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Preparation of ceria with large particle size and high appearance density¡£Cerium is one of the most abundant rare earth elements in both bastnasite and monazite. Ceria has been widely used in optical, catalytic, electrolyte, and sensor materials, with unique performances. With the development of functional materials, great interest has been focused on the synthesis and characterization of specific fine/mesoporous ceria powder. In this study, the modified precipitation and recrystallization processes combined with a controlled calcination process for fabricating the ceria with large particle size and high appearance density was reported. Dunng precipitation, a certain amount of mineral acid such as nitric acid served as an additive, to adjust the precipitation and crystallization processes of cerium oxalates. An appropriate acidic condition could lead the process into the Oswald ripening stage and made the particles become bigger. Thus, the appearance density of powder was increased. The optimized conditions, such as the temperature, feeding speed. type and concentration of mineral acids, and the concentration of cerium-contained stock solution, were investigated and evaluated. Rare earth oxalate eluted or immersed with mineral acid could act as a precursor, to obtain an oxide with large particle size and high appearance density, by decomposition in controlled calcinations, in which the moisture must be gradually released first. The treatment of precipitates and the calcination process could affect the particle size distribution and appearance density. The optimized condition approached in this study is: (1) To increase the particle size and appearance density, the solution of nitric acid (5 mol/L) and oxalic acid (1 0 g/L) can be used as an eluent or immersing reagent. (2) The programmed calcination process is necessary, that is, heating the as-elutedhmmersed oxalates mildly from room temperature to 300¡æat a heating rate of 5¡æ/min, and keeping the samples at 300 "C for 1 h; consecutively, heating to 900¡æat 10¡æ/min, and then keeping for 4 h. After the above-mentioned optimization process, the particle size and appearance density of ceria could reach 20 pm and 1.9 g/cm3, respectively. This method could also be applied to prepare praseodymium oxides, however, it was not successful in preparing other light rare earth oxides. Compared with other processes, this study provided a facile strategy with low cost. |
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С¼×009(½ð±Ò+85,VIP+0): 11-25 14:43
С¼×009(½ð±Ò+85,VIP+0): 11-25 14:43
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Preparation of ceria with large particle size and high appearance density¡£ ´óÁ£¶È£¬¸ß±í¹Û±ÈÖØÑõ»¯îæµÄºÏ³É¡£ Cerium is one of the most abundant rare earth elements in both bastnasite and monazite. îæÔªËØÔÚ·úÌ¼îæ¿óºÍ¶À¾Óʯ¿óÖÐÌìÈ»·á¶ÈºÜ¸ß¡£ Ceria has been widely used in optical, catalytic, electrolyte, and sensor materials, with unique performances. Ñõ»¯²§Òѱ»¹ã·ºÓ¦ÓÃÓÚ¹âѧ¡¢´ß»¯¡¢µç½âÖÊ¡¢´«¸ÐÆ÷²ÄÁÏÖУ¬¾ßÓжÀÌØµÄÐÔÄÜ¡£ With the development of functional materials, great interest has been focused on the synthesis and characterization of specific fine/mesoporous ceria powder. Ëæ×Ź¦ÄܲÄÁϵIJ»¶Ï·¢Õ¹£¬¸÷ÖÖÌØÊâÎïÀíÐÔÄܵÄÑõ»¯²§·ÛÌåµÄºÏ³ÉºÍÐÔÄܱíÕ÷Ñо¿Ê®·Ö»îÔ¾ In this study, the modified precipitation and recrystallization processes combined with a controlled calcination process for fabricating the ceria with large particle size and