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haidaochi木虫 (正式写手)
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[求助]
热分解法制备四氧化三铁
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请教大家一个问题： 热分解法制备四氧化三铁时候，油酸铁和溶剂的比例是多少啊，为什么我每次做出的磁性粒子都有杂质啊。就是xrd有很多杂峰。 |
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 四氧化三铁纳米颗粒制备、修饰及包覆 |
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阳光西骑士
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【答案】应助回帖
haidaochi(金币+2): 2011-05-07 08:19:19
haidaochi(金币+1): 2011-05-07 23:18:04
haidaochi(金币+1): 2011-05-17 09:35:48
haidaochi(金币+3): 2011-05-24 08:50:01
haidaochi(金币+1): 2011-05-07 23:18:04
haidaochi(金币+1): 2011-05-17 09:35:48
haidaochi(金币+3): 2011-05-24 08:50:01
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参考这篇文献试试 Ultra-large-scale syntheses of monodisperse nanocrystals JONGNAM PARK1, KWANGJIN AN1, YOSUN HWANG2, JE-GEUN PARK2, HAN-JIN NOH3, JAE-YOUNG KIM3, JAE-HOON PARK3, NONG-MOON HWANG4 AND TAEGHWAN HYEON1* 1National Creative Research Center for Oxide Nanocrystalline Materials and School of Chemical Engineering, Seoul National University, Seoul 151-744, Korea 2Department of Physics and Institute of Basic Science, Sungkyunkwan University, Suwon 440-746, Korea 3Department of Physics and Pohang Light Source, Pohang University of Science and Technology, Pohang 790-784, Korea 4School of Materials Science & Engineering and Nano-Systems Institute (NSI-NCRC), Seoul National University, Seoul 151-744, Korea *e-mail: thyeon@plaza.snu.ac.kr 下面是合成过程 SYNTHESIS OF IRON–OLEATE COMPLEX The metal–oleate complex was prepared by reacting metal chlorides and sodium oleate. In a typical synthesis of iron–oleate complex, 10.8 g of iron chloride (FeCl3·6H2O, 40 mmol, Aldrich, 98%) and 36.5 g of sodium oleate (120 mmol, TCI, 95%) was dissolved in a mixture solvent composed of 80 ml ethanol, 60 ml distilled water and 140 ml hexane. The resulting solution was heated to 70 °C and kept at that temperature for four hours. When the reaction was completed, the upper organic layer containing the iron–oleate complex was washed three times with 30 ml distilled water in a separatory funnel. After washing, hexane was evaporated off, resulting in iron–oleate complex in a waxy solid form. SYNTHESIS OF IRON OXIDE NANOCRYSTALS The following is a typical synthetic procedure for monodisperse iron oxide (magnetite) nanocrystals with a particle size of 12 nm. 36 g (40 mmol) of the iron-oleate complex synthesized as described above and 5.7 g of oleic acid (20 mmol, Aldrich, 90%) were dissolved in 200 g of 1-octadecene (Aldrich, 90%) at room temperature. The reaction mixture was heated to 320 °C with a constant heating rate of 3.3 °C min–1, and then kept at that temperature for 30 min. When the reaction temperature reached 320 °C, a severe reaction occurred and the initial transparent solution became turbid and brownish black. The resulting solution containing the nanocrystals was then cooled to room temperature, and 500 ml of ethanol was added to the solution to precipitate the nanocrystals. The nanocrystals were separated by centrifugation. |
2楼2011-05-06 23:49:32
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3楼2011-05-06 23:51:15
haidaochi
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4楼2011-05-06 23:59:22
haidaochi
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5楼2011-05-06 23:59:52
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6楼2011-05-07 00:15:02
阳光西骑士
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★
nuaajsh(金币+1): 鼓励交流 2011-06-16 23:02:59
nuaajsh(金币+1): 鼓励交流 2011-06-16 23:02:59
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http://muchong.com/bbs/viewthread.php?tid=2879676&fpage=1 这里也有个讨论你问题的帖子 可以看下 |
7楼2011-05-07 00:16:34
greattom365
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8楼2011-05-07 00:51:11
refnew
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9楼2011-05-07 09:42:25
haidaochi
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10楼2011-05-07 11:42:25
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