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Processes 2021, 9, 528 5 of 14 To exploit the phase purity and structure of the composite membranes, we also use the room-temperature XRD to characterize the sintered membranes (Figures S1–S3). Figures S1–S3 show the XRD patterns for the CPM-PSFA (M = Fe, Co, Ni, Cu) dual-phase membranes after sintering at 1275 ◦C, 1350 ◦C, and 1400 ◦C for 5 h, respectively. As shown in Figures S1–S3, all these sintered membranes also consist of CPM and PSFA two phases. No other impurities can be observed. XRD results imply that all four sintered composite membranes that were studied kept the same structures as the powders, suggesting the sintered CPM-PSFA composite membranes were prepared successfully. Moreover, we further perform XRD refinements for all the dual-phase powders obtained by heating at 950 ◦C for 10 h using the Rietveld model to get more information in detailed. The obtained cell parameters are listed in Table 1. There is hardly change in the cell parameters of PSFA phase from the CPM-PSFA composite, whereas the cell parameters of CPM phase significantly decreased compared with that of the undoped fluorite phase (CP). The shrinking lattice parameters in CPM (M = Fe, Co, Ni, and Cu) are all smaller than that of the undoped CP because of the smaller ion radius of Fe3+ (0.0645 nm), Co2+ (0.0745 nm), Ni2+ (0.056 nm), and Cu2+ (0.073 nm) compared with that of Ce4+ (0.087 nm). In other words, since ionic radius of these dopants (Cu2+, Co2+, Fe3+, and Ni2+) is smaller than that of Ce4+, the lattice constant a in CPM is expected to be smaller than that of the pristine CP, further implying that these transition metal elements have been successfully substituted into CP phase instead of PSFA phase. Table 1. Unit cell parameters of CPM-PSFA powders obtained by heating at 950 ◦C for 10 h. Materials CPFe-PSFA CPCo-PSFA CPNi-PSFA CPCu-PSFA CP-PSFA 1 CP a = b = c (Å) 5.4100 (3) 5.4099 (3) 5.4099 (4) 5.4102 (3) 5.4131 (3) a (Å) 5.4419 (4) 5.4415 (3) 5.4413 (3) 5.4416 (2) 5.4414 (3) PSFA (t = 0.86195) b (Å) 7.7355 (3) 7.7358 (2) 7.735 (3) 7.7359 (4) 7.7356 (3) c (Å) 5.4848 (4) 5.4842 (3) 5.4845 (3) 5.4844 (4) 5.4844 (4) 1 The data is from ref. [33]. 3.2. Morphology Characterization To check the density of the sintered membranes before being used for the oxygen permeability test, SEM is employed to characterize the microscopic morphology of the CPM-PSFA (M = Fe, Co, Ni, Cu) membranes. After several sintering temperature attempts, we finally found out that the appropriate sintering temperature for the CPM-PSFA (M = Fe, Co, Ni, Cu) composite membranes is in the temperature range of 1250–1300 ◦C. Compared with the sintering temperature of undoped CP-PSFA (1450–1500 ◦C, 5 h), the sintering temperature for CPM-PSFA can be remarkably reduced after adding the transition metals (M = Fe, Co, Ni, and Cu) into the fluorite phase being as the sintering aids. The significant reduction of sintering temperature is not only in favor of the reduction of the energy consumption in the material preparation process but also the requirements for equipment. Here, for better comparison, we adopt the final sintering temperature at 1275 ◦C for 5 h for all the samples. As presented in Figure 2, there are no cracks or interlocking pores on the surfaces of these composite membranes after sintering in air at 1275 ◦C for 5 h, indicating that all these sintered membranes were dense. In addition, the backscattered scanning electron microscope (BSEM) images can be distinguished by two different colors, which indicates that the sintered membranes are mainly composed of two phases. The bright region represents the CPM phase and the dark region represents the PSFA phase due to the increase of the strength of backscattered electron signal with the increase of atomic number. Moreover, it is obvious that the grain sizes of the CPM phase and PSFA phase are very similar. In addition, the copper-doping membrane CPCu-PSFA obviously displays the largest grain size of the other three membranes. Two phases are evenly distributed in the membranes and form the percolated paths, which play an important part in thePDF Image | CO2-Tolerant Oxygen Permeation Membranes
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