This paper reports on the successful preparation of LaPO4-x wt.% LiF (x = 0–5) ceramics using the traditional solid-state reaction method. The crystal structures, sintering behaviors, and dielectric response at microwave and terahertz frequencies were investigated. XRD results indicate that all the diffraction peaks were attributed to LaPO4, and no secondary phase was observed. Rietveld refinement was conducted to analyze the variation of the crystal structure of LaPO4-x wt.% LiF. SEM indicates that the addition of LiF significantly decreased the grain size while increasing the apparent density of the ceramics. When x = 3, the optimum microwave dielectric properties εr = 10.03, Q × f = 81,467 GHz, and τf = −43.79 ppm/°C were achieved in LaPO4-3 wt.% LiF ceramic at 750 °C. The infrared reflectance spectrum and terahertz time-domain spectroscopy were analyzed and compared with the dielectric properties measured at microwave frequency to investigate the inherent dielectric response. The findings indicate that the dielectric constant attributed to ionic displacement polarization and oxygen vacancy is an essential factor affecting dielectric loss. Moreover, it is worth noting that the LaPO4-3 wt.% LiF ceramic demonstrates excellent compatibility with silver powders, suggesting its immense potential as a dielectric material in LTCC applications.
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