Infrared nonlinear optical crystal material, preparation method and application thereof
A nonlinear optics and crystal material technology, applied in the field of nonlinear optical materials, can solve the problems of unsatisfactory comprehensive performance, low laser damage threshold, large crystal growth, etc., and achieve excellent infrared nonlinear optical performance, simple steps, and crystallinity. Good results
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[0035] Example 1 Preparation of powder crystal sample
[0036] Mix the raw materials with the flux, grind them evenly, place them in the quartz reaction tube, and evacuate to 10 -2 Pa and use a hydrogen-oxygen flame to fuse and seal the quartz reaction tube. Put the quartz reaction tube in a high temperature furnace, heat it to the solid melting temperature, and keep it for a period of time. Then, the temperature is lowered to 300° C. at a rate of no more than 5° C. / hour, the heating is stopped, and the nonlinear optical crystal material is obtained by natural cooling to room temperature.
[0037] The sample number, type and proportion of raw materials, type and amount of flux, solid melting temperature and holding time are shown in Table 1. The substances indicated by only element symbols in the table are simple substances.
[0038] Table 1
[0039]
[0040]
Example Embodiment
[0041] Example 2 Preparation of single crystal sample
[0042] The type and ratio of raw materials are the same as that of sample 2 in Example 1. # , The raw materials and flux are uniformly ground and placed in the quartz reaction tube, and the vacuum is pumped to 10 -2 Pa and use a hydrogen-oxygen flame to fuse and seal the quartz reaction tube. Put the quartz reaction tube in a high temperature furnace, heat to 650℃, keep it for 2 hours, then increase the temperature to 950℃ and keep it for 24 hours, then cool down to 300℃ at a rate of no more than 5℃ / hour, stop heating and cool naturally The single crystal sample of the nonlinear optical crystal material is obtained at room temperature, which is recorded as sample 7 # .
Example Embodiment
[0043] Example 3 Characterization of the structure of the sample
[0044] Sample 1 # ~7 # The X-ray powder diffraction phase analysis (XRD) was performed on the MiniFlex II X-ray diffractometer of Rigaku Company, Cu target, and Kα radiation source (λ=0.154184nm). The results show that the sample 1 prepared in Examples 1 and 2 # ~7 # They are all samples of high purity and high crystallinity, typical representatives such as figure 1 Medium sample 1 # ~4 # XRD spectrum. Sample 5 # ~Sample 7 # The XRD spectrum results of figure 1 Same, that is, the position and shape of the diffraction peaks are basically the same, and the relative peak intensity fluctuates within ±5%. Description sample 1 # ~7 # Have the same crystal structure.
[0045] Sample 7 # The X-ray single crystal diffraction was performed on a Mercury CCD single crystal diffractometer, Mo target, Kα radiation source (λ=0.07107nm), and the test temperature was 293K. And through Shelxtl97 for structural analysis. The theore...
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