Comparing Methods for Calculating Nano Crystal Size of Natural Hydroxyapatite Using X-Ray Diffraction.
Comparing Methods for Calculating Nano Crystal Size of Natural Hydroxyapatite Using X-Ray Diffraction.
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DOI：
10.3390/nano10091627
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发表时间：
2020-08-19
期刊：
影响因子：
--
通讯作者：
Janusas G
中科院分区：
文献类型：
--
作者：
Rabiei M;Palevicius A;Monshi A;Nasiri S;Vilkauskas A;Janusas G
我们报道了基于XRD图计算晶体尺寸的方法的比较。在这种情况下，从牛、猪和鸡的骨头中提取羟基磷灰石的XRD峰。羟基磷灰石是通过在950℃下对天然骨进行热处理合成的。通过X-Pert软件的调整，选择了每种方法的XRD图，并计算了晶体的大小。方法包括Scherrer（三种模型）、Monshi-Scherrer、Williamson-Hall三种模型（即均匀变形模型（UDM）、均匀应力变形模型（USDM）和均匀变形能量密度模型（UDEDM））、Halder-Wanger （H-W）和尺寸应变图法（SSP）。这些方法已被一起使用和比较。考虑所有可用峰（直线模型），各方法对牛、猪、鸡羟基磷灰石的XRD谱图在Scherrer法中得到的晶粒尺寸分别为1371、457和196 nm。新的模型（直线通过原点）给出了60nm， 60nm和53nm，显示出很大的改进。对于牛、猪和鸡，三种方法的平均模型分别为56、58和52 nm。Monshi-Scherrer法给出60、60和57 nm。UDM法测定的值分别为56、62和65 nm。USDM法计算的值分别为60、62、62 nm。牛、猪、鸡的UDEDM值分别为62、62、65 nm。此外，在H-W法中，所有样品的晶体尺寸值均为4 nm。分别在牛、猪和鸡的SSP法中计算43、62和57 nm的值。从各方法的值比较来看，考虑所有峰值的Scherrer方法（直线模型）导致了不合理的值。然而，其他值在可接受范围内，与文献中报道的值相似。实验分析，如气体吸附比表面积（布鲁诺尔-埃米特-泰勒（BET））和透射电镜（TEM）。在最后的比较中，考虑了精度、计算容易、研究人员有一个检查点、所得值与BET和TEM实验分析的差异等参数。Monshi-Scherrer方法通过对线性图应用最小二乘来简化计算并减少误差。这条线有一个检查点，即斜率不能离1太远。然后，截距给出最精确的晶体尺寸。在本研究中，BET值（56,52和49 nm）的设置也与Monshi-Scherrer方法相似，并建议将其用于纳米技术的研究。
We report on a comparison of methods based on XRD patterns for calculating crystal size. In this case, XRD peaks were extracted from hydroxyapatite obtained from cow, pig, and chicken bones. Hydroxyapatite was synthesized through the thermal treatment of natural bones at 950 °C. XRD patterns were selected by adjustment of X-Pert software for each method and for calculating the size of the crystals. Methods consisted of Scherrer (three models), Monshi–Scherrer, three models of Williamson–Hall (namely the Uniform Deformation Model (UDM), the Uniform Stress Deformation Model (USDM), and the Uniform Deformation Energy Density Model (UDEDM)), Halder–Wanger (H-W), and the Size Strain Plot Method (SSP). These methods have been used and compared together. The sizes of crystallites obtained by the XRD patterns in each method for hydroxyapatite from cow, pig, and chicken were 1371, 457, and 196 nm in the Scherrer method when considering all of the available peaks together (straight line model). A new model (straight line passing the origin) gave 60, 60, and 53 nm, which shows much improvement. The average model gave 56, 58, and 52 nm, for each of the three approaches, respectively, for cow, pig, and chicken. The Monshi–Scherrer method gave 60, 60, and 57 nm. Values of 56, 62, and 65 nm were given by the UDM method. The values calculated by the USDM method were 60, 62, and 62 nm. The values of 62, 62, and 65 nm were given by the UDEDM method for cow, pig, and chicken, respectively. Furthermore, the crystal size value was 4 nm for all samples in the H-W method. Values were also calculated as 43, 62, and 57 nm in the SSP method for cow, pig, and chicken tandemly. According to the comparison of values in each method, the Scherrer method (straight line model) for considering all peaks led to unreasonable values. Nevertheless, other values were in the acceptable range, similar to the reported values in the literature. Experimental analyses, such as specific surface area by gas adsorption (Brunauer–Emmett–Teller (BET)) and Transmission Electron Microscopy (TEM), were utilized. In the final comparison, parameters of accuracy, ease of calculations, having a check point for the researcher, and difference between the obtained values and experimental analysis by BET and TEM were considered. The Monshi–Scherrer method provided ease of calculation and a decrease in errors by applying least squares to the linear plot. There is a check point for this line that the slope must not be far from one. Then, the intercept gives the most accurate crystal size. In this study, the setup of values for BET (56, 52, and 49 nm) was also similar to the Monshi–Scherrer method and the use of it in research studies of nanotechnology is advised.
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DOI：
10.6028/jres.109.042
发表时间：
2004-11
影响因子：
1.5
作者：
Markovic M;Fowler BO;Tung MS
通讯作者：
Tung MS
影响因子：
2
作者：
Dey, P. C.;Das, R.
通讯作者：
Das, R.
影响因子：
5.2
作者：
Ayatollahi, M. R.;Yahya, Mohd Yazid;Abu Hassan, Shukur
通讯作者：
Abu Hassan, Shukur
DOI：
10.1007/bf02894766
发表时间：
1984-01-01
期刊：
PRAMANA
影响因子：
--
作者：
DE, M;SENGUPTA, SP
通讯作者：
SENGUPTA, SP
影响因子：
3.3
作者：
Madhavi, S;Ferraris, C;White, TJ
通讯作者：
White, TJ