研究目的
The preparation of infra-red windows grade zinc selenide (ZnSe) by the reactive diffusion process between liquid zinc and selenium.
研究成果
Single-phase zinc selenide was successfully fabricated using a low-cost reactive diffusion method in sealed ampoules. The wurtzite phase formed at lower temperatures (750-850°C) but transformed to the stable cubic zinc-blende structure at 950°C, suitable for IR window applications. The formation involved a continuous porous layer at the zinc/selenium interface, explained by Kirkendall effects due to different diffusion coefficients of selenium and zinc. This method offers a viable alternative to expensive techniques like CVD, with potential for optimization to reduce porosity and impurities.
研究不足
The study is limited by the formation of porous structures in the zinc selenide layer due to differential diffusion rates, which may affect optical properties. The process requires high temperatures (up to 950°C) and sealed systems to handle high vapor pressures, potentially limiting scalability. Impurities from precursors and ampoules were detected, indicating possible contamination issues.
1：Experimental Design and Method Selection:
The study employed a reactive diffusion process in a sealed quartz ampoule to fabricate zinc selenide (ZnSe) from high-purity zinc and selenium elements. The method was chosen for its potential to produce high-quality ZnSe at low cost, based on the Kirkendall theory for diffusion mechanisms.
2：Sample Selection and Data Sources:
High-purity zinc (average size 60 μm) and selenium (average size 2 mm) were purchased from Merck Company. A nominal composition of Zn50Se50 was used, with samples prepared by milling in a planetary ball mill under argon atmosphere at 250 rpm for 30 minutes.
3：List of Experimental Equipment and Materials:
Equipment included a planetary ball mill, vacuum-packed quartz ampoules, annealing furnace for temperatures 550-950°C, Philips PW3710 X-ray diffractometer (λ=0.15406 nm; 40 kV), Fourier transform infrared spectroscopy equipment (Model JASCO 680-PLUS), and VEGA-TESCAN-XMU FESEM (V=20 kV). Materials were high-purity zinc and selenium from Merck.
4：15406 nm; 40 kV), Fourier transform infrared spectroscopy equipment (Model JASCO 680-PLUS), and VEGA-TESCAN-XMU FESEM (V=20 kV). Materials were high-purity zinc and selenium from Merck.
Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: The as-milled samples were sealed in quartz ampoules and annealed at temperatures from 550 to 950°C for various times (e.g., 5 hours for equilibrium). Phase determination was done using XRD, FTIR for functional group analysis, and FESEM for morphological and compositional analysis via EDS.
5：Data Analysis Methods:
XRD patterns were analyzed for phase identification, FTIR spectra for impurity detection, and SEM/EDS for morphological and compositional uniformity. Data interpretation relied on comparing with standard references and theoretical models like Kirkendall theory.
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