0/","page":"814","source":"DOI.org(Crossref)","title":"TheProperty,PreparationandApplicationofTopologicalInsulators:AReview","title-short":"TheProperty,PreparationandApplicationofTopologicalInsulators","volume":"10","author":[{"family":"Tian","given":"Wenchao"},{"family":"Yu","given":"Wenbo"},{"family":"Shi","given":"Jing"},{"family":"Wang","given":"Yongkun"}],"issued":{"date-parts":[["2017",7,17]]}},"label":"page"},{"id":173,"uris":["/users/local/lqtbcmXZ/items/KHAL6PEF"],"itemData":{"id":173,"type":"document","title":"三硒化二铋微_纳米晶的可控合成"},"label":"page"}],"schema":"/citation-style-language/schema/raw/master/csl-citation.json"}[3,5]等合成方法，而本文实验采用一锅溶剂热法合成，具有操作简洁、反应高效和产率高等优点，我们将Na2SeO3和Bi(NO3)3·5H2O的乙二醇溶液和适量PVP和AA的乙二醇溶液混合反应合成拓扑绝缘体Bi2Se3，并且探讨反应时间对产物的形貌影响。1.2拓扑绝缘体Bi2Se3的基本性质1.2.1晶体结构与化学组成Bi2Se3的晶体结构为菱面体结构（R3m空间群），其化学组成由铋（Bi）和硒（Se）两种元素组成。该材料具备五层按周期性重复的单元，称为五重层（Quintuplelayer），每个单元包含两个硒原子层（Se1和Se2）和两个铋原子层（Bi），以及一个第三层硒原子（Se2）ADDINZOTERO_ITEMCSL_CITATION{"citationID":"GoiBFGNt","properties":{"formattedCitation":"\\super[6]\\nosupersub{}","plainCitation":"[6]","noteIndex":0},"citationItems":[{"id":199,"uris":["/users/local/lqtbcmXZ/items/JPTHU9XS"],"itemData":{"id":199,"type":"article-journal","container-title":"iScience","DOI":"10.1016/j.isci.2021.103291","ISSN":"25890042","issue":"11","journalAbbreviation":"iScience","language":"en","page":"103291","source":"DOI.org(Crossref)","title":"2DBi2Se3materialsforoptoelectronics","volume":"24","author":[{"family":"Wang","given":"FakunK."},{"family":"Yang","given":"SijieJ."},{"family":"Zhai","given":"TianyouY."}],"issued":{"date-parts":[["2021",11]]}}}],"schema":"/citation-style-language/schema/raw/master/csl-citation.json"}[6]。这些原子层借助弱范德华力相互作用，呈垂直堆叠状态，形成了层叠结构ADDINZOTERO_ITEMCSL_CITATION{"citationID":"98TYwuyi","properties":{"formattedCitation":"\\super[1]\\nosupersub{}","plainCitation":"[1]","noteIndex":0},"citationItems":[{"id":174,"uris":["/users/local/lqtbcmXZ/items/X7N82YRL"],"itemData":{"id":174,"type":"document","title":"拓扑绝缘体Bi_2Se_3单晶体的研究进展"}}],"schema":"/citation-style-language/schema/raw/master/csl-citation.json"}[1]。在晶体中，Bi原子坐落于六边形环的中心，而Se原子分布在环的顶点、边缘位置ADDINZOTERO_ITEMCSL_CITATION{"citationID":"O9BNmMC9","properties":{"formattedCitation":"\\super[1]\\nosupersub{}","plainCitation":"[1]","noteIndex":0},"citationItems":[{"id":174,"uris":["/users/local/lqtbcmXZ/items/X7N82YRL"],"itemData":{"id":174,"type":"document","title":"拓扑绝缘体Bi_2Se_3单晶体的研究进展"}}],"schema":"/citation-style-language/schema/raw/master/csl-citation.json"}[1]。该排列方式使Bi2Se3具备独特的电子特性，例如拓扑绝缘体展现的特性ADDINZOTERO_ITEMCSL_CITATION{"citationID":"pouIcJVS","properties":{"formattedCitation":"\\super[7]\\nosupersub{}","plainCitation":"[7]","noteIndex":0},"citationItems":[{"id":204,"uris":["/users/local/lqtbcmXZ/items/SSEDP6IE"],"itemData":{"id":204,"type":"article-journal","abstract":"Bi2Se3,Bi2Te3andSb2Te3compoundsarerecentlypredictedtobe3-dimentional(3D)strongtopologicalinsulators.Inthispaper,basedonab-initiocalculations,westudyindetailthetopologicalnatureandthesurfacestatesofthisfamilycompounds.Thepenetrationdepthandthespin-resolvedFermisurfacesofthesurfacestateswillbeanalyzed.Wewillalsopresentanprocedure,fromwhichhighlyaccurateeffectiveHamiltoniancanbeconstructed,basedonprojectedatomicWannierfunctions(whichkeepthesymmetriesofthesystems).SuchHamiltoniancanbeusedtostudythesemi-infinitesystemsorslabtypesupercellsefficiently.Finally,wediscussthe3DtopologicalphasetransitioninSb2(Te1-xSex)3alloysystem.","container-title":"NewJournalofPhysics","DOI":"10.1088/1367-2630/12/6/065013","ISSN":"1367-2630","issue":"6","journalAbbreviation":"NewJ.Phys.","language":"en","note":"arXiv:1003.5082[cond-mat]","page":"065013","source":"arX","title":"FirstPrinciplesStudieson3-DimentionalStrongTopologicalInsulators:Bi2Te3,Bi2Se3andSb2Te3","title-short":"FirstPrinciplesStudieson3-DimentionalStrongTopologicalInsulators","volume":"12","author":[{"family":"Zhang","given":"Wei"},{"family":"Yu","given":"Rui"},{"family":"Zhang","given":"Hai-Jun"},{"family":"Dai