溶胶凝胶法结合电纺技术合成纳米结构纤维及其电化学性质研究
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摘要
本论文主要讨论溶胶凝胶结合电纺技术合成纳米结构纤维,并测试其作为锂离子电池正极材料的电化学性质。
第一章主要分三部分,分别介绍了溶胶凝胶化学、电纺技术和锂离子电池。第一部分主要介绍了溶胶凝胶-电纺的基本原理,通过描述其基本过程揭示最终产物的影响因素,并简单介绍了溶胶凝胶-电纺技术的国内外概况;第二部分主要介绍了锂离子电池对正极材料的要求,并详细介绍了锂离子电池正极材料的发展,以及纳米结构纤维材料作为正极材料的优势。第三节说明了本文的选题思路及研究目的。
第二章主要介绍了核壳结构Li(Ni_(1/3)Co_(1/3)Mn_(1/3))O_2/Li(Ni_(1/2)Mn_(1/2))O_2纳米纤维的合成、表征及其作为锂离子电池正极材料的电化学性质表征。本实验采用醋酸盐为原料提供锂离子及过渡金属离子(钴、镍、锰),以柠檬酸为螯合剂,去离子水为溶剂通过溶胶凝胶法合成可纺性溶胶,对溶胶进行同轴电纺得到核壳结构纳米纤维,将纤维干燥后在不同温度下对其进行烧结,在700℃得到最终晶化产物:核壳结构Li(Ni_(1/3)Co_(1/3)Mn_(1/3))O_2/Li(Ni_(1/2)Mn_(1/2))O_2纳米纤维。我们对样品进行了TG、IR、XRD、TEM、SEM等基本表征,以确定样品的烧结过程中组分和结构的演化,以及样品的晶化程度和形貌变化。并将核壳结构纳米纤维Li(Ni_(1/3)Co_(1/3)Mn_(1/3))O_2/Li(Ni_(1/2)Mn_(1/2))O_2作为锂离子电池正极材料,通过组装锂离子电池,测试了电池的充放电性能和循环性能。
第三章主要介绍了中空纳米结构Li(Ni_(0.8)Co_(0.2))O_2纤维的合成、表征及其作为锂离子电池正极材料的电化学性质表征。同样以醋酸盐提供金属离子,柠檬酸为螯合剂,PVP为添加剂,去离子水为溶剂通过溶胶凝胶过程合成可纺性溶胶,再通过单管电纺过程得到纤维结构,经过烧结后得到最终产物:中空纳米结构Li(Ni_(0.8)Co_(0.2))O_2纤维。对样品进行了TG、IR、XRD、TEM及SEM等基本表征,以确定样品的烧结过程中组分和结构的演化,以及样品的晶化程度和形貌变化。并将中空纳米结构Li(Ni_(0.8)Co_(0.2))O_2纤维作为锂离子电池正极材料,通过组装锂离子电池,测试电池的充放电性能和循环性能。
第四章主要介绍了纳米结构LiFePO_4纤维的制备、基本表征其作为锂离子电池正极材料的电化学性质表征。本实验以二价铁源为原料,以醋酸锂提供锂离子、以柠檬酸为螯合剂、去离子水为溶剂,在70℃水浴中形成可纺性溶胶;通过电纺过程形成纳米结构纤维。再于惰气下进行烧结,最终形成纳米结构LiFePO_4纤维。我们对样品进行了TG、IR、XRD、TEM及SEM等基本表征,以确定样品烧结过程中组分和结构的演化,以及样品的晶化程度和形貌变化。并将纳米结构LiFePO_4纤维作为锂离子电池正极材料,通过组装锂离子电池,测试电池的充放电性能和循环性能。
The nanostructured fibers were synthesized by a sol-gel process combined with electrospinning technique.The contents include the preparation of the fibers and the investigation of electrochemical performance as cathode materials for lithium ion batteries.