high appearance density was reported. ±¾ÎÄÖУ¬±¨µÀÁËÒ»ÖÖ¶Ô³Áµí¹ý³ÌºÍ½á¾§¹ý³ÌµÄÓÅ»¯ÒÔ¼°¶ÔÉÕ½á¹ý³ÌµÄ¿ØÖÆÀ´ÖƱ¸´óÁ£¶È£¬¸ß±íÃæ±ÈÖØµÄÑõ»¯îæ·ÛÌå¡£ Dunng precipitation, a certain amount of mineral acid such as nitric acid served as an additive, to adjust the precipitation and crystallization processes of cerium oxalates. ³Áµí¹ý³ÌÖУ¬ÒÔÒ»¶¨ÊýÁ¿µÄ¿óÎïËáÈçÏõËá×÷ΪÌí¼Ó¼Á£¬À´µ÷Õû²ÝËáîæµÄ³ÁµíºÍ½á¾§¹ý³Ì¡£ An appropriate acidic condition could lead the process into the Oswald ripening stage and made the particles become bigger. Thus, the appearance density of powder was increased. Êʵ±µÄËáÐÔÌõ¼þ½«ÓÐÖúÓÚʹ·´Ó¦¹ý³ÌÇ÷ÏòOsward½á¾§½×¶Î£¬²¢Ê¹µÃÁ£×Ó±ä´ó¡£Òò´Ë£¬·ÛÌåµÄ±í¹Û±ÈÖØ»áÌá¸ß¡£ The optimized conditions, such as the temperature,feeding speed. type and concentration of mineral acids, and the concentration of cerium-contained stock solution, were investigated and evaluated. Ñо¿ºÍÆÀ¹ÀÁËÓÅ»¯µÄ·´Ó¦Ìõ¼þ£¬±ÈÈçζȣ¬¼ÓËáËÙ¶È£¬¿óÎïËáµÄÖÖÀàºÍŨ¶Èº¬îæÈÜÒºµÄŨ¶ÈµÈ¡£ Rare earth oxalate eluted or immersed with mineral acid could act as a precursor, to obtain an oxide with large particle size and high appearance density, by decomposition in controlled calcinations, in which the moisture must be gradually released first. ΪÁË»ñµÃ´óÁ£¶ÈºÍ¸ß±í¹Û±ÈÖØµÄÑõ»¯ÎϡÍÁ²ÝËáÑÎÏ´Ìá»ò½þÈë¿óÎïËὫ¿ÉÒԳ䵱ǰÇýÌ壬ÔÚ¿ØÖÆÉÕ½áÌõ¼þÏ·ֽ⣬ÕâÀïÊªÆøÊ×ÏÈÐèÒªÖð½¥ÅÅ·Å¡£ The treatment of precipitates and the calcination process could affect the particle size distribution and appearance density. ¶Ô³ÁµíÎïµÄ´¦ÀíºÍÉÕ½á¹ý³ÌµÄ¿ØÖƽ«»áÓ°Ïìµ½Á£×ӵij߶ȷֲ¼ºÍ±í¹Û±ÈÖØ¡£ The optimized condition approached in this study is: ±¾ÎÄÓÅ»¯µÄÌõ¼þºÍ·½·¨ÈçÏ£º (1) To increase the particle size and appearance density, the solution of nitric acid (5 mol/L) and oxalic acid (1 0 g/L) can be used as an eluent or immersing reagent. ΪÁËÌá¸ßÁ£¶ÈºÍ±í¹Û±ÈÖØ£¬5mol/LµÄÏõËáºÍ10g/LµÄ²ÝËá»ìºÏ³äµ±ÁÜÏ´Òº»ò½þÅÝ·´Ó¦Îï¡£ (2) The programmed calcination process is necessary, that is, heating the as-elutedhmmersed oxalates mildly from room temperature to 300¡æat a heating rate of 5¡æ/min, and keeping the samples at 300 "C for 1 h; consecutively, heating to 900¡æat 10¡æ/min, and then keeping for 4 h. After the above-mentioned optimization process, the particle size and appearance density of ceria could reach 20 pm and 1.9 g/cm3, respectively. ³Ì¿ØµÄÉÕ½á¹ý³ÌÊDZØÐëµÄ£¬Õâ¾ÍÊÇ£¬°´5¶È/·ÖÖÓÖð²½¼ÓÈȰ´ÕâÖÖÁÜÏ´ÖÆ±¸µÄ²ÝËáÑε½300¶È£¬±£ÎÂ1Сʱ£»½Ó×Å£¬°´10¶È/·ÖÖÓ¼ÓÈȵ½900¶È£¬±£ÎÂ4Сʱ¡£¾¹ýÉÏÊöÓÅ»¯¹ý³ÌÒÔºó£¬Ñõ»¯îæµÄÁ£¶ÈºÍ±í¹Û±ÈÖØ·Ö²¼´ïµ½20 pmºÍ1.9 g/cm3¡£ This method could also be applied to prepare praseodymium oxides, however, it was not successful in preparing other light rare earth oxides. Compared with other processes, this study provided a facile strategy with low cost. ÕâÖÖ·½·¨¿ÉÒÔÓ¦Óõ½ÖƱ¸Ñõ»¯ï裬µ«ÊÇ£¬ÎÞ·¨³É¹¦Ó¦Óõ½ÖƱ¸ÆäËûÇáÏ¡ÍÁÑõ»¯Îï¡£ºÍÆäËû·½·¨±È½Ï£¬ÕâÖÖ·½·¨²Ù×÷¼òµ¥£¬³É±¾µÍÁ®¡£ |
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3Â¥2009-11-22 13:16:56
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С¼×009(½ð±Ò+5,VIP+0): 11-25 14:43
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ɳ·¢ºÃÇ¿°¡£¡£¡µ«ÊÇÓÐЩµØ·½¿ÉÄܲ»Ì«¾«È· µÚÎå¾ä»°£º In this study, the modified precipitation and recrystallization processes combined with a controlled calcination process for fabricating the ceria with large particle size and high appearance density was reported. modified precipitation ¡ª¡ª¸ÄÐÔ³Áµí recrystallization processes ¡ª¡ªÔٽᾧ¹ý³Ì ¸öÈ˾õµÃÕâÀï ÊÇ : ±¨µ¼ÁËÒ»ÖÖ Óë¿ØÖÆÉÕ½á´óÁ£¶È£¬¸ß±íÃæ±ÈÖØµÄÑõ»¯îæµÄ¹ý³Ì Ïà½áºÏµÄ¸ÄÐÔ³ÁµíÓëÔٽᾧ¹ý³Ì¡£ |

4Â¥2009-11-24 08:45:29
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