","given":"Xi"},{"family":"Fang","given":"Zhong"}],"issued":{"date-parts":[["2010",6,17]]}}}],"schema":"/citation-style-language/schema/raw/master/csl-citation.json"}[7]，Bi2Se3的晶体结构还可借助六方晶胞或三棱柱原胞来描述，进一步呈现其几何特点ADDINZOTERO_ITEMCSL_CITATION{"citationID":"JcQdqao1","properties":{"formattedCitation":"\\super[7]\\nosupersub{}","plainCitation":"[7]","noteIndex":0},"citationItems":[{"id":204,"uris":["/users/local/lqtbcmXZ/items/SSEDP6IE"],"itemData":{"id":204,"type":"article-journal","abstract":"Bi2Se3,Bi2Te3andSb2Te3compoundsarerecentlypredictedtobe3-dimentional(3D)strongtopologicalinsulators.Inthispaper,basedonab-initiocalculations,westudyindetailthetopologicalnatureandthesurfacestatesofthisfamilycompounds.Thepenetrationdepthandthespin-resolvedFermisurfacesofthesurfacestateswillbeanalyzed.Wewillalsopresentanprocedure,fromwhichhighlyaccurateeffectiveHamiltoniancanbeconstructed,basedonprojectedatomicWannierfunctions(whichkeepthesymmetriesofthesystems).SuchHamiltoniancanbeusedtostudythesemi-infinitesystemsorslabtypesupercellsefficiently.Finally,wediscussthe3DtopologicalphasetransitioninSb2(Te1-xSex)3alloysystem.","container-title":"NewJournalofPhysics","DOI":"10.1088/1367-2630/12/6/065013","ISSN":"1367-2630","issue":"6","journalAbbreviation":"NewJ.Phys.","language":"en","note":"arXiv:1003.5082[cond-mat]","page":"065013","source":"arX","title":"FirstPrinciplesStudieson3-DimentionalStrongTopologicalInsulators:Bi2Te3,Bi2Se3andSb2Te3","title-short":"FirstPrinciplesStudieson3-DimentionalStrongTopologicalInsulators","volume":"12","author":[{"family":"Zhang","given":"Wei"},{"family":"Yu","given":"Rui"},{"family":"Zhang","given":"Hai-Jun"},{"family":"Dai","given":"Xi"},{"family":"Fang","given":"Zhong"}],"issued":{"date-parts":[["2010",6,17]]}}}],"schema":"/citation-style-language/schema/raw/master/csl-citation.json"}[7]。1.2.2表面态与拓扑特性Bi2Se3是一种典型的三维拓扑绝缘体，其表面态呈现出独特的狄拉克锥结构，表现出显著的拓扑特性。这些表面态由时间反演对称性保护，能够实现电子和空穴的分离，并且在费米能级附近与体态保持远距离分离ADDINZOTERO_ITEMCSL_CITATION{"citationID":"LHBD4TbF","properties":{"formattedCitation":"\\super[3]\\nosupersub{}","plainCitation":"[3]","noteIndex":0},"citationItems":[{"id":197,"uris":["/users/local/lqtbcmXZ/items/ENV3JPNV"],"itemData":{"id":197,"type":"article-journal","abstract":"Topologicalinsulator(TI),apromisingquantumandsemiconductormaterial,hasgaplesssurfacestateandnarrowbulkbandgap.Firstly,theproperties,classificationsandcompoundsofTIareintroduced.Secondly,thepreparationanddopingofTIareassessed.Someresultsarelisted.(1)AlthoughvariouspreparationmethodsareusedtoimprovethecrystalqualityoftheTI,itcannotreachtheindustrialization.Fermilevelregulationstillfaceschallenges;(2)ThecarriertypeandlatticeofTIareaffectedbynon-magneticimpurities.Themostpromisingpropertyisthesuperconductivityatlowtemperature;(3)Magneticimpuritiescandestroythetime-reversalsymmetryoftheTIsurface,whichopensthebandgapontheTIsurfaceresultinginsomenovelphysicaleffectssuchasquantumanomalousHalleffect(QAHE).Thirdly,thispapersummarizesvariousapplicationsofTIincludingphotodetector,magneticdevice,field-effecttransistor(FET),laser,andsoon.Furthermore,manyoftheirparametersarecomparedbasedonTIandsomecommonmaterials.ItisfoundthatTI-baseddevicesexhibitexcellentperformance,butsomeparameterssuchassignaltonoiseratio(S/N)arestilllowerthanothermaterials.Finally,itsadvantages,challengesandfutureprospectsarediscussed.Overall,thispaperprovidesanopportunitytoimprovecrystalquality,dopingregulationandapplicationofTI.","container-title":"Materials","DOI":"10.3390/ma10070814","ISSN":"1996-1944","issue":"7","journalAbbreviation":"Materials","language":"en","license":"/licenses/by/4.0/","page":"814","source":"DOI.org(Crossref)","title":"TheProperty,PreparationandApplicationofTopologicalInsulators:AReview","title-short":"TheProperty,PreparationandApplicationofTopologicalInsulators","volume":"10","author":[{"family":"Tian","given":"Wenchao"},{"family":"Yu","given":"Wenbo"},{"family":"Shi","given":"Jing"},{"family":"Wang","g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