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A low-temperature sintered rare earth sulfide γ-ln 2 the s 3 A method for infrared transparent ceramics

A rare earth sulfide and transparent ceramic technology, applied in the field of materials, can solve the problems of easy oxidation transmittance, difficult sintering, poor uniformity and other problems of samples

Active Publication Date: 2021-04-20
陕西智航昱铠新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to avoid the deficiencies of the prior art, the present invention proposes a low-temperature sintered rare earth sulfide γ-Ln 2 S 3 (Ln=La, Ce, Pr, Nd, Y) The method of infrared transparent ceramics solves the problem of γ-La 2 S 3 The representative light rare earth sulfide ceramics have the disadvantages of low transmittance, difficult sintering and poor uniformity due to the high sintering temperature, which leads to the sample being easily oxidized in the hot pressing preparation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: A low-temperature sintered γ-La 2 S 3 A method for infrared transparent ceramics

[0029] Step 1 Nanoscale Polysulfide LaS 2 Powder preparation: Weigh 5.0 grams of analytically pure oxyhydrogen carbonate powder La(OH)CO 3 ·nH 2 O (n = 1 ~ 8), put the powder in the atmosphere tube furnace, feed Ar gas with a gas flow rate of 30ml / min, and the tube furnace will heat up at a heating rate of 2°C / min; when the furnace temperature rises to 650 ℃, change the gas flow into Ar gas and CS with a flow rate of 30ml / min 2 The mixed gas, where the volume ratio of the mixed gas is Ar:CS 2 1:1, heat preservation 4h, after the heat preservation is over, change the gas flow into Ar gas with a flow rate of 30ml / min, and the tube furnace is naturally cooled to room temperature; take out the powder from the furnace, and use deionized water and no Wash the powder twice with water and ethanol, then put the powder into a vacuum drying oven, dry for 3 hours at 80°C and a vacuum...

Embodiment 2

[0032] Example 2: A low-temperature sintered γ-La 2 S 3 A method for infrared transparent ceramics

[0033] Step 1 Nanoscale Polysulfide LaS 2 Powder preparation: Weigh 5.0 grams of analytically pure oxyhydrogen carbonate powder La(OH)CO 3 ·nH 2 O (n = 1 ~ 8), put the powder in the atmosphere tube furnace, feed Ar gas with a gas flow rate of 40ml / min, and the tube furnace will heat up at a heating rate of 5°C / min; when the furnace temperature rises to 600 ℃, change the gas flow into Ar gas and CS with a flow rate of 40ml / min 2 The mixed gas, where the volume ratio of the mixed gas is Ar:CS 2 1:1, heat preservation 2h, after the heat preservation is over, change the gas flow into Ar gas with a flow rate of 40ml / min, and the tube furnace is naturally cooled to room temperature; take out the powder from the furnace, and use deionized water and no Wash the powder twice with water and ethanol, then put the powder into a vacuum drying oven, dry for 6 hours at 80°C and a vacuum...

Embodiment 3

[0036] Example 3: A low-temperature sintered γ-La 2 S 3 A method for infrared transparent ceramics

[0037] Step 1 Nanoscale polysulfide LaS 2 Powder preparation: Weigh 5.0 grams of analytically pure oxyhydrogen carbonate powder La(OH)CO 3 ·nH 2 O (n = 1 ~ 8), put the powder in the atmosphere tube furnace, feed Ar gas with a gas flow rate of 50ml / min, and the tube furnace will heat up at a heating rate of 3°C / min; when the furnace temperature rises to 600 °C, change the gas flow into Ar gas and H with a flow rate of 50ml / min 2 A mixed gas of S, where the volume ratio of the mixed gas is Ar:H 2 S is 1:1, heat preservation for 3h, after the heat preservation is over, change the gas flow into Ar gas with a flow rate of 50ml / min, and the tube furnace is naturally cooled to room temperature; take out the powder from the furnace, and use deionized water and Wash the powder twice with absolute ethanol, then put the powder in a vacuum drying oven, dry for 5 hours at 80°C and a v...

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Abstract

The invention relates to a low-temperature sintered rare earth sulfide γ-Ln 2 S 3 The method of infrared transparent ceramics can be sintered under ultra-high pressure and relatively low temperature to prepare rare earth sulfide infrared transparent ceramics with high stability, high density and high transmittance. Compared with the existing ceramic sintering technology, this method uses ultra-high pressure and nano-powder to effectively reduce the sintering temperature, making the sintering temperature lower than γ‑Ln 2 S 3 The oxidation starting temperature can effectively avoid the problem of easy oxidation during the sintering process of rare earth sulfide polycrystalline ceramics. At the same time, nano-scale powders are helpful to solve the problems of difficult sintering and poor uniformity. In addition, the use of low-melting co-solvents is conducive to achieving densification. The ultra-high pressure will inhibit the abnormal growth of grains, so the γ‑Ln with high microstructure consistency and good optical transmittance can be obtained 2 S 3 Transparent ceramic. At the same time, the method has simple process, low cost and high efficiency, is suitable for large-scale preparation of rare earth sulfide infrared transparent ceramics, and has broad application prospects.

Description

technical field [0001] The invention belongs to the technical field of materials, and relates to low-temperature sintering rare earth sulfide γ-Ln 2 S 3 (Ln=La, Ce, Pr, Nd, Y) A method for infrared transparent ceramics, specifically related to a low-temperature, ultra-high-pressure preparation of high-stability, high-density, high-transmittance rare earth sulfide γ-Ln 2 S 3 A method for infrared transparent ceramics. Background technique [0002] Rare earth sulfide γ-Ln 2 S 3 (Ln=La, Ce, Pr, Nd, Y), with cubic Th 3 P 4 structure (with metal vacancies), which can be made into transparent ceramics by densification and sintering. Such materials generally have a melting point higher than 2000°C, high mechanical strength, high hardness, good thermal stability, and excellent resistance to rain erosion and sand erosion, and because the Ln-S bond has no absorption in the infrared region, making γ -Ln 2 S 3 It has good transmittance in the infrared band (there is a certain ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/547C04B35/622C04B35/645C04B35/626
CPCC04B35/547C04B35/622C04B35/626C04B35/62645C04B35/62675C04B35/6268C04B35/645C04B2235/442C04B2235/444C04B2235/5454C04B2235/6562C04B2235/6565C04B2235/6567C04B2235/9653
Inventor 李焕勇任晓宇郗鹏飞
Owner 陕西智航昱铠新材料有限责任公司