R. Köferstein, T. Walther, D. Hesse, S. Ebbinghaus
{"title":"淀粉-凝胶法制备纳米铁氧体镁粉体及其陶瓷表征","authors":"R. Köferstein, T. Walther, D. Hesse, S. Ebbinghaus","doi":"10.2139/ssrn.3206736","DOIUrl":null,"url":null,"abstract":"The synthesis and characterization of nano-sized MgFe2O4 by a starch-gel method is described herein. A phase-pure nano-sized MgFe2O4 powder (1a) was obtained after calcining a (MgFe) starch gel at 550 °C. The powder has a specific surface area of 60.6 m2/g and a crystallite size of 9 nm. TEM investigations reveal particles in the range of 7 to 15 nm. The activation energy of the crystallite growth process was calculated as 89 ± 14 kJ/mol. The shrinkage and sintering behaviour of resulting compacts were studied. UV−VIS investigations of the nano-sized powder 1a reveal an optical band gap of 2.38 eV, whereas calcination at 1100 °C (powder 1g) leads to a crystallite size of 129 nm and a band gap of 2.16 eV. Magnetization loops at 300 K and the temperature dependence of both the field-cooled (FC) and the zero-field-cooled (ZFC) agnetization indicate a superparamagnetic behaviour. The blocking temperature for powder 1a was determined as 140 K at a field of H = 500 Oe. We found different saturation magnetizations (Ms) depending on the calcination temperature. Calcination at 550 °C (1a) results in Ms = 20.0 emu/g which increases with calcination temperature to a maximum of 37.7 emu/g for powder 1e calcined at 900 °C. Ceramic bodies sintered between 1450 and 1600 °C exhibit Ms values of 25−28 emu/g. Magnetic investigations at 10 K on powders 1a−1g show hysteresis loops with coercivities up to 950 Oe, remanences to 10 emu/g and Ms values to 50.4 emu/g. Additionally, the nano-scaled powders show a shift of the hysteresis loops.","PeriodicalId":399389,"journal":{"name":"Inorganic Chemistry eJournal","volume":"77 1","pages":"0"},"PeriodicalIF":0.0000,"publicationDate":"2013-10-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Preparation and Characterization of Nano-Sized Magnesium Ferrite Powders By a Starch-Gel Process and Corresponding Ceramics\",\"authors\":\"R. Köferstein, T. Walther, D. Hesse, S. Ebbinghaus\",\"doi\":\"10.2139/ssrn.3206736\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"The synthesis and characterization of nano-sized MgFe2O4 by a starch-gel method is described herein. A phase-pure nano-sized MgFe2O4 powder (1a) was obtained after calcining a (MgFe) starch gel at 550 °C. The powder has a specific surface area of 60.6 m2/g and a crystallite size of 9 nm. TEM investigations reveal particles in the range of 7 to 15 nm. The activation energy of the crystallite growth process was calculated as 89 ± 14 kJ/mol. The shrinkage and sintering behaviour of resulting compacts were studied. UV−VIS investigations of the nano-sized powder 1a reveal an optical band gap of 2.38 eV, whereas calcination at 1100 °C (powder 1g) leads to a crystallite size of 129 nm and a band gap of 2.16 eV. Magnetization loops at 300 K and the temperature dependence of both the field-cooled (FC) and the zero-field-cooled (ZFC) agnetization indicate a superparamagnetic behaviour. The blocking temperature for powder 1a was determined as 140 K at a field of H = 500 Oe. We found different saturation magnetizations (Ms) depending on the calcination temperature. Calcination at 550 °C (1a) results in Ms = 20.0 emu/g which increases with calcination temperature to a maximum of 37.7 emu/g for powder 1e calcined at 900 °C. Ceramic bodies sintered between 1450 and 1600 °C exhibit Ms values of 25−28 emu/g. Magnetic investigations at 10 K on powders 1a−1g show hysteresis loops with coercivities up to 950 Oe, remanences to 10 emu/g and Ms values to 50.4 emu/g. Additionally, the nano-scaled powders show a shift of the hysteresis loops.\",\"PeriodicalId\":399389,\"journal\":{\"name\":\"Inorganic Chemistry eJournal\",\"volume\":\"77 1\",\"pages\":\"0\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2013-10-02\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Inorganic Chemistry eJournal\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.2139/ssrn.3206736\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Inorganic Chemistry eJournal","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.2139/ssrn.3206736","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
Preparation and Characterization of Nano-Sized Magnesium Ferrite Powders By a Starch-Gel Process and Corresponding Ceramics
The synthesis and characterization of nano-sized MgFe2O4 by a starch-gel method is described herein. A phase-pure nano-sized MgFe2O4 powder (1a) was obtained after calcining a (MgFe) starch gel at 550 °C. The powder has a specific surface area of 60.6 m2/g and a crystallite size of 9 nm. TEM investigations reveal particles in the range of 7 to 15 nm. The activation energy of the crystallite growth process was calculated as 89 ± 14 kJ/mol. The shrinkage and sintering behaviour of resulting compacts were studied. UV−VIS investigations of the nano-sized powder 1a reveal an optical band gap of 2.38 eV, whereas calcination at 1100 °C (powder 1g) leads to a crystallite size of 129 nm and a band gap of 2.16 eV. Magnetization loops at 300 K and the temperature dependence of both the field-cooled (FC) and the zero-field-cooled (ZFC) agnetization indicate a superparamagnetic behaviour. The blocking temperature for powder 1a was determined as 140 K at a field of H = 500 Oe. We found different saturation magnetizations (Ms) depending on the calcination temperature. Calcination at 550 °C (1a) results in Ms = 20.0 emu/g which increases with calcination temperature to a maximum of 37.7 emu/g for powder 1e calcined at 900 °C. Ceramic bodies sintered between 1450 and 1600 °C exhibit Ms values of 25−28 emu/g. Magnetic investigations at 10 K on powders 1a−1g show hysteresis loops with coercivities up to 950 Oe, remanences to 10 emu/g and Ms values to 50.4 emu/g. Additionally, the nano-scaled powders show a shift of the hysteresis loops.