- LiFe y Ti x Mn 2-x-y O 4 (0x, y1)

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Φωκάς Καλαμογδάρτης
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1 LiFe y Ti x Mn 2xy O 4 0x y1) !"#$%&%$ " ' 2007

2 $ ) $ : * + & #' : )! * )!* ':! * «21» ' / ) # $ : ' 1 ) # $ ' " 2

3 ! 3 3 / ' '/' «1» '' %* 1 4 / " 1 ' LiMn 2 O ~ 4! Li)! 4 4 ' * d LiFe y Mn 2y O 4 0 < y 05) 3 ' ! Li [1] ' Fe 3+ /Fe 4+ : '' 1 LiFe y Mn 2y O 4 ' 4! ' Mn 3+ /Mn 4+ ) * ' ~5! LiFeMnO 4 1 LiMn 2 O 4 ) !! ) * LiFeTiO 4 [2] LiMnTiO 4 [3] C Li 4 Ti 5 O ' ~ 17 2! Li [4]" LiFeMnTi) 2 O 4 Fd3m) 1 * 3 * 4 ' 6/ LiFe Ti Mn) 2 O 4 1

4 4 " 3* 73 * LiFe y Ti x Mn 2xy O 4 0 y 1) ) ' 4 #5 LiFe y Ti x Mn 2xy O 4 0 y 1)!) 3 3*:! LiFe Mn Ti) 2 O 4 * * 4 1 ' ' '' 1 4 ' 4 4 ' 4 : 3* 1 * ' ; 3 ' / ) ' /' + ) # $ ) 1

5 $ ) $ ' ) INTAS 9 YF ) $& ) # $ 2006 * 3* 1: & 1 ' LiFe Mn Ti) 2 O 4! 4 LiFe y Ti x Mn 2xy O 4 0 y 1) 4 4 ' ' 4 ' $ 1 ' 1 ):"" # $ 1 1 : International Symposium on New Trends in Intercalation Compounds for Energy Storage and Conversion 205 th the Electrochemical Society Meeting 30 April 2 May 2003 Paris France; III IV # $ +# $ 2003; % 2004) II International Conference "Mechanochemical Synthesis and Sintering" 1517 June 2004 Novosibirsk; * «&» ; International Conference on Solid State Chemistry 1415 Sept 2004 Prague Czech Rep;! c ' ": ' 2004" %; VIII 1 ' «& 4 4» ;! ' ' ") " ; 15 th International Conference on Solid State Ionics SSI15) 1722 July 2005 BadenBaden Germany; V International Conference on Mechanochemistry and Mechanical Alloying INCOME2006) July 36 Novosibirsk; Topical Meeting of the European Ceramic Society Structural Chemistry of Partially Ordered Systems Nanoparticles and Nanocomposites June St Petersburg; 8 th International Symposium on Systems with Fast Ionic Transport 8 th ISSFIT) 2327 May 2007 Vilnius Lithuania; 16 th International Conference on Solid State Ionic SSI16) 16 July 2007 Shanhai China! '

6 '! 1 ):"" # $ : " 3 ;;; +; )0 # $! 7; 60 + / ); 3 + ) ' ' 29 4 ' ' 5 /' 5 1 ' ' ' 1 ' 1 * * 3* LiMn 2 O 4 4 # 1 ' 4 # 3* LiFe Mn Ti) 2 O 4 3 3* ) ' / 5 ' ' " LiFe y Ti x Mn 2xy O 4 0 x y 1) : «auto ignition» ): ' LiOH H 2 O MnO 2 TiO 2 ) Fe 2 O 3 xh 2 O/γFe 2 O 3 ' A# o C 10