In chapter one,we introduced three contents:the sol-gel process,the technique of electrospining,lithium-ion batteries.The first part,include the phylogeny,character, principle,process of the sol-gel process,and the influence of the processing parameters on every step.In the second part,we introduced the phylogeny,principle and procedures of the electrospinning,especially in the modification of collector and spinneret and the main factors effecting on the structure and shape of the fiber.In the third part,we introduced the phylogeny,principle and composing of lithium-ion batteries,especially in the development of cathode materials of lithium-ion batteries. In the end,we also described why and how chose this thesis.
In chapter two,the nanostructured Li(Ni_(1/3)Co_(1/3)Mn_(1/3))O_2/Li(Ni_(1/2)Mn_(1/2))O_2 fibers were prepared by electrospinning combined with the sol-gel method.Using metal acetate as starting materials,citric acid as chelating agent to synthesize sol; electrospinning the sol to gain fiber structure,sinter the fiber to gain the final production:core-shell Li(Ni_(1/3)Co_(1/3)Mn_(1/3))O_2/Li(Ni_(1/2)Mn_(1/2))O_2 nanostructured fiber. Characterize the final fiber with TG,IR,XRD,TEM,SEM ect.and testing it's electrochemical characteration as cathode material of lithium ion battery.
In chapter three,the nanostructured Li(Ni_(0.8)Co_(0.2))O_2 fibers were prepared by electrospinning combined with the sol-gel method.Using metal acetate as starting materials,citric acid as chelating agent and PVP as additive to synthesize sol; electrospinning the sol to gain fiber structure,sinter the fiber to gain the final production:nanostructured Li(Ni_(0.8)Co_(0.2))O_2 fiber.As the additive increased the final morphology are different with each other.The same as chapter two,we characterize the final fiber with TG,IR,XRD,TEM,SEM ect.and testing it's electrochemical characteration as cathode material of lithium ion battery.
In chapter four,the nanostructured LiFePO_4 fibers were prepared by electrospinning combined with the sol-gel method.Using Fe(Ⅱ),lithium acetate, and citric acid as chelating agent to synthesize sol;electrospinning the sol to gain fiber structure,sinter the fiber in inert gas to gain the final production:LiFePO_4 nanostructured fiber.Characterized the final fiber with TG,IR,XRD,TEM,SEM ect. and testing it's electrochemical characteration as cathode material of lithium ion battery.
第一章主要分三部分,分别介绍了溶胶凝胶化学、电纺技术和锂离子电池。第一部分主要介绍了溶胶凝胶-电纺的基本原理,通过描述其基本过程揭示最终产物的影响因素,并简单介绍了溶胶凝胶-电纺技术的国内外概况;第二部分主要介绍了锂离子电池对正极材料的要求,并详细介绍了锂离子电池正极材料的发展,以及纳米结构纤维材料作为正极材料的优势。第三节说明了本文的选题思路及研究目的。
第二章主要介绍了核壳结构Li(Ni_(1/3)Co_(1/3)Mn_(1/3))O_2/Li(Ni_(1/2)Mn_(1/2))O_2纳米纤维的合成、表征及其作为锂离子电池正极材料的电化学性质表征。本实验采用醋酸盐为原料提供锂离子及过渡金属离子(钴、镍、锰),以柠檬酸为螯合剂,去离子水为溶剂通过溶胶凝胶法合成可纺性溶胶,对溶胶进行同轴电纺得到核壳结构纳米纤维,将纤维干燥后在不同温度下对其进行烧结,在700℃得到最终晶化产物:核壳结构Li(Ni_(1/3)Co_(1/3)Mn_(1/3))O_2/Li(Ni_(1/2)Mn_(1/2))O_2纳米纤维。我们对样品进行了TG、IR、XRD、TEM、SEM等基本表征,以确定样品的烧结过程中组分和结构的演化,以及样品的晶化程度和形貌变化。并将核壳结构纳米纤维Li(Ni_(1/3)Co_(1/3)Mn_(1/3))O_2/Li(Ni_(1/2)Mn_(1/2))O_2作为锂离子电池正极材料,通过组装锂离子电池,测试了电池的充放电性能和循环性能。
