氧分压对铁铝尖晶石稳定性的影响
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摘要
将烧结铁铝尖晶石制成1.0~0.088 mm样品,控制气氛中氧气体积分数,进行25~1 400℃的热重分析,研究不同含氧分压下铁铝尖晶石的氧化行为,并对氧化前后样品进行X射线衍射、扫描电子显微镜及能谱分析。结果表明:烧结铁铝尖晶石的氧化为保护型氧化,气氛中氧气体积分数在0.3%左右时,铁铝尖晶石较为稳定,晶粒表面氧化形成排列规整致密的刚玉及赤铁矿致密保护层,内部未氧化;氧气体积分数在8.0%左右时,铁铝尖晶石完全氧化,产生片状、粒状的刚玉相及赤铁矿相;氧气体积分数在18.0%左右时,样品中残留较多纯净铁铝尖晶石相,铁铝尖晶石晶粒表面氧化形成无定形刚玉及赤铁矿相,氧化程度较为剧烈,晶粒保留八面体结构。
A sintered hercynite powder with the sizes of 1.0–0.088 mm was prepared via grinding. The oxidation behavior of the sintered hercynite powder at different oxygen volume fractions was investigated through the thermogravimetric analysis at 25– 1 400 ℃. The fired samples were characterized by X-ray diffraction, scanning electron microscopy and energy dispersive spectrometry, respectively. The results show that the oxidation of sintered hercynite is protective oxidation. When the oxygen volume fraction is 0.3%, hercynite is more relatively stable and there are some dense and regular arrangement phases of corundum and hematite on the grain surface as a protective layer, and the inside of the grains is not oxidized. When the oxygen volume fraction is 8.0%, hercynite is completely oxidized to form flaky and grainy phases of corundum and hematite. When the oxygen volume fraction is 18.0%, there are some residual pure hercynite phases existed in the specimen, the surface of hercynite grains is oxidized to form some shapelessness phases of corundum and hematite. The oxidization is more serious and the grains are still in an octahedral structure.
A sintered hercynite powder with the sizes of 1.0–0.088 mm was prepared via grinding. The oxidation behavior of the sintered hercynite powder at different oxygen volume fractions was investigated through the thermogravimetric analysis at 25– 1 400 ℃. The fired samples were characterized by X-ray diffraction, scanning electron microscopy and energy dispersive spectrometry, respectively. The results show that the oxidation of sintered hercynite is protective oxidation. When the oxygen volume fraction is 0.3%, hercynite is more relatively stable and there are some dense and regular arrangement phases of corundum and hematite on the grain surface as a protective layer, and the inside of the grains is not oxidized. When the oxygen volume fraction is 8.0%, hercynite is completely oxidized to form flaky and grainy phases of corundum and hematite. When the oxygen volume fraction is 18.0%, there are some residual pure hercynite phases existed in the specimen, the surface of hercynite grains is oxidized to form some shapelessness phases of corundum and hematite. The oxidization is more serious and the grains are still in an octahedral structure.
引文
[1]陈肇友.水泥回转窑烧成带用无铬耐火材料[J].耐火材料,2010,44(6):404–408.CHEN Zhaoyou.Refractories(in Chinese),2010,44(6):404–408.
[2]HARRISON R J,REDFERN S A T,O’NEILL H S C.The temperature dependence of the cation distribution in synthetic hercynite(Fe Al2O4)from in-situ neutron structure refinements[J].Am Mine,1998,83:1092–1099.
[3]ANDREOZZI G B,LUCCHESI S.Intersite distribution of Fe2+and Mg in the spinel(sensu stricto)–hercynite series by single-crystal X-ray diffraction[J].Am Miner,2002,87:1113–1120.
[4]HILL R J.X-ray powder diffraction profile refinement of synthetic hercynite[J].Am Miner,1984,69:937–942.
[5]CHEN J H,YU L Y,SUN J L,et al.Synthesis of hercynite by reaction sintering[J].J Eur Ceram Soc,2011(31):259–263.
[6]陆兆鑫,李志坚,吴锋,等.不同氧化铝源对合成铁铝尖晶石稳定性的影响[J].人工晶体学报,2015,44(5):1320–1324.LU Zhaoxin,LI Zhijian,WU Feng,et al.J Synth Cryst(in Chinese),2015,44(5):1320–1324.
[7]马淑龙,李勇,孙加林,等.氮气气氛下铁铝尖晶石的合成[J].硅酸盐学报,2011,39(2):424–429.MA Sulong,LI Yong,SUN Jialin,et al.J Chin Ceram Soc,2011,39(2):424–429.
[8]马淑龙,李勇,孙加林,等.添加Mg O对铁铝尖晶石合成和烧结的影响[J].耐火材料,2010,44(5):334–337.MA Sulong,LI Yong,SUN Jialin,et al.Refractories(in Chinese),2010,44(5):334–337.
[9]杨斌,顾华志,汪厚植.原位合成方镁石–铁铝尖晶石材料的烧结工艺及性能研究[J].武汉科技大学学报,2009,32(1):86–89.YANG Bin,GU Huazhi,WANG Houhzhi.J Wuhan Univ Sci Technol(in Chinese),2009,32(1):86–89.