7 o C 15 ): 3! [5] 3 4 ' 1 ')! 3 3* : LiNO 3 FeNO 3 ) 3 9H 2 O TiO 2 ) MnNO 3 ) 2 H 2 O/ MnC 2 H 3 O 2 ) 2 4H 2 O) ) / ' ' :! P123 µ =5800 / )! FeSO 4 7H 2 O/FeCl 2 4H 2 O LiOH H 2 O MnNO 3 ) 2 H 2 O TiC 12 H 28 O 4 ) 3* : 1 < ) P ) ' 4 C 2 H 6 O < ) * 24 ) # ' 3* : ) /$#4 Co Cu Kα Bruker D8 ADVANCE Cu Kα 5 2Θ= ' Li Fe Mn Ti) Varian 280 FS 1 Mn 3+ *3 4 Philips CM30T JEM 2000FX LaB ! 1 )!" NZ640/2!$) ) α Fe ) 57 Co ' Cr ' 1 1 *

8 # ' ' Hewlett Packard 4284A Precision LCRMeter " : 3 ± 05 0 #$ CR2320 Hohsen) 1 4 LiPF 6 1M) EC/DMC 1:2) /c '3 Solvay) Carbon black >999% <10 =m; Alfa) 01 mm; Fluka) 80:10:3:7; 3* ' 12 NMP MerckSchuchardt) 3 * * 200 µ * 70 = 4 14 #$ $ > ' 4 05LiClO 4 05Al 2 O 3 [6] «4» 400 3* / 4 4 ' * Al Ni V '' % / %! / 05LiClO 4 05Al 2 O 3 / 0 5! 200 *3 $ ! 3 210!/ 3 APPA 107!%& $ ; 40 *3 ' 1 : Li Mn Fe Ti! LiFe 3+ ymn 4+ 1δMn 3+ 1+δyO 405δ 0 < y < 1)

9 $ 1 LiFe y Ti x Mn 2xy O 4 0 x y 1) δ δ max =02) : LiFe y Ti x Mn 2xy O 4 0 x y 1) 0 3* LiOH?H 2 O: Li 7% Fe8% Mn27% Ti13% *3 1) * $ 2 # * 3 * LiFeTiO 4 LiFeMnO 4 LiMn 2 O 4 * LiFeTiMn) 2 O 4 2)! ' 1

10 Fd3m) 4 a c '' < y < 11; x = 0 3) a c 1 1* ' x = 0; 0 y 05) 3 [1]; LiFeTiO 4 a c = 8362±0002Å) [2] ' LiFeMnO Li 2 MnO 3 ' 1 4 ' 2[Mn Mn4+ ] x x + O O 2[Mn 3+ Mn ]' + V O + 1 / 2 O 2 '' Mn 3+ $ 3 LiFe y Ti x Mn 2xy O 4 0 x y 1) '' ' $ 4 LiFe y Ti x Mn 2xy O 4 x=0)! '' 1 $ LiFe y Ti x Mn 2xyO 4 0 < x y < 1) 4 ; LiFe y Ti x Mn 2xy O 4 * < y < 06 x=0) y > 06 3 : MnNO 3 ) 2 H 2 O Li 2 MnO 3 ' ' 3

LiFeyTixMn2yxO4 0 < x y < 1) * 3 4 5 $ ' LiFe05Mn15O4

11 6 4 5 '! ' / ' Mn2+ Mn4+)! ' 3* 1 1 : y > 06) 3 ' ac 3 4) LiMn2O4 ' * 3 4 ) *» ' LiFeyTixMn2yxO4 0 < x y < 1) * $ ' LiFe05Mn15O4 3* ' LiFe07Mn13O4 LiTiMnO4 ' ) "! 100 ' «1); 1 $ 5 6!: LiFe07Mn13O4 2) 2 ' LiFe05Mn15O4 1); LiTiMnO4 3) ' ' ' % % $ 4 LiFeyTixMn2yxO4 0 < y 1 x=0) 3 3 3* 50 3 " 1 1 *! " $ 6) : '