第三章主要介绍了中空纳米结构Li(Ni_(0.8)Co_(0.2))O_2纤维的合成、表征及其作为锂离子电池正极材料的电化学性质表征。同样以醋酸盐提供金属离子,柠檬酸为螯合剂,PVP为添加剂,去离子水为溶剂通过溶胶凝胶过程合成可纺性溶胶,再通过单管电纺过程得到纤维结构,经过烧结后得到最终产物:中空纳米结构Li(Ni_(0.8)Co_(0.2))O_2纤维。对样品进行了TG、IR、XRD、TEM及SEM等基本表征,以确定样品的烧结过程中组分和结构的演化,以及样品的晶化程度和形貌变化。并将中空纳米结构Li(Ni_(0.8)Co_(0.2))O_2纤维作为锂离子电池正极材料,通过组装锂离子电池,测试电池的充放电性能和循环性能。
第四章主要介绍了纳米结构LiFePO_4纤维的制备、基本表征其作为锂离子电池正极材料的电化学性质表征。本实验以二价铁源为原料,以醋酸锂提供锂离子、以柠檬酸为螯合剂、去离子水为溶剂,在70℃水浴中形成可纺性溶胶;通过电纺过程形成纳米结构纤维。再于惰气下进行烧结,最终形成纳米结构LiFePO_4纤维。我们对样品进行了TG、IR、XRD、TEM及SEM等基本表征,以确定样品烧结过程中组分和结构的演化,以及样品的晶化程度和形貌变化。并将纳米结构LiFePO_4纤维作为锂离子电池正极材料,通过组装锂离子电池,测试电池的充放电性能和循环性能。
The nanostructured fibers were synthesized by a sol-gel process combined with electrospinning technique.The contents include the preparation of the fibers and the investigation of electrochemical performance as cathode materials for lithium ion batteries.
In chapter one,we introduced three contents:the sol-gel process,the technique of electrospining,lithium-ion batteries.The first part,include the phylogeny,character, principle,process of the sol-gel process,and the influence of the processing parameters on every step.In the second part,we introduced the phylogeny,principle and procedures of the electrospinning,especially in the modification of collector and spinneret and the main factors effecting on the structure and shape of the fiber.In the third part,we introduced the phylogeny,principle and composing of lithium-ion batteries,especially in the development of cathode materials of lithium-ion batteries. In the end,we also described why and how chose this thesis.
In chapter two,the nanostructured Li(Ni_(1/3)Co_(1/3)Mn_(1/3))O_2/Li(Ni_(1/2)Mn_(1/2))O_2 fibers were prepared by electrospinning combined with the sol-gel method.Using metal acetate as starting materials,citric acid as chelating agent to synthesize sol; electrospinning the sol to gain fiber structure,sinter the fiber to gain the final production:core-shell Li(Ni_(1/3)Co_(1/3)Mn_(1/3))O_2/Li(Ni_(1/2)Mn_(1/2))O_2 nanostructured fiber. Characterize the final fiber with TG,IR,XRD,TEM,SEM ect.and testing it's electrochemical characteration as cathode material of lithium ion battery.
In chapter three,the nanostructured Li(Ni_(0.8)Co_(0.2))O_2 fibers were prepared by electrospinning combined with the sol-gel method.Using metal acetate as starting materials,citric acid as chelating agent and PVP as additive to synthesize sol; electrospinning the sol to gain fiber structure,sinter the fiber to gain the final production:nanostructured Li(Ni_(0.8)Co_(0.2))O_2 fiber.As the additive increased the final morphology are different with each other.The same as chapter two,we characterize the final fiber with TG,IR,XRD,TEM,SEM ect.and testing it's electrochemical characteration as cathode material of lithium ion battery.
