Diffraction peaks, broadening

Determined by inductively coupled plasma-mass spectrometry of acid digested catalyst samples Calculated from X-ray diffraction peak broadening at (101) foranatase and (110) formtile TiOa Mean particle diameter measured from transmission electron microscopy pictures of gold catalysts... 

Cemy, R.,etal., Anisotropic diffraction peak broadening and dislocation substructnre in hydrogen-cycled LaNi5 and snbstitntional derivatives. Journal of Applied Crystallography, 2000, 33(4) p. 997-1005. 

It was well known that Williamson-Hall method is more accurate method to calculate crystallite size as compared to Debye-Scherrer method. The Fig. 2 represents the Williamson-Hall (W-H) plot for YP04 Eu nanostructure phosphor. As shown in Fig. 2, the Y- intercept is 0.0027 taking X as 0.154 nm, the grain size was found to be around 62 nm. The calculated particle size was in good concurrence with the Debye-Scherrer data. The small variation in the size of grains calculated by Debye-Scherrer and W-H method was due to the fact that in Debye-Scherrer formula strain component was assumed to be zero and the diffraction peak broadening was assumed to be due to reduced grain size only. 

The analogy of a crystal surface as a diffraction grating also suggests how surface defects can be probed. Recall that for a diffraction grating the width of a diffracted peak will decrease as the number of lines in the grating is increased. This observation can be used in interpreting the shape of RHEED spots. Defects on a crystal surfr.ee can limit the number of atomic rows that scatter coherendy, thereby broadening RHEED features. 

X-Ray diffraction has an important limitation Clear diffraction peaks are only observed when the sample possesses sufficient long-range order. The advantage of this limitation is that the width (or rather the shape) of diffraction peaks carries information on the dimensions of the reflecting planes. Diffraction lines from perfect crystals are very narrow, see for example the (111) and (200) reflections of large palladium particles in Fig. 4.5. For crystallite sizes below 100 nm, however, line broadening occurs due to incomplete destructive interference in scattering directions where the X-rays are out of phase. The two XRD patterns of supported Pd catalysts in Fig. 4.5 show that the reflections of palladium are much broader than those of the reference. The Scherrer formula relates crystal size to line width ... 

This approach also allows an easy correction of the diffraction peaks from the instrumental broadening that can be obtained by fitting the peak profile of a standard... 

The 500 nm size is a limit value crystallites below this size tend to broaden the diffraction peaks in a spectrum, while size distributions above this value produce particularly sharp signals whose half width is a function only of the wavelength of the X-ray beam and the equipment. Signal broadening is at its maximum in materials known as X-ray amorphous substances, featuring particle size distributions below 8 nm. These afford flattened, washed-out spectra of little analytical value. 

In amorphous solids there is a considerable disorder and it is impossible to give a description of their structure comparable to that applicable to crystals. In a crystal indeed the identification of all the atoms in the unit cell, at least in principle, is possible with a precise determination of their coordinates. For a glass, only a statistical description may be obtained to this end different experimental techniques are useful and often complementary to each other. Especially important are the methods based on diffraction experiments only these will be briefly mentioned here. The diffraction pattern of an amorphous alloy does not show sharp diffraction peaks as for crystalline materials but only a few broadened peaks. Much more limited information can thus be extracted and only a statistical description of the structure may be obtained. The so-called radial distribution function is defined as ... 

The broadening of the characteristic peaks of the silicon XRD signal provides information about stress and size of the crystallites. Figure 7.4 shows the diffraction pattern of microporous silicon powders scraped from p-type Si electrodes and of a bulk silicon powder sample. The peak broadening increases with increasing formation current density. For low formation current densities a superposition of... 

The first zero occurs ain q, =1, i.e. the width of the diffraction peak varies inversely as the number of atoms. We expect appreciable broadening of diffraction spots for crystallites less than a few nanometres on edge and this is indeed observed. 

Characterization of photonic nanoparticles is as important as its fabrication. Nanoparticles are often called clusters. While cluster size is determined in most cases by transmission electron microscopy, line broadening of the x-ray diffraction peaks, or... 

As the crystallite size decreases, the width of the diffraction peak increases. To either side of the Bragg angle, the diffracted beam will destructively interfere and we expect to see a sharp peak. However, the destructive interference is the resultant of the summation of all the diffracted beams, and close to the Bragg angle it takes diffraction from very many planes to produce complete destructive interference. In small crystallites not enough planes exist to produce complete destructive interference, and so we see a broadened peak. 

X-ray diffraction of the powder precipitated in solution confirmed it to be HgSe (sphalerite). The spectrum of the film showed a strong (111) peak and virtually no other reflection, suggesting a high degree of texture of these films. From the peak broadening, a crystal size of 7.7 nm was calculated. 

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