12 d '! 07 < y 1 $ 6 4 ' y07 y>07 a ) * [Fe 3+ tetra]) '' ' ': 3 4 1! LiFe y Ti x Mn 2yx O 4 01 y 05 x=0) " LiFe y Ti x Mn 2yxO 4 01 y 1) 78) # 4 ' 4 ' '' 4 '' ' ' '' ' ! LiFeTiO 4 ) 0294! LiMn 2 O 4 ) 1 5 ' Mn 3+ ' Mn 4+ ) Mn 3+ 3 ' 3* '

13 $ 7 LiFe y Ti x Mn 2xy O 4 0 x y 1) $ 8 LiFe y Ti x Mn 2yx O 4 0 x y 1) '' ' 203 0!!%& "$$ $ % " ' % " 6 LiFe y Ti x Mn 2yx O 4 0 x y 1) 0! Li/LiFe y Ti x Mn 2xy O 4 0 x y 1) 4 4 : !! ' '/' ) 9 3* 4 ': / 1 1* 9 ; %)): ' / ' Mn 3+ /Mn 4+ : LiFe y Ti x Mn 2xy O 4 <=>Li y [Fe y Ti x Mn 2yx ]O 4 + 1y)Li + +1y)e 42! 1) 3* Fe 3+ /Fe 4+ '

14 Li y [Fe y Ti x Mn 2yx ]O 4 <=>[Fe y Ti x Mn 2yx ]O 4 + yli + + ye 47 5! 2); / LiTiMnO 4 9! )): LiTi x Mn 2x O 4 <=>V Li [Ti x Mn 1x O] 4 + Li + +e 4042! 3); / LiFeTiO 4 9/)): LiFeTiO 4 + Li + + e <=> Li 2 FeTiO ! 4) 4042! 1 '' ' III) 4750!) '' 1 " $ 9 LiFe 05 Mn 15 O 4 ;) LiTiMnO 4! ) LiFeTiO 4 /) LiFe 04 Ti 01 Mn 15 O 4 %) 0 ')! ') 1 1* ' 0

15 ! 3 3 ' ' *3 : ' ' ' 4 ' 1 ' 9 %) 1 1* # ' 3 4 ' ' * Mn 4+ ' ) Fe 4+ ' 4 ) #$ " " 4 3 # 3 3;! 4 4 ' 3 ' 4 05LiClO 4 05Al 2 O Li 5 Ti 4 O 12 / 05LiClO 4 05Al 2 O 3 / LiMn 2 O 4 1) LiMn 2 O 4 / 05LiClO 4 05Al 2 O 3 /LiFe 08 Mn 12 O 4 2) LiMn 2 O 4 / 05LiClO 4 05Al 2 O 3 / LiMn 2 O 4 3) ! Li 5 Ti 4 O 12 6/ 22! 6/ Li/Li + /LiMn 2 O 4 4!) Li/Li + /Li 5 Ti 4 O 12 17!) 10 LiFe 08 Mn 12 O 4 1) 2) ' 4 LiFe 08 Mn 12 O 4 ' 4 ' '' Mn 4+ 3* ' 1)) 3* ; 3* 4 : )LiMn 2 O 4 / 05LiClO 4 05Al 2 O 3 / LiMn 2 O 4 +) )

16 )Li 4 Ti 5 O 12 / 05LiClO 4 05Al 2 O 3 / LiFe 05 Mn 15 O 4 +) ;); $ 11! 4 3 3* ': : LiMn 2 O 4 + xli + + e <=> Li 1+x Mn 2 O 4 ~ 3! Li/Li + ); Li 4 Ti 5 O e +3Li + <=> Li 7 Ti 5 O 12 ; ~ 17! Li/Li + ); : LiMn 2 O 4 <=> xli + + Li 1x Mn 2 O 4 + xe ~ 3942! Li/Li + ); LiFe 05 Mn 15 O 4 <=> xli + + Li 1x Fe 05 Mn 15 O 4 + xe ; 4 ~ 5! Li/Li + ) $ 10 ) 13; ) ' LiFe 08 Mn 12 O 4 1) 2) ' / 2 ; 4 7 $ 11! )" ;) ' 10!/ ' 10!/) 3 ~16! 3* ' ' LiMn 2 O 4 11 )) ' 6/ 15! % LiFe 05 Mn 15 O 4 2