In chapter four,the nanostructured LiFePO_4 fibers were prepared by electrospinning combined with the sol-gel method.Using Fe(Ⅱ),lithium acetate, and citric acid as chelating agent to synthesize sol;electrospinning the sol to gain fiber structure,sinter the fiber in inert gas to gain the final production:LiFePO_4 nanostructured fiber.Characterized the final fiber with TG,IR,XRD,TEM,SEM ect. and testing it's electrochemical characteration as cathode material of lithium ion battery.
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[1].(a)Kim,C.;Yang,K.S.Electrochemical properties of carbon nanofiber web as an electrode for supercapacitor prepared by electrospinning Appl.Phys.Lett.2003,83,1216-1218.;
(b)Choi,S.W.;Jo,S.M.;Lee,W.S.;Kim,Y.-R.An electrospun poly(vinylidene fluoride)nanofibrous membrane and its battery applications,Adv.Mater.2003,15,2027-2032.
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(b)Kobayashi,S.;Hamasaki,N.;Suzuki,M.;Kimura,M.;Shirai,H.;Hanabusa,K.Preparation of helical transition-metal oxide tubes using organogelators as structure-directing agents,J.Am.Chem.Soc.2002,124,6550-6551.
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(b)McCann,J.T.;Li,D.;Xia,Y.Electrospinning of nanofibers with core-sheath,hollow,or porous structures,J..Mater.Chem.2005,15,735-738.
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[7].C.Ramana,K.Zaghib,C.Julien,Highly Oriented Growed of Pulsed-Laser Deposited LiNi_(0.8)Co_(0.2)O_2 Films for Application in Microbatteries,Chem.Mater.2006,18,1397-1400.
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[14].Y.Gu,D.Chen,X.Jiao,Synthesis and characterization of hollow LINiO_2 fibers via a simple electrospinning methode.,J.Sol-GeL Sci.Tech.,2007,43(2),245-249
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[16].S.Schougaard,J.Breger,M.Jiang,C.Grey,J.Goodenough,LiNi_(0.5+δ)Mn_(0.5+δ)O_2-A High-Rate,High-Capacity Cathode for Lithium Rechargeable Batteries,Adv.Mater.,2006,18,905-909.
[1].A.K.Padhi,K.S.Nanjundaswamy,J.B.Goodenough,.Phospho-oliveines an Positiv-Electrode Materials for Rechargeable Lithium Batteries.J.Electrochem.Soc.1997,144,1188-1196.
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[7].L.N.Wang,Z.G.Zhang,K.L.Zhang,A simple cheap soft synthesis routine for LiFePO_4 using iron(Ⅲ)raw material,Journal of Power Sources,2007,167,200-205
[8].C.Alvaro,C.Manuel,M.Julia,S.Jesus,R.Enrique,A New and Fast Synthesis ofNanosized LiFePO_4 Electrode Materials,Eur.J.Inorg.Chem.,2006,1758,1758-1764.
[9].R.Dominko,M.Bele,M.Gaberseek,M.Remskar,D.Hanzel,J.M.Goupil,S.Pejovnik,J.Jamnik,Porous olivine composites synthesized by sol-gel technique,Journal of Power Sources,2006,153,274-280.
[10].G.X.Wang,S.Needhama,J.Yaoa,J.Z.Wang,R.S.Liu,H.K.Liu,A study on LiFePO_4 and its doped derivatives as cathode materials for lithium-ion batteries,Journal of Power Sources,2006,159,282-286.
[11].T.Shiratsuehi,S.Okadaa,J.Yamaki,S.Yamashita,Y.Nishida,Cathode performance of olivine-type LiFePO_4 synthesized by chemical lithiation,Journal of Power Sources,2007,173,979-984.
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[11].Y.Gu,D.Chen,X.Jiao,Synthesis and electrochemical properties of nanostructured LiCoO_2 fibers as cathode materials for lithium-ion batteries Journal of Physical Chemistry B 2005,109(38),17901-17906.
[12].Li,D.;McCann,L.T.;Xia,Y.Use of electrospinning to directly fabricate hollow nanofibers with functionalized inner and outer surfaces,Small,2005,1(1),83-86.
