A method of preparing gamma-La2S3 infrared transparent ceramic having a high infrared transmittance

A technology of infrared transmittance and transparent ceramics, which is applied in the field of new materials, can solve the problems of low infrared transmittance, easy oxidation, low infrared transmittance and strong absorption of sulfur oxides, etc., and achieves simple process and infrared transmittance. High and good thermal stability

Active Publication Date: 2017-03-22
陕西智航昱铠新材料有限责任公司
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AI Technical Summary

Problems solved by technology

In 1981, A.A.Kamarzin grew γ-La by high temperature melt method 2 S 3 Single crystal (Journalof Crystal Growth, 1981,52:619-622.), the first experiment confirmed the γ-La 2 S 3 The excellent photoelectric performance of single crystal, especially confirmed that it has a certain transmittance in the 2.5-20μm band; in 1993, P.N.Kumta et al. prepared γ-La by hot pressing sintering method 2 S 3 ceramic materials (Journal of Materials Research, 1993, 8(6): 1394~1410.), and reported its infrared optical properties, indicating that γ-La 2 S 3 The material can be used as an infrared transparent material in the 8-14 μm band, but its reported infrared transmittance is lower than 25%, and because of the oxophilicity of lanthanum, γ-La 2 S 3 Very easily oxidized; subsequently in 1994 Ming Shyong Tsai passed Ca 2+ Doping attempts to improve γ-La 2 S 3 Infrared performance, prepared La-rich CaLa 2 S 4 (Journal of Materials Research, 1994,9(11):2939-2943.); People such as Peisen Li, Huanyong Li also reported Ca 2+ 、Na 2+ and Bi 3+ Doped γ-La 2 S 3 Hot-pressed preparation and infrared properties of ceramics (Journal of Synthetic Crystals, 2010, 39(3): 568-572; Journal of Physics D-Applied Physics, 2011, 44(9): 095402-095407; Journal of the American Ceramic Society, 2011,94(4):1162–1166; Scripta Materialia,2011,64:1023-1027.)
But currently about γ-La 2 S 3 Hot-pressed infrared transparent ceramics have low infrared transmittance and strong absorption of sulfur oxides in the 8-14 μm band, which seriously affects the γ-La 2 S 3 Properties and Applications of Infrared Transparent Ceramics

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: 0.08mol

[0026]Step 1, at 25 °C, 28.0 g of analytically pure LaCl 3 ·6H 2 O was dissolved in 80ml deionized water to obtain a concentration of 1.0mol L -1 The solution of lanthanum chloride; 24.7 grams of analytically pure sodium citrate (chemical formula Na 3 C 6 h 5 o 7 ) was dissolved in 85ml deionized water to obtain a concentration of 1.0mol L -1 Sodium citrate solution; 4.1 g of NaBr was dissolved in 12 ml of deionized water to make a saturated solution of NaBr. The mass ratio of the solute between the above solutions is LaCl 3 ·6H 2 O: sodium citrate: NaBr = 1.0: 1.2: 0.5. Mix the lanthanum chloride solution and the sodium citrate solution at 25°C, stir evenly with a magnetic stirrer, then transfer to a stainless steel autoclave with a polytetrafluoroethylene liner, the filling degree is 90%, and the high-pressure reaction The autoclave was closed, then the autoclave was placed in an electric furnace, the temperature was raised to 120 °C at ...

Embodiment 2

[0031] Example 2: 0.05mol

[0032] Step 1, at 25 °C, 17.5 g of analytically pure LaCl 3 ·6H 2 O was dissolved in 50ml deionized water to obtain a concentration of 1.0mol L -1 The solution of lanthanum chloride; 15.4 grams of analytically pure sodium citrate (chemical formula Na 3 C 6 h 5 o 7 ) was dissolved in 55ml deionized water to obtain a concentration of 1.0mol L -1 Sodium citrate solution; 2.6 g of NaBr was dissolved in 10 ml of deionized water to make a saturated solution of NaBr. The mass ratio of the solute between the above solutions is LaCl 3 ·6H 2 O: sodium citrate: NaBr = 1.0: 1.2: 0.5. Mix the lanthanum chloride solution and the sodium citrate solution at 25°C, stir evenly with a magnetic stirrer, then transfer to a stainless steel autoclave with a polytetrafluoroethylene liner, the filling degree is 90%, and the high-pressure reaction The autoclave is closed, then the autoclave is placed in an electric furnace, the temperature is raised to 150 °C at a ...

Embodiment 3

[0037] Example 3: 0.03mol

[0038] Step 1, at 25 °C, 10.6 g of analytically pure LaCl 3 ·6H 2 O was dissolved in 30ml deionized water to obtain a concentration of 1.0mol L -1 The solution of lanthanum chloride; 9.3 grams of analytically pure sodium citrate (chemical formula Na 3 C 6 h 5 o 7 ) was dissolved in 35ml deionized water to obtain a concentration of 1.0mol L -1 Sodium citrate solution; 1.5 g of NaBr was dissolved in 8 ml of deionized water to make a saturated solution of NaBr. The mass ratio of the solute between the above solutions is LaCl 3 ·6H 2 O: sodium citrate: NaBr = 1.0: 1.2: 0.5. Mix the lanthanum chloride solution and the sodium citrate solution at 25°C, stir evenly with a magnetic stirrer, then transfer to a stainless steel autoclave with a polytetrafluoroethylene liner, the filling degree is 90%, and the high-pressure reaction The autoclave is closed, then the autoclave is placed in an electric furnace, the temperature is raised to 130 °C at a ra...

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Abstract

The invention relates to a method of preparing gamma-La2S3 infrared transparent ceramic having a high infrared transmittance. The gamma-La2S3 infrared transparent ceramic which is in a cubic phase at a temperature ranging from room temperature to 1300 DEG C and is stable in structure can be prepared under conditions of a low preparing temperature, a low vacuum degree, low pressure and short temperature maintaining time. Technical problems that a liquid phase is difficult to generate, ceramic microstructure uniformity is poor and optical transmittance in the prior art is low are overcome. The gamma-La2S3 infrared transparent ceramic the average transmittance of which in a waveband of 8-14 [mu]m is not less than 50% can be prepared. Compared with the prior art, the prepared gamma-La2S3 hot-press infrared transparent ceramic has characteristics of good thermal stability, a simple process and the high infrared transmittance.

Description

technical field [0001] The invention belongs to the technical field of new materials and relates to a method for preparing γ-La 2 S 3 A method for infrared transparent ceramics, specifically relating to a γ-La with high infrared transmittance in the 8-14 μm band 2 S 3 Preparation method of transparent ceramics. Background technique [0002] γ-La 2 S 3 As a rare earth chalcogenide with cubic Th 3 P 4 structure (with metal vacancies), can be made into transparent ceramics by hot pressing and sintering. At present, one of the main applications of this material is as a long-wave infrared wave-transmitting material in the 8-14 μm band, but its theoretical wave-transmitting range is 2.5-20 μm. The material has a melting point of 2100°C and a hardness of up to 6.7GPa / mm 2 , the optical bandgap is 2.76eV and the bandgap temperature variation coefficient is extremely small dE g / dT=4.9×10 –4 eV / K, refractive index in the 1-15μm band n=2.6, thermal conductivity κ=2.3×10 –2 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/50C04B35/626C04B35/645
CPCC04B35/5156C04B35/547C04B35/626C04B35/645C04B2235/444C04B2235/9653
Inventor 李焕勇田雷远丁文忠
Owner 陕西智航昱铠新材料有限责任公司
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