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Application of X-Ray Methods for Determining the Dimensions of Nanoparticles in the Nanosized Anatase–Poly(N-vinylcaprolactam) System
Crystallography Reports ( IF 0.6 ) Pub Date : 2020-07-28 , DOI: 10.1134/s1063774520040161
S. P. Mulakov , P. V. Konarev , O. I. Timaeva , G. M. Kuz’micheva

Abstract

Nanocomposites prepared by mechanical mixing with grinding and mechanical activation of a mixture of Hombifine N with nanosized anatase (NA) and poly(N-vinylcaprolactam) (PVCL) polymer (PVCL25 and PVCL40 polymers were obtained by drying a PVC aqueous solution at 25 and 40°C, respectively) in different weight ratios have been studied by wide-angle X-ray scattering (WAXS) and (for the first time) small-angle X-ray scattering (SAXS). Amorphization of anatase (decrease in the average size of the coherent-scattering region), selection of X-ray amorphous hydrated titanium dioxide from the amorphous shell of anatase nanoparticles, destruction of PVCL, and disordering of its heterocycles in NA/PVCL (NA : PVCL = 1 : 1) nanocomposites upon mechanical activation have been revealed. The interaction (with water molecule exchange) between anatase, anatase, and PVCL nanoparticles during formation of NA/PVCL25 (NA : PVCL = 1 : 2) upon mechanical mixing with grinding is found to lead to segregation of anatase nanoparticles into two groups: particles with reduced and enhanced (formation of texture) degree of crystallinity (average sizes of coherent-scattering regions) in comparison with the initial anatase. SAXS made it possible to reveal structural inhomogeneities of different sizes in PVCL25 and PVCL40, which change differently upon mechanical activation, retaining the tendency to smaller sizes in PVCL25 (a coil) in comparison with PVCL40 (a globule). It is shown that the effects of mechanical activation and mechanical mixing with grinding on the components of NA–PVCL system differ, and that anatase nanoparticles play a decisive role in NA/PVCL nanocomposites, facilitating averaging of the inhomogeneity sizes upon mechanical activation. The results of studying the photocatalytic activity in the reaction of methyl orange decomposition (UV irradiation) in the presence of NA–PVCL samples indicate that it depends on the average sizes of coherent-scattering regions and is independent of the inhomogeneity sizes.


中文翻译:

X射线方法在确定锐钛矿型聚(N-乙烯基己内酰胺)纳米系统中纳米粒子的尺寸中的应用

摘要

通过将25%和40%的PVC水溶液干燥而获得的纳米复合材料是通过机械混合研磨和机械活化Hombifine N与纳米锐钛矿(NA)和聚(N-乙烯基己内酰胺)(PVCL)聚合物(PVCL25和PVCL40聚合物)的混合物而制备分别通过广角X射线散射(WAXS)和(首次)小角X射线散射(SAXS)研究了不同重量比的℃。锐钛矿的非晶化(相干散射区域的平均尺寸减小),从锐钛矿纳米颗粒的非晶态壳中选择X射线非晶态水合二氧化钛,破坏PVCL以及在NA / PVCL中破坏其杂环(NA: PVCL = 1:1)已经揭示了机械活化后的纳米复合材料。锐钛矿,锐钛矿之间的相互作用(与水分子交换)发现在机械混合与研磨过程中形成NA / PVCL25(NA:PVCL = 1:2)的过程中,PVC和PVCL纳米颗粒会导致锐钛矿型纳米颗粒偏析成两类:结晶度降低和增强(质地形成)的颗粒(相干散射区域的平均大小)与初始锐钛矿相比。SAXS可以揭示PVCL25和PVCL40中不同尺寸的结构不均匀性,这些不均匀性在机械激活后会发生变化,与PVCL40(小球)相比,保留了PVCL25(线圈)中尺寸较小的趋势。结果表明,机械活化和机械混合与研磨对NA–PVCL体系组分的影响不同,并且锐钛矿纳米颗粒在NA / PVCL纳米复合材料中起决定性作用,促进机械激活时不均匀尺寸的平均。研究在NA–PVCL样品存在下甲基橙分解反应(紫外线照射)中的光催化活性的结果表明,它取决于相干散射区域的平均大小,并且与不均匀性大小无关。
更新日期:2020-07-28
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