Lityum iyon pillerinin katot malzemesi olan LixMy(PO4)z ve LixMyO4 tipindeki bileşiklerin bazı metaller kullanılarak sentezi ve karakterizasyonu

Abstract

Bu tez çalışmasında, lityum iyon bataryalarda katot malzemesi olmaya aday LixMy(PO4)z (M=Mn, Ni, Cu, Cr, Fe, Mo ve Pb) ve LixMyO4 (M=Mn, Ni, Cu, Cr, Fe, Mo ve Pb) genel formülüne sahip malzemeler; LiNO3, metal oksitler ve metal fosfatlar kullanılarak mikrodalga enerji sentez yöntemi ve yüksek sıcaklık katı hal sentez yöntemi ile sentezlenmiştir. Mikrodalga enerji sentez yöntemi ile yapılan deneylerde 400 W ve 800 W güç değerlerinde 10 dakika süre ile çalışılmıştır. Yüksek sıcaklık katı hal yöntemi ile yapılan deneylerde ise 400 °C’ de ön kalsinasyon işleminin ardından 800 ºC’ de sentezler gerçekleştirilmiştir. Elde edilen ürünlerin karakterizasyonu X-Işınları Toz Kırınımı (X-Ray Diffraction) ve Fourier Geçişli Kızılötesi Spektroskopisi (Fourier Transform, FT-IR) ile yapılmıştır. Mikrodalga enerji sentez yöntemi kullanılarak yapılan deneylerde, Li3PO4 (ICSD 02-0208), Li1,85Na0,15V2O6 (ICSD 02-5559), FePO4 (ICSD 09-8064), Fe3PO4 (ICSD 03-6207), Mn(V2O6) (ICDD 72-1837), Li(Mo2P2O11) (ICSD 08-2205), Li0,301Ni1,699O2 (ICSD 04-4266), Li0,56Fe1,41Mn0,99O4 (ICSD 09-3827), Li0,208Ni1,792O2 (ICSD 04-4267), LiCr0,3614Mn1,6386O4 (ICSD 08-8651) ve MnMoO4 (ICSD 07-8328) bileşikleri tek faz olarak elde edilirken; Cr0,11O5,16V2 (ICSD 08-6180)- LiN2O3(ICDD 35-0925), Li2VPO6 (ICSD 07-3868)-FePO4 (ICSD 04-0864), LiMnPO4 (ICSD 03-8208)-LiVO3(ICSD 00-2899), LiCoO2 (ICSD 16-4802)-Fe2,937O4 (ICSD 08-2444), Li0,301Ni1,699O2 (ICSD 04-4266)- Fe2O3 (ICSD 05-1122), Li0,429Fe1,143Mn1,429O4 (ICSD 15-5278)-Mn2O3 (00-9090), Li0,956Mn2,044O4 (ICSD 09-0131)-Cr2O3 (ICSD 02-9298), Li0,2Mn1,9O4 (ICSD 41-2043)- LiCoO2 (ICSD 16-4802) ve Li0,78Mn0,85O2 (ICSD 17-3134)-NiO (ICSD 64-6096) bileşikleri çift faz olarak elde edilmiştir. Yüksek sıcaklık katı hal sentez yöntemi kullanılarak yapılan deneylerde Li3Fe2(PO4)3 (ICSD 06-9347), Li0,3CoFe2O4 (ICDD 40-1119), Li0,63Fe1,37O2 (ICSD 07-8713), LiMn1,5Fe3,5O8 (ICSD 05-1695), CoCr2O4 (ICSD 06-1612), Li0,301Ni1,699O2 (ICSD 04-4266), LiMn1,825Cr0,175O4 (ICSD 15-6096), Li2CoMn3O8(ICSD 09-0649), LiMn1,5Ni0,5O4 (ICSD 07-0047), CoMoO4 (ICSD 02-3808), NiMoO4 (ICSD 08-1059), Cu1,49Mo8O24 (ICSD 07-4893), MnMoO4 (ICSD 07-8328), (ICSD 08-0449) ve Cr2Mo3O12 (ICSD 41-8845) bileşikleri tek faz olarak sentezlenirken; Cr0,11V2O5,16 (ICSD 08-6180)-Li2V2(PO4)3 (ICSD 09-6963)bileşikleri çift faz olarak sentezlenmiştir.

In this thesis, LixMy(PO4)z (M = Mn, Ni, Cu, Cr, Fe, Mo and Pb) and LixMyO4 (M = Mn, Ni, Cu, Cr, Fe, Mo) materials of general formula; LiNO3 was synthesized by microwave energy synthesis method using metal oxides and metal phosphates and high temperature solid state synthesis method. In the experiments conducted with microwave energy synthesis method, 400 W and 800 W power values were studied for 10 minutes. In the experiments conducted with high-temperature solid-state method, 400 ° C followed by pre-calcination at 800 ºC. Characterization of the products was done by X-Ray Diffraction and Fourier Transition Infrared Spectroscopy (Fourier Transform, FT-IR). In experiments using microwave energy synthesis method Li3PO4 (ICSD 02-0208), Li1,85Na0,15V2O6 (ICSD 02-5559), FePO4 (ICSD 09-8064), Fe3PO4 (ICSD 03-6207), Mn(V2O6) (ICDD 72-1837), Li(Mo2P2O11) (ICSD 08-2205), Li0,301Ni1,699O2 (ICSD 04-4266), Li0,56Fe1,41Mn0,99O4 (ICSD 09-3827), Li0,208Ni1,792O2 (ICSD 04-4267), LiCr0,3614Mn1,6386O4 (ICSD 08-8651) and MnMoO4 (ICSD 07-8328) compounds were synthesized as single phase; Cr0,11O5,16V2 (ICSD 08-6180)- LiN2O3(ICDD 35-0925), Li2VPO6 (ICSD 07-3868)-FePO4 (ICSD 04-0864), LiMnPO4 (ICSD 03-8208)-LiVO3(ICSD 00-2899), LiCoO2 (ICSD 16-4802)-Fe2,937O4 (ICSD 08-2444), Li0,301Ni1,699O2 (ICSD 04-4266)- Fe2O3 (ICSD 05-1122), Li0,429Fe1,143Mn1,429O4 (ICSD 15-5278)-Mn2O3 (00-9090), Li0,956Mn2,044O4 (ICSD 09-0131)-Cr2O3 (ICSD 02-9298), Li0,2Mn1,9O4 (ICSD 41-2043)- LiCoO2 (ICSD 16-4802) and Li0,78Mn0,85O2 (ICSD 17-3134)-NiO (ICSD 64-6096) were obtained as a double phase. Experiments using high temperature solid state method Li3Fe2(PO4)3 (ICSD 06-9347), Li0,3CoFe2O4 (ICDD 40-1119), Li0,63Fe1,37O2 (ICSD 07-8713), LiMn1,5Fe3,5O8 (ICSD 05-1695), CoCr2O4 (ICSD 06-1612), Li0,301Ni1,699O2 (ICSD 04-4266), LiMn1,825Cr0,175O4 (ICSD 15-6096), Li2CoMn3O8(ICSD 09-0649), LiMn1,5Ni0,5O4 (ICSD 07-0047), CoMoO4 (ICSD 02-3808), NiMoO4 (ICSD 08-1059), Cu1,49Mo8O24 (ICSD 07-4893), MnMoO4 (ICSD 07-8328), (ICSD 08-0449) ve Cr2Mo3O12 (ICSD 41-8845) compounds were synthesized as single phase; Cr0,11V2O5,16 (ICSD 08-6180)-Li2V2(PO4)3 (ICSD 09-6963) were synthesized as as a double phase.