[13].(a)Y.Gu,D.Chen,X.Jiao,LiCoO_2/MgO coaxial fibers:co-electrospun fabrication,characterization and electrochemical properties,Journal of Material Chemistry,2007,18,1769-1776.;
(b)S.Zhan,D.Chen,X.Jiao,Long TiO_2Hollow Fiber with Mesoporous Walls:Sol-Gel Combined Electrospun Fabrication and Photocatalytic Properties,J.Phys.Chem.B,2006,110,11199-11204.;
(c)C.Gong,D.Chen,X.Jiao,Q.Wang,Continuous hollow α-Fe_2O_3 and α-Fe fibers prepared by the sol-gel method,J.Mater.Chem.,2002,1844-1847.
[14].C.Djordjevic,M.Lee,E.Sinn,Oxoperoxo(citrato)- and dioxo(citrato)vanadates(V):synthesis,spectra,and structure of a hydroxyl oxygen bridged dimer K_2[VO(O_2)(C_6H_6O_7)]_2·2H_2O,Inorg.Chem.1989,28,719-723.
[15].S.Schougaard,J.Breger,M.Jiang,C.Grey,J.Goodenough,LiNi_(0.5+δ)Mn_(0.5+δ)O_2-A High-Rate,High-Capacity Cathode for Lithium Rechargeable Batteries,Adv.Mater.,2006,18,905-909.
[1].(a)Kim,C.;Yang,K.S.Electrochemical properties of carbon nanofiber web as an electrode for supercapacitor prepared by electrospinning Appl.Phys.Lett.2003,83,1216-1218.;
(b)Choi,S.W.;Jo,S.M.;Lee,W.S.;Kim,Y.-R.An electrospun poly(vinylidene fluoride)nanofibrous membrane and its battery applications,Adv.Mater.2003,15,2027-2032.
[2].(a)Hwa.Jung,J.;Kobayashi,H.;van Bommel,K.J.C.;Shinkai,S.;Shimizu,T. Creation of novel helical ribbon and double-layered nanotube TiO_2 structures using an organogel template,Chem.Mater.2002,14,1445-1447.;
(b)Kobayashi,S.;Hamasaki,N.;Suzuki,M.;Kimura,M.;Shirai,H.;Hanabusa,K.Preparation of helical transition-metal oxide tubes using organogelators as structure-directing agents,J.Am.Chem.Soc.2002,124,6550-6551.
[3].Loscertales,I.G.;Barrero,A.;Marquez,M.;Spretz,R.;Velarde-Ortiz,R.;Larsen,G.Electrically Forced coaxial nanojets for one-step hollow nanofiber design,J..Am.Chem.Soc.,2004,126,5376-5377.
[4].Gong,C.;Chen,D.;Jiao,X.;Wang,Q.Continuous hollow α-Fe_2O_3 and α-Fe fibers prepared by the sol-gel method,J..Chem.Mater.2002,12/6,1844-1847.
[5].(a)Li,D.;Xia,Y.Direct fabrication of composite and ceramic hollow nanofibers by electrospinning,Nano Lett.2004,4/5,933-938.;
(b)McCann,J.T.;Li,D.;Xia,Y.Electrospinning of nanofibers with core-sheath,hollow,or porous structures,J..Mater.Chem.2005,15,735-738.
[6]。吴宇平,万春荣,姜长印等。,电源技术 2000,24(2),112-115。
[7].C.Ramana,K.Zaghib,C.Julien,Highly Oriented Growed of Pulsed-Laser Deposited LiNi_(0.8)Co_(0.2)O_2 Films for Application in Microbatteries,Chem.Mater.2006,18,1397-1400.
[8].(a)M.Thomas,W.David,J.Goodenough,P.Groves,Synthesis and structural characterization of the normal spinel LiNi_2O_4.Mater.Res.Bull.1985,20,1137-1146.;
(b).T.Ohzuku,T.Yanagawa,M.Kouguchi,A.Ueda,Innovative insertion material of LiAl_(1/4)Ni_(3/4)O_2(R-m)for lithium-ion(shuttlecock)batteries.J.Power Sources.1997,68,131.