17 3* 4 ' Mn 3+ /Mn 4+ Fe 3+ /Fe 4+ ' 6/ ; ~29! 11 ;)) ' 4 ' ' #$%& 1! LiFe y Ti x Mn 2xy O 4 0 y1)!)! 4 2 # * * * LiMnFeTi) 2 O ' 1 1 y 07) LiFe y Ti x Mn 2xy O 4 Fe d ' / '' Fe #1 ' 1 '' ' LiFe y Ti x Mn 2xyO 4 0 y1); 4 '' ' * 5! LiFe y Ti x Mn 2xy O 4 0 y 1) 4 * 0 3 / 3 ' 3 3 ' ) 6 #* 4 ' 4 4 ' 4

18 ')! 1 T Ohzuku K Ariyoshi S Takeda YSakai // Electrochimica Acta 2001 V 46 P Crystal structure and electrical properties of LiFeTiO 4 / MA Arillo ML Lopez E PerezCappe C Pico ML Veiga // Solid State Ionics 1997 V 107 P Structural characterisation and physical properties of LiMMnO 4 M=Cr Ti) spinels / MA Arillo G Guello ML López P Martin C Pico ML Veiga // Solid State Sciences 2005 V 7 Issue 1 P Li Insertion into Li 4 Ti 5 O 12 SpinelCharge Capability vs Particle Size in ThinFilm Electrodes / L Kavan J Prochazk TM Spitler MKalba M Zukalova T Drezen M Gratzel // J of The Electrochem Soc 2003 V150 7) P A1000A ' 8 : ) Composite solid electrolytes LiClO 4 Al 2 O 3 / AS Ulihin NF Uvarov Yu G Mateyshina LI Brezhneva AA Matvienko // Solid State Ionics 2006 V177 P # ' 3 * : 1 1 1* ' / &+ "3 // : C Electrochemical modification of spinel oxide materials using lithium solid state electrolyte/ Yu G Mateyshina NF Uvarov AS Ulihin Yu T Pavlyukhin // Solid State Ionics 2006 V177 P Composite solid electrolytes LiClO 4 Al 2 O 3 / AS Ulihin NF Uvarov Yu G Mateyshina LI Brezhneva AA Matvienko // Solid State Ionics 2006 V177 P Solid state electrochemical lithium cells with oxides electrodes and solid composition electrolyte/ Yu G Mateyshina NF Uvarov AS Ulihin // V43 95 P Synthesis and characterization of new ironcontaining materials for 5V lithium batteries/ Yu G Mateyshina N F Uvarov// In: New trends in intercalation compounds for energy storage conversion ed by K Zaghib C M Julien J Prakash) Proc Intern Symp Paris France 30 April 2 May 2003) Electrochem Soc Pennington V P ' / &+ "3 //& 4 4 VI 1 ' ) " 4 4 LiClO 4 Al 2 O 3 / + 81 &+ // & 4 4