[10]刘会林,沈卫平,李勇.铁铝尖晶石料的烧结合成[J].耐火材料,2003,6:333–335.LIU Huilin,SHEN Weiping,LI Yong.Refractories(in Chinese),2003,6:333–335.
[11]杨斌,顾华志,汪厚植.原位合成方镁石–铁铝尖晶石材料[J].稀有金属材料与工程,2009,38(2):1229–1232.YANG Bin,GU Huazhi,WANG Houzhi.Rare Met Mater Eng(in Chinese),2009,38(2):1229–1232.
[12]FREER R,O’REILY W.The diffusion of Fe2+ions in spinels with relevance to the process of maghemitization[J].Miner Mag,1980,43(9):889–899.
[13]SCHOLLENBRUCH K,WOODLAND A B,FROST D J.The stability of hercynite at high pressures and temperatures[J].Phys Chem Miner,2010,37:137–143.
[14]PETUSKEY W T,BOWEN H K.Thermal segregation of cations in iron aluminate spinels[J].J Am Ceram Soc,1981,64(10):611–617.
[15]KLEMME S,MILTENBURG J C V.Thermodynamic properties of hercynite(Fe Al2O4)based on adiabatic calorimetry at low temperatures[J].Am Miner,2003,88:68–72.
[16]LAVINA B,PRINCIVALLE F,GIUSTA A D.Controlled time–temperature oxidation reaction in a synthetic Mg–hercynite[J].Phys Chem Miner,2005,32:83–88.
[2]HARRISON R J,REDFERN S A T,O’NEILL H S C.The temperature dependence of the cation distribution in synthetic hercynite(Fe Al2O4)from in-situ neutron structure refinements[J].Am Mine,1998,83:1092–1099.
[3]ANDREOZZI G B,LUCCHESI S.Intersite distribution of Fe2+and Mg in the spinel(sensu stricto)–hercynite series by single-crystal X-ray diffraction[J].Am Miner,2002,87:1113–1120.
[4]HILL R J.X-ray powder diffraction profile refinement of synthetic hercynite[J].Am Miner,1984,69:937–942.
[5]CHEN J H,YU L Y,SUN J L,et al.Synthesis of hercynite by reaction sintering[J].J Eur Ceram Soc,2011(31):259–263.
[6]陆兆鑫,李志坚,吴锋,等.不同氧化铝源对合成铁铝尖晶石稳定性的影响[J].人工晶体学报,2015,44(5):1320–1324.LU Zhaoxin,LI Zhijian,WU Feng,et al.J Synth Cryst(in Chinese),2015,44(5):1320–1324.
[7]马淑龙,李勇,孙加林,等.氮气气氛下铁铝尖晶石的合成[J].硅酸盐学报,2011,39(2):424–429.MA Sulong,LI Yong,SUN Jialin,et al.J Chin Ceram Soc,2011,39(2):424–429.
[8]马淑龙,李勇,孙加林,等.添加Mg O对铁铝尖晶石合成和烧结的影响[J].耐火材料,2010,44(5):334–337.MA Sulong,LI Yong,SUN Jialin,et al.Refractories(in Chinese),2010,44(5):334–337.
[9]杨斌,顾华志,汪厚植.原位合成方镁石–铁铝尖晶石材料的烧结工艺及性能研究[J].武汉科技大学学报,2009,32(1):86–89.YANG Bin,GU Huazhi,WANG Houhzhi.J Wuhan Univ Sci Technol(in Chinese),2009,32(1):86–89.
[10]刘会林,沈卫平,李勇.铁铝尖晶石料的烧结合成[J].耐火材料,2003,6:333–335.LIU Huilin,SHEN Weiping,LI Yong.Refractories(in Chinese),2003,6:333–335.
[11]杨斌,顾华志,汪厚植.原位合成方镁石–铁铝尖晶石材料[J].稀有金属材料与工程,2009,38(2):1229–1232.YANG Bin,GU Huazhi,WANG Houzhi.Rare Met Mater Eng(in Chinese),2009,38(2):1229–1232.
[12]FREER R,O’REILY W.The diffusion of Fe2+ions in spinels with relevance to the process of maghemitization[J].Miner Mag,1980,43(9):889–899.
[13]SCHOLLENBRUCH K,WOODLAND A B,FROST D J.The stability of hercynite at high pressures and temperatures[J].Phys Chem Miner,2010,37:137–143.
[14]PETUSKEY W T,BOWEN H K.Thermal segregation of cations in iron aluminate spinels[J].J Am Ceram Soc,1981,64(10):611–617.
[15]KLEMME S,MILTENBURG J C V.Thermodynamic properties of hercynite(Fe Al2O4)based on adiabatic calorimetry at low temperatures[J].Am Miner,2003,88:68–72.
[16]LAVINA B,PRINCIVALLE F,GIUSTA A D.Controlled time–temperature oxidation reaction in a synthetic Mg–hercynite[J].Phys Chem Miner,2005,32:83–88.