[9].Chebiam,R.V.;Prado,F.;Manthiram,A.Soft Chemistry Synthesis and Characterization of Layered Li_(1-x)Ni_(1-y)Co_yO_(2-δ)(0≤x ≤1 and 0 ≤y≤1),Chem.Mater.2001,13,2951.
[10].C.Delmas,G.Prado,A.Rougier,E.Suard,and L.Fourne's,Effect of iron on the electrochemical behaviour of lithium nickelate:from LiNiO_2 to 2D-LiFeO_2.Solid State Ionics 2000,135,71-79.
[11].Hench,L.L.;West,J.K.The sol-gel process,Chem.Rev.1990,90,33-72
[12].Aizawa,M.;Nakagawa,Y.;Nosaka,Y.;Fujii,N.;Miyama,H.Preparation of hollow TiO_2 fibers,J.Non-Cryst.Solids 1990,124,112-115.
[13].Wienk,I.M.;Boom,R.M.;Beerlage,M.A.M.;Bulte,A.M.W.;Smolders,C.A.;Strathrnann,H.Recent advances of the formation of phase inversion membranes made from amorphous or semi-crystalline polymers,J.Member.Sci.1996,113,361-371.
[14].Y.Gu,D.Chen,X.Jiao,Synthesis and characterization of hollow LINiO_2 fibers via a simple electrospinning methode.,J.Sol-GeL Sci.Tech.,2007,43(2),245-249
[15].Jang,Y.-I.;Neudecker,B.J.;Dudney,N.J.Electrochem.Solid-StateLett.2001,4,A74.
[16].S.Schougaard,J.Breger,M.Jiang,C.Grey,J.Goodenough,LiNi_(0.5+δ)Mn_(0.5+δ)O_2-A High-Rate,High-Capacity Cathode for Lithium Rechargeable Batteries,Adv.Mater.,2006,18,905-909.
[1].A.K.Padhi,K.S.Nanjundaswamy,J.B.Goodenough,.Phospho-oliveines an Positiv-Electrode Materials for Rechargeable Lithium Batteries.J.Electrochem.Soc.1997,144,1188-1196.
[2].G.Rousse,J.Rodriguez-Carvajal,S.Patoux,C.Masquelier,Magnetic Structures of the Triphylite LiFePO_4 and of Its Delithiated Form FePO_4.,Chem.Mater.2003,15,4082-4087.
[3].Yamada A.,Chung S.C.,Hinokuma K.,Optimized LiFePO_4 for lithium battery cathodes.,J.Electrochem.Soc.,2001,148(3),224-229.
[4].H.Huang,S.-C.Yin,L.F.Nazar,Electrochem.Solid-State Lett.2001,4,A170.
[5].A.Andersson.,J.Thomas.,The source of First-cycle Capacity Loss in LiFePO_4.,J.Power.Source.,2001,97-98,498-502.
[6].A.Padhi.,K.Nanjundaswamy.,J.Goodenough.,Phospho-olives as Positive-Electrode Material for Rechargeable Lithium Batteries.,J.electrochem.Soc.,1997,144(4),1188-1193.
[7].L.N.Wang,Z.G.Zhang,K.L.Zhang,A simple cheap soft synthesis routine for LiFePO_4 using iron(Ⅲ)raw material,Journal of Power Sources,2007,167,200-205
[8].C.Alvaro,C.Manuel,M.Julia,S.Jesus,R.Enrique,A New and Fast Synthesis ofNanosized LiFePO_4 Electrode Materials,Eur.J.Inorg.Chem.,2006,1758,1758-1764.
[9].R.Dominko,M.Bele,M.Gaberseek,M.Remskar,D.Hanzel,J.M.Goupil,S.Pejovnik,J.Jamnik,Porous olivine composites synthesized by sol-gel technique,Journal of Power Sources,2006,153,274-280.
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