19 VI 1 ' ) / + //! ' ' «)» ) ' / & + // " ' ) C " 4 4 LiClO 4 Al 2 O 3 / + // " ' ) C Synthesis and characterization of new ironcontaining materials for 5V lithium batteries / Yu G Mateyshina N F Uvarov // International Symposium on New trends in intercalation compounds for energy storage conversion Paris France 30 April 2 May 2003) Paris Mechanochemical synthesis of ironcontaining lithium spinels/ YuGMateyshina NFUvarov YuTPavlyukhin// II Intern Conf on Fundamental Bases of Mechanochemical Technologies "Mechanochemical synthesis and sintering" Novosibirsk Russia 1517 June 2004) Novosibirsk 2004 P Transport properties of solid solutions LiFe x Mn 2x O 4 / YuGMateyshina NFUvarov YuTPavlyukhin // 7th Meeting «Fundamental Problems of Solid State Ionics" Chernogolovka Russia 1618 June 2004) Chernogolovka Structure and electrochemical properties of solid solutions LiFe 1y Ti 1 xmn x+y O 4 / YuGMateyshina NFUvarov YuTPavlyukhin // Conf on Solid State Chemistry Prague Czech Rep 1415 Sept 2004) Prague Crystal Structure and Transport Properties of Solid Solutions LiFe X Mn 2 XO 4 / YuGMateyshina NFUvarov YuTPavlyukhin // 4th Intern Conf on Inorganic Materials Antwerpen Belgium 1921 Sept 2004) Antwerpen ) LiFe 1y Ti 1x Mn x+y O 4 / + & 3 "// Vlll 1 ' «& 4 4» % ) % ' / &+ "3 // VI 1 0 «& 4 4» ) / + //! ' ' «)» ) ' / + & // " ' C 98101

20 20 " 4 4 LiClO 4 Al 2 O 3 / + // ' 4 4 LiClO 4 Al 2 O 3 / &+ "3 81 // IV C C# $ +# $ "" " c 2005 ) Composite solid electrolytes LiClO 4 Al 2 O 3 / ASUlihin NFUvarov YuGMateyshina LIBrezhneva AAMatvienko // XV Intern Conference on Solid State Ionics SSI15) BadenBaden Germany 1722 July 2005) BadenBaden 2005 P Effect of mechanical activation on cation distribution in lithium ironmanganese spinels / YuG Mateyshina YuT Pavlyukhin N F Uvarov // V International Conference on Mechanochemistry and Mechanical Alloying INCOME 2006) Novosibirsk Russia July ) Novosibirsk 2006 P Solid state electrochemical lithium cells with oxide electrodes and composite solid electrolyte/ YuG Mateyshina NF Uvarov AS Ulihin // Abstracts of 8 th International Meeting Fundamental Problems of Solid State Ionics Chernogolovka Russia June ) Chernogolovka 2006 P Nanocomposite solid electrolytes for intermediate temperature lithium batteries / YuGMateyshina ASUlihin NYuShestakova NFUvarov // Abstracts of Topical Meeting of the European Ceramic Society Structural Chemistry of Partially Ordered Systems Nanoparticles and Nanocomposites St Petersburg Russia June ) St Petersburg 2006 P Influence of the chemical nature of nanocrystalline oxide on ionic conductivity of composite solid electrolytes based on LiClO 4 / AS Ulihin YuGMateyshina LI Brezhneva NFUvarov OAKharlamov VPIsupov // Abstracts of 2 Russian Conference on Nanomaterials NANO2007)Novosibirsk Russia 1316 March 2007) Novosibirsk 2007 P Autoignition synthesis and investigation of nanocrystalline complex lithium oxides / YuGMateyshina NFUvarov BBBokhonov YuTPavlyukhin ULafont EM Kelder // Abstracts of 2nd Russian Conference on Nanomaterials NANO2007) Novosibirsk Russia 1316 March 2007) Novosibirsk 2007 P Physical and electrochemical properties of lithium manganeseiron oxides prepared by different methods / YuGMateyshina ULafont NF Uvarov E M Kelder // Abstract of 8 th International Symposium on Systems with Fast Ionic Transport 8 th ISSFIT) Vilnius Lithuania 2327 May 2007) Vilnius 2007 P Crystal structure and electrochemical properties of solid solutions in the system LiMn 2 O 4 LiFe 2 O 4 LiTi 2 O 4 / YuGMateyshina NFUvarov BBBokhonov ULafont EM Kelder // Abstract 16 th International Conference on Solid State Ionic SSI16) Shanhai China 16 July 2007) Shanhai 2007 P754

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