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综合报道了本实验室关于黄铜矿类I-III-VI2型系列晶体的研究进展。采用两温区气相输运温度振荡法合成出高纯、单相、致密的多晶材料,在三温区立式炉中用坩埚旋转下降法生长出AgGaS2、AgGaSe2和AgGa1-xInxSe2等系列单晶体,X射线单晶衍射谱和回摆谱表明晶体的结晶性好,结构完整;红外透过率接近理论值,吸收系数低于0.017 cm-1,表明生长的晶体光学质量高。研究出一种新的能对AgGa1-xInxSe2晶体(112)晶面进行择优腐蚀的腐蚀剂:(30 g CrO3+10 mL H2O)∶H4PO4(85%)∶HNO3(65~68%)∶HF(40%)=10∶10∶10∶2(体积比),在60℃下腐蚀40 min,能够清晰地显示出AgGa1-xInxSe2晶体(112)面取向一致的三角形腐蚀坑,边界清晰,蚀坑密度大约为105/cm2数量级。采用自行研制的晶体定向切割新方法,加工出AgGa1-xInxSe2-OPO器件,获得了3~5μm的激光输出,光-光转换效率达21%。
This paper comprehensively reports the progress of our laboratory on the type I-III-VI2 crystals of chalcopyrite. High purity, single phase and dense polycrystalline materials were synthesized by gas-phase transport temperature oscillation in two temperature zones. Single crystals of AgGaS2, AgGaSe2 and AgGa1-xInxSe2 were grown by rotary crucible descent in a three-temperature vertical furnace. X-ray single crystal diffraction spectrum and back-swing spectrum show that the crystal has good crystallinity and complete structure. The infrared transmittance is close to the theoretical value, and the absorption coefficient is less than 0.017 cm-1, indicating that the grown crystal has high optical quality. A new etchant capable of selectively etching the (112) crystal plane of AgGa1-xInxSe2 crystal has been developed: (30 g CrO3 + 10 mL H2O): H4PO4 (85%): HNO3 %) = 10:10:10:2 (volume ratio), and then etched at 60 ℃ for 40 min, the triangle corrosion pits with consistent orientation of (112) AgGa1-xInxSe2 crystals can be clearly seen. 105 / cm2 order of magnitude. The AgGa1-xInxSe2-OPO device was fabricated by a new method of directional crystal cutting by itself. Laser output of 3 ~ 5μm was obtained. The light-to-light conversion efficiency reached 21%.