Crystal material, preparation method thereof and nonlinear optical crystal including same
A technology of nonlinear optics and crystal materials, applied in the direction of nonlinear optics, polycrystalline material growth, optics, etc., can solve problems such as crystal comprehensive performance defects, and achieve the effect of simple steps, high yield and high purity
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Embodiment 1
[0040] The preparation of embodiment 1 sample
[0041] Sample I-1 # preparation of
[0042] Na 2 After S (23.2mg), In (136.3mg) and Se (140.5mg) are batched and mixed evenly, they are packed into a graphite crucible, placed in a quartz tube, and evacuated to 10 -4 Torr (1 torr = 133.322 Pa) seal the tube, put it into the muffle furnace and slowly heat it to 850 °C, keep it warm for 72 hours, after cooling down to 300 °C after 3 °C / h, turn off the muffle furnace and naturally cool to room temperature, and get The chemical formula is Na 2 In 4 SSe 6 red crystals, denoted as sample I-1 # .
[0043] Sample I-2 # ~Sample I-5 # preparation of
[0044] The specific preparation process is the same as sample I-1 # , the difference lies in the proportion of ingredients, high-temperature solid-phase reaction temperature, high-temperature solid-phase reaction time, cooling rate;
[0045] Table 1 Sample I-2 # ~Sample I-6 # preparation of
[0046]
[0047] Sample II-...
Embodiment 2
[0055] The structural characterization of embodiment 2 sample
[0056] Sample I-1 # ~I-6 # The X-ray powder diffraction phase analysis (XRD) was carried out on the MiniFlex II X-ray diffractometer of Rigaku Company, Cu target, Kα radiation source (λ=0.154184nm). The results showed that sample I-1 # ~I-6 # They are all samples with high purity and high crystallinity, the crystal structure type is the same, the peak positions of the main characteristic peaks are the same, and the peak intensity of each peak varies slightly with the difference of A element, M element, and Q element.
[0057] Sample I-1 # The X-ray single crystal diffraction was carried out on a Rigaku Pilatus type single crystal diffractometer, Mo target, Kα radiation source (λ=0.07107nm), test temperature 293K. And through the structure analysis of Shelxtl 97, the analysis result is:
[0058] The chemical formula is Na 2 In 4 SSe 6 , belonging to the orthorhombic Pca2 1 The space group, the unit cell p...
Embodiment 3
[0071] The frequency doubling test of embodiment 3 sample
[0072] respectively for sample I-1 # ~I-6 # , Sample II-1 # ~II-6 # Do the multiplier test, the specific steps are as follows:
[0073]The laser with a wavelength of 1910nm generated by OPO technology is used as the fundamental frequency light to irradiate the crystal powder to be tested, and the intensity of the 955nm second harmonic generated by the charge-coupled device (CCD) is used to detect the intensity of the second harmonic of 955nm generated by the test sample and the standard sample AgGaS 2 Grind separately, and use a standard sieve to sieve crystals of different particle sizes, the particle sizes are 30-50 μm, 50-75 μm, 75-100 μm, 100-125 μm, 125-150 μm and 150-200 μm. Observe the change trend of the frequency multiplier signal with the particle size, and judge whether it can achieve phase matching. Under the same conditions, compare the intensity of the second harmonic generated by the sample with tha...
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