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3. Results and discussion 3.1. FTIR analysis FTIR spectra are commonly employed to identify the change of characteristic groups. Fig. 1 presented the FTIR spectra of PAL samples. It could be seen that the absorption bands at 1030 and 983 cm−1 were ascribed to the Si\O stretching vibrations [22], and the absorption bands at 519 and 478 cm−1 were attributed to the Si\O bending vibrations. The bands at 3411 and 1646 cm−1 were assigned to the characteristic O\H stretching and H\O\H bending vibration of the coordinated and adsorbed water in PAL samples, respectively. The broad bands at 3621–3543 cm−1 were ascribed to the stretching vibrations of (Al)O\H and (Mg)O\H bonds. As could be seen from Fig. 1, compared with the spectrum of PAL-0, for PAL-6, the absorption bands (1030 and 983 cm−1) became blunt and the strength reduced. And there were no other obvious differences among the characteristic absorption bands of PAL samples.3.2. FESEM analysis The FESEM micrographs of PAL-0, PAL-4, PAL-6 and PAL-8 were observed and shown in Fig. 2. It can be seen from Fig. 2a, the rodlike crystals of PAL were well developed with a length up to 1 μm and a diameter of about 50–80 nm. The rod-like crystals of PAL were tightly packed due to the actions of van der Waals force and hydrogen bonds. After grinding treatment (PAL-4 and PAL-6), some rod-like crystals of PAL became shorter (Fig. 2b and c), the crystal bundles were partially dissociated and the dispersion degree of PAL crystals was improved. However, the rod-like crystals obviously got shorter when the grinding times were further increased (PAL-8), and most of them were in the form of granules (Fig. 2d). The crystal aggregates were significantly dissociated and the structure of PAL-8 was modified. The results could be explained as follows. The interaction among the rod–like single crystals of PAL is weak because of a line–line like contact [23]. When raw PAL was grinded, the two disks of stone miller generated strong compression, shearing stress and looping stress, which split the crystal bundles into individual rodlike crystals and the crystal aggregates were dissociated. With increasing the grinding times, the continual shearing stress and looping stress acting on the rod-like crystals of PAL increased, and induced the breakage of rod-like crystals, and therefore the crystal rods will be shorter. That is to say, large shearing forces resulting from the stone miller operating on the PAL can make the crystal aggregates and bundles into several crystal bundles or single crystals. However, if the strong shearing stress continues for a long time, it can cause serious damage to the long single crystals of PAL before obtaining high dispersion. In this case, to search out appropriate grinding times is essential and it can be said that the method of grinding treatment on PAL with appropriate grinding times can disperse part of the crystal aggregates into small crystal bundles and rod-like single crystals, which is helpful to extend the practical application of PAL. 3.3. XRD analysis X-ray diffraction patterns of PAL samples were presented in Fig. 3. A characteristic reflection peak of PAL at 2θ=8.38º (d=10.6 Å  [24]can be observed for all the PAL samples with greater intensity, indicating the order–disorder structural degree of PAL was very high. The appearance of the diffraction peak at 2θ=26.5º (d=3.36 Å and 2θ=31.0º (d=2.88 Å revealed that PAL contains minor contents(contaminants) of quartz and dolomite [24,25]. As the grinding times increased to 4, no significant change in diffraction peaks can be observed between the X-ray patterns of PAL-0, PAL-2 and PAL-4, suggesting the crystal structure of PAL was not affected in the processesystals, which is helpful to extend the practical application of PAL. |
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2楼2012-10-22 16:22:11
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3.1 傅里叶红外光谱（FTIR）分析 红外光谱通常被用来鉴别特征基团的变化。图1为PAL样品的红外光谱。可以看出1030和983cm-1出的吸收谱带归属于Si\O的伸缩振动，519和478处的吸收峰被归属为Si\O的弯曲振动。3411和1646处峰分别是PAL样品中配合水和吸收水中O/H伸缩振动及H/O/H弯曲振动。3621-3543处的宽峰归属为 (Al)O\H 和(Mg)O\H键的伸缩振动。从图1可以看出，与PAL-0的谱图相比，PAL-6在1030和983处的吸收峰变宽且强度降低。此外PAL样品的特征吸收峰之间并无明显差异。 太多了，自个慢慢翻译吧。  |
3楼2012-10-22 19:23:06