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cuiguanwei

金虫 (正式写手)

院士

[求助] 表征一个微米级核壳结构,如何得到断面?

做了一个短棒状核壳结构材料,直径2微米,长8微米,因没法表征核壳结构,我想把棒切断了,用SEM表征断面,可是研磨效果不好,这个材料非常脆,全碎了,看不到断面,请教各位如何制造一个平整好看的断面啊?谢谢啦!
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jackycj

铁杆木虫 (知名作家)

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感谢参与,应助指数 +1
cuiguanwei: 金币+4, ★★★很有帮助, 谢谢,我这个材料不能用强的电子束打,一打就熔化,我用环氧树脂包埋切片吧!SEM可以吗? 2012-06-29 09:10:35
至少有两种方案可供选择:
1. 将所制得的样品包埋在环氧树脂(Epoxy resin)中,固化后用玻璃刀切片,然后在透射电镜(TEM)下观察;
2. 将样品粘在扫描电镜(SEM)样品托上,用聚焦离子束/电子束进行切割,可以得到很好的断面,然后再在扫描电镜下观察。
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5楼2012-06-28 18:25:56
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jackycj

铁杆木虫 (知名作家)

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cuiguanwei: 金币+10, ★★★★★最佳答案, 5 2012-06-29 23:28:40
tt.yao: 回帖置顶 2012-08-24 14:28:00
请详见JOURNAL OF APPLIED PHYSICS VOLUME 95, NUMBER 12 15 JUNE 2004, pp8097-8110. Artificial dielectric properties of microscopic metallized rodlike bacteria cells in composites.  
论文叙述了金属化杆菌在环氧树脂中分散以及固化工艺,具体如下面英文所示。主要参考环氧树脂组成、牌号以及固化条件。你做包埋时不需要对样品分散分散,直接拿牙签蘸一些你的样品干粉,混在小离心管内的环氧树脂底部即可(方便将来切片),然后固化。将固化后的样品拿到测试分析实验师那边让老师帮你切片,由于切片非常薄,SEM不太方便取样观察,建议使用透射电镜(TEM)。
The metallized bacteria were rinsed with distilled water and dehydrated in an alcohol series, then dispersed in acetone and suspended therein to be used for composite formation. The concentration of metallized bacteria in organic solvent
suspension was determined by drying and weighing an aliquot of the mixture. The metallized bacteria were cast in epoxy by adding the bacteria/acetone slurry to the epoxy resin, Epon 812. This mixture was vigorously stirred by hand
for several minutes to make them more homogeneous, removing the acetone by rotary evaporation in vacuum for about 2 h. Then the curing agent ~DDSA!, solidifying agent ~Methylnadic anhydride!, and accelerator agent ~2-4-6 Tris
Phenol! were added in proportion and mixed for another 10 min. The concentrations of metallized bacteria cells in the composites varied from 5 to 20 vol %. The composites were then poured into tubules and placed in a vacuum oven for degassing for 1 h, after which the samples were
placed in a thermotank and allowed to cure at 60 °C for 24–36 h. The samples were removed from the molds after full cure and machined to sizes suitable for dielectric measurement.
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9楼2012-06-29 16:36:09
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jackycj

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cuiguanwei: 金币+2, ★★★很有帮助 2012-06-29 23:30:18
直白点的,如下:
金属化微生物细胞经乙醇系列脱水后,倒入已经配制好的树脂中(树脂配方如表所示),手动搅拌均匀,静置4~6小时,令其充分浸润。在60oC条件下固化24~36小时。
表5.2  粘结剂——树脂的组成
树脂        Epon812        DDSA(固化剂)        MNA(硬化剂)        DMP-30(加速剂)
10ml        4.5 ml        3.0 ml        2.5 ml        0.1 ml
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10楼2012-06-29 16:41:12
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