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haidaochi

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[求助] 热分解法制备四氧化三铁

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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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
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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阳光西骑士

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nuaajsh(金币+1): 鼓励交流 2011-06-16 23:02:39
很多篇合成油酸铁都是采用的这个方法,我第一步用的是烧杯,不过合成的油酸铁是红棕色的……
3楼2011-05-06 23:51:15
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haidaochi

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我的也是啊,请问你合成出来的铁是纯相么?
4楼2011-05-06 23:59:22
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haidaochi

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引用回帖:
Originally posted by 阳光西骑士 at 2011-05-06 23:51:15:
很多篇合成油酸铁都是采用的这个方法,我第一步用的是烧杯,不过合成的油酸铁是红棕色的……

我的也是啊,请问你合成出来的铁是纯相么? 我用的是sun的方法。
5楼2011-05-06 23:59:52
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阳光西骑士

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不好意思我这两天刚做的这个实验,只做到油酸铁,第二步还没做,正准备做呢
6楼2011-05-07 00:15:02
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阳光西骑士

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nuaajsh(金币+1): 鼓励交流 2011-06-16 23:02:59
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
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greattom365

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【答案】应助回帖

haidaochi(金币+1): 2011-05-24 08:50:21
!!!到外文网站搜资料
不求有功但求无过
8楼2011-05-07 00:51:11
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refnew

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【答案】应助回帖

haidaochi(金币+1): 2011-05-16 23:05:46
你连油酸铁都没合成出来,
9楼2011-05-07 09:42:25
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haidaochi

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引用回帖:
Originally posted by refnew at 2011-05-07 09:42:25:
你连油酸铁都没合成出来,

我合成出油酸铁了啊
10楼2011-05-07 11:42:25
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