新型Na掺杂双钙钛矿氧化物的制备与性质研究
摘要
采用高温固相合成法制备了8种新型钠掺杂的双钙钛矿氧化物。其中,Na由于具有挥发性而使得人们对其掺杂的结构研究比较少,而含四价Fe或四价Cr的双钙钛矿型氧化物由于其很难制备纯的样品及产物的不稳定性使得对其的研究更是少之甚少。考虑到以上原因,我们开创性地制备了几种Na掺杂的双钙钛矿型氧化物,同时又在同一个双钙钛矿结构中既引入Na又包含四价Fe或四价Cr。新型双钙钛矿氧化物的制备及性质研究为无机新材料的设计和定向合成探明了道路,并为相关的理论研究打下了一定的基础。
Perovskite complex mental oxides have attracted more and more attention due to their complicated magnetic and electrical properties. In recent decades, various methods have been used to prepare A-doped or B-doped Perovskite complex metal oxides, such as conventional solid state reaction, sol-gel technique, hydrothermal technique, coprecipitation method, pulsed laser technique and self-propagating high-temperature synthesis. Many powder, film or single crystal materials were obtained by exchanging the doped element or varying the content of doped element in perovskite complex mental oxides. So far, however, there is not comprehensive conclusion about the physical and chemical properties of perovskite complex mental oxides, and some phenomenon is still in doubt. In view of the great value and study scope of these materials, more and more researchers are indulging in the study of perovskites.
There are many new perovskites, double perovskites and their doped metal oxides, however, most of them are focused on the easily prepared oxides, such as manganese-based complex oxides and molybdenum-based complex oxides. The reports about difficultly prepared oxides are very rare. For example, due to the volatility of Na, there are little reports about Na-doped perovskites. It is difficult to obtain pure Fe(IV)-doped or Cr(IV)-doped perovskites, and the Fe(IV)-doped or Cr(IV)-doped perovskites are unstable, which makes people unwilling to study these oxides. In view of the reasons mentioned above, we have prepared eight Na-containing perovskite complex metal oxides through conventional solid state reaction. Besides, we introduce Fe(IV) or Cr(IV) into these Na-containing oxides, which are not reported previously.
1. We have synthesized four novel double perovskites containing Na+ of LaNaFe(Ⅲ)TaO_6、LaNaFe(Ⅲ)NbO_6、LaNaMn(Ⅲ)TaO_6、LaNaMn(Ⅲ)NbO_6 through conventional solid state reaction. XRD analysis displays that all compounds have high degree of crystallization. SEM shows that the microstructure of these compounds is irregular, the crystalline grain exhibit different shape and dimension. TGA analysis displays all compounds are stable below 1000 oC at 10%H2-Ar atmosphere. Magnetic property test indicates that LaNaFe(Ⅲ)TaO_6 and LaNaFe(Ⅲ)NbO_6 contain weak ferromagnetic component,while LaNaMn(Ⅲ)TaO_6 and LaNaMn(Ⅲ)NbO_6 are soft magnets.
2. With the goal of introducing Na+ and Fe~(4+) or Cr~(4+) into the same compound, we have synthesized four novel double perovskites of CaNaFe(IV)TaO_6、SrNaFe(IV)TaO_6、CaNaCr(IV)TaO_6、SrNaCr(IV)TaO_6. XRD analysis displays that all compounds have high degree of crystallization. SEM shows that the microstructure of CaNaFe(IV)TaO_6 and SrNaFe(IV)TaO_6 is non-uniform, the crystalline grain exhibit different shape and dimension, however, the crystalline grain of CaNaCr(IV)TaO_6 and SrNaCr(IV)TaO_6 exhibit regular shape and dimension. TGA analysis displays a loss-step is observed at high temperature under 10%H2-Ar atmosphere, which is attributed to the reduction of Fe~(4+) or Cr~(4+). Magnetic property study indicates that CaNaFe(IV)TaO_6, CaNaCr(IV)TaO_6 and SrNaCr(IV)TaO_6 are soft magnets, while SrNaFe(IV)TaO_6 is hard magnet..
Perovskite complex mental oxides have attracted more and more attention due to their complicated magnetic and electrical properties. In recent decades, various methods have been used to prepare A-doped or B-doped Perovskite complex metal oxides, such as conventional solid state reaction, sol-gel technique, hydrothermal technique, coprecipitation method, pulsed laser technique and self-propagating high-temperature synthesis. Many powder, film or single crystal materials were obtained by exchanging the doped element or varying the content of doped element in perovskite complex mental oxides. So far, however, there is not comprehensive conclusion about the physical and chemical properties of perovskite complex mental oxides, and some phenomenon is still in doubt. In view of the great value and study scope of these materials, more and more researchers are indulging in the study of perovskites.
There are many new perovskites, double perovskites and their doped metal oxides, however, most of them are focused on the easily prepared oxides, such as manganese-based complex oxides and molybdenum-based complex oxides. The reports about difficultly prepared oxides are very rare. For example, due to the volatility of Na, there are little reports about Na-doped perovskites. It is difficult to obtain pure Fe(IV)-doped or Cr(IV)-doped perovskites, and the Fe(IV)-doped or Cr(IV)-doped perovskites are unstable, which makes people unwilling to study these oxides. In view of the reasons mentioned above, we have prepared eight Na-containing perovskite complex metal oxides through conventional solid state reaction. Besides, we introduce Fe(IV) or Cr(IV) into these Na-containing oxides, which are not reported previously.
1. We have synthesized four novel double perovskites containing Na+ of LaNaFe(Ⅲ)TaO_6、LaNaFe(Ⅲ)NbO_6、LaNaMn(Ⅲ)TaO_6、LaNaMn(Ⅲ)NbO_6 through conventional solid state reaction. XRD analysis displays that all compounds have high degree of crystallization. SEM shows that the microstructure of these compounds is irregular, the crystalline grain exhibit different shape and dimension. TGA analysis displays all compounds are stable below 1000 oC at 10%H2-Ar atmosphere. Magnetic property test indicates that LaNaFe(Ⅲ)TaO_6 and LaNaFe(Ⅲ)NbO_6 contain weak ferromagnetic component,while LaNaMn(Ⅲ)TaO_6 and LaNaMn(Ⅲ)NbO_6 are soft magnets.
2. With the goal of introducing Na+ and Fe~(4+) or Cr~(4+) into the same compound, we have synthesized four novel double perovskites of CaNaFe(IV)TaO_6、SrNaFe(IV)TaO_6、CaNaCr(IV)TaO_6、SrNaCr(IV)TaO_6. XRD analysis displays that all compounds have high degree of crystallization. SEM shows that the microstructure of CaNaFe(IV)TaO_6 and SrNaFe(IV)TaO_6 is non-uniform, the crystalline grain exhibit different shape and dimension, however, the crystalline grain of CaNaCr(IV)TaO_6 and SrNaCr(IV)TaO_6 exhibit regular shape and dimension. TGA analysis displays a loss-step is observed at high temperature under 10%H2-Ar atmosphere, which is attributed to the reduction of Fe~(4+) or Cr~(4+). Magnetic property study indicates that CaNaFe(IV)TaO_6, CaNaCr(IV)TaO_6 and SrNaCr(IV)TaO_6 are soft magnets, while SrNaFe(IV)TaO_6 is hard magnet..
引文
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