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The assertion that the three scattering peaks observed at the relative peak positions of 1:(8/3)1/2:(12/3)1/2 were associated with the fee lattice might be subjected to suspicion that the peak located at 0.37 nm-1 was the satellite peak of the primary peak that was masked by the DM peak at 0.41 nm-1; in that case, the actual diffraction peaks were located at 0.41, 0.61, and 0.76 nm-1. However, we did not consider the peak at 0.37 nm-1 to be the satellite peak because this peak was reproducible in terms of its intensity and position relative to those of the DM peak for the experiments using three independent samples. Such a reproducibility was not expected for a satellite peak because the intensity and position of the satellite peak depended on the orientation of the large grains with respect to the incident beam and such an orientation varied from one sample to another. Moreover, if the actual diffraction peaks were loca
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-1. In this case, the position ratio was 1:1.65:2.05, which closely agreed with that (1:1.63:2.0) prescribed by the fee lattice.
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17
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33847065745
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The first three bcc scattering peaks exhibit the relative position of 1:21/2:31/2. The 21/2 peak showed up clearly in the profile collected at 197°C in Figure 2, while the 31/2 peak was hardly discernible. By contrast, the 21/2 peak was absent in the profiles collected at 180, 170, and 155°C, whereas the 31/2 peak was visible. Both 21/2 and 31/2 peaks were visible in the scattering profiles collected by heating in Figure 1. The diminishment of the scattering peaks was again attributable to the relatively large grains developed during cooling from the DM phase, as illustrated in the Supporting Information. Because the grains were able to rotate when the temperature of the specimen was changed during the SAXS measurement, their orientations with respect to the incident beam may vary from one temperature to another, thereby leading to 2-D patterns with different distributions of the scattering
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1/2 peaks were observable. For the sample containing a small number of relatively large grains that give rise to a series of diffraction spots, the relative intensities of the scattering peaks collected by the linear detector should be carefully treated for further analysis because the intensities along the linear detector strongly depend on the grain orientations, which change with temperature in the cooling experiment due to grain rotations. However, the relative positions of the peaks appeared in the 1-D intensity profile are still reliable for identifying the type of lattice structure if a sufficient number of peaks are present.
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