硫系玻璃原料提纯及模压成型工艺研究
发布时间:2018-06-19 09:43
本文选题:硫系玻璃 + 提纯 ; 参考:《西安工业大学》2017年硕士论文
【摘要】:硫系玻璃具有结构稳定,红外透过范围较宽,在8~12μm红外透过率高,以及制备周期短、原料成本低等优点,在红外热成像和红外光学领域具有广泛的应用前景。但是由于杂质吸收峰的存在导致硫系玻璃的红外透过波段不能完全被利用,并且模压成型技术的不成熟也制约了其在红外光学领域的应用。本文通过X射线衍射分析、傅里叶红外光谱分析、差示扫描量热分析、硬度、密度和热膨胀测量等,对Ge_(23)Se_(67)Sb_(10)硫系玻璃的结构和性能进行了表征。通过钛镁提纯法和蒸馏法对Ge_(23)Se_(67)Sb_(10)硫系玻璃原料进行提纯处理,制备出高透过率、低损耗的玻璃样品。最后研究了模压成型快速制备玻璃镜片的制备工艺,分析了不同温度、压力、时间条件下的玻璃制品质量与工艺之间的关系,确定出最佳的制备工艺。本文的研究结果如下:(1)通过盐浴淬火成功制备出直径达到80 mm Ge_(23)Se_(67)Sb_(10)玻璃试样,发现大尺寸玻璃的红外透过率受内部成分分布和玻璃厚度影响。其中直径为50 mm玻璃试样径向红外透过率由边缘向中心递减,厚度对试样的红外透过率影响呈指数型,越厚则红外透过率越低。采用镀膜处理可将玻璃红外透过率从60%提高到80%以上。(2)采用钛镁提纯法和蒸馏法对玻璃中的杂质进行提纯处理,成功消除了玻璃在2~16μm波段(除4.5μm处)的杂质吸收,并且降低了4.5μm处的杂质吸收,玻璃红外透过率可达62%以上。(3)卤素碘的引入成功将Ge_(23)Se_(67)Sb_(10)玻璃的红外透过范围从2.5~16μm扩展到了2.5~25μm。发现随着碘含量的增加,试样的密度与硬度均逐渐减小,其热膨胀系数也随着先增加后减小。在加入7 wt.%的碘后,试样的红外透过率在2.5~16μm波段达到66%,在16~25μm波段达到40%。(4)模压温度和保压时间是硫系玻璃热压成型的关键因素,通过实验发现在330℃模压后并保压20 min制品表面粗糙度相对最低,红外透过率可达50%以上。模压后样品硬度达161.5 kg·mm~(-2)左右,比熔融淬冷法制备出的玻璃硬度增加了10 kg·mm~(-2)左右。
[Abstract]:Sulfur glasses have the advantages of stable structure, wide infrared transmission range, high infrared transmittance at 812 渭 m, short preparation period, low raw material cost, and so on. It has a wide application prospect in infrared thermal imaging and infrared optics. However, due to the existence of impurity absorption peak, the infrared transmission band of sulfur glasses can not be fully utilized, and the immaturity of molding technology also restricts its application in infrared optics. By means of X-ray diffraction, Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), hardness, density and thermal expansion measurements, the structure and properties of the glass of the sulfur series Geal _ 23Seal _ (67) SbSP _ (10) have been characterized. The high transmittance and low loss glass samples were prepared by purifying and distilling the raw materials of GeS23SeSch _ (67) SB _ (+ 10) S _ 2O _ (10) glass by means of the methods of purification and distillation of titanium and magnesium. In the end, the preparation process of glass lens was studied, and the relationship between the quality of glass products under different temperature, pressure and time was analyzed, and the optimum preparation process was determined. The results of this paper are as follows: (1) through salt bath quenching, the glass samples up to 80 mm in diameter are successfully prepared. It is found that the infrared transmittance of large size glasses is affected by the distribution of internal components and the thickness of glass. The radial infrared transmittance of the glass sample with diameter of 50 mm decreases from the edge to the center, and the influence of thickness on the infrared transmittance of the sample is exponential. The thicker the sample is, the lower the infrared transmittance is. The infrared transmittance of glass can be increased from 60% to more than 80% by coating treatment. The impurity in glass can be purified by titanium and magnesium purification method and distillation method. The impurity absorption of glass in the band of 2x 16 渭 m (except 4.5 渭 m) has been successfully eliminated. Moreover, the impurity absorption at 4.5 渭 m was reduced, and the infrared transmittance of the glass was over 62%. 3) the introduction of halogen iodine successfully extended the infrared transmission range of the glass from 2.5 ~ 16 渭 m to 2.5 ~ 25 渭 m. It is found that the density and hardness of the sample decrease with the increase of iodine content, and the coefficient of thermal expansion increases first and then decreases. After the addition of iodine for 7 wt.%, the infrared transmittance of the sample reached 66 in the band of 2.5 ~ 16 渭 m, and reached 40 ~ 4 at the band of 16 ~ 25 渭 m) the molding temperature and the holding time were the key factors in the hot pressing of the sulfur glass. It is found that the surface roughness of 20 min products is the lowest after moulding at 330 鈩,
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