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Method for preparing Tb:Lu2O3 ceramic by laser sintering

A technology of laser sintering and lu2o3, which is applied in the field of ceramic material preparation, can solve the problems of large size (10-30 μm, affecting the luminous quality of ceramics, poor mechanical properties, etc., achieve good mechanical properties, avoid unbalanced electricity prices, and suppress Tb4+ The effect of ion generation

Active Publication Date: 2018-11-06
徐州华焰特种陶瓷有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the introduction of sintering aids will lead to an imbalance in electricity prices
During sintering, the charge compensation effect will lead to Tb 3+ ion to Tb 4+ Ion transitions, which affect the luminous quality of ceramics
Therefore, it is difficult to use vacuum sintering for Tb during sintering 3+ To Tb 4+ effective control over the transformation of
Moreover, traditional vacuum sintering requires a higher sintering temperature (1600-1800°C) and a longer holding time (8-20h), which also leads to a generally large grain size of the sintered ceramics (10-30μm), and mechanical properties Poor, it is difficult to meet the current market demand for its mechanical properties

Method used

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  • Method for preparing Tb:Lu2O3 ceramic by laser sintering

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: (Lu 0.999 Tb 0.001 ) 2 o 3 transparent ceramic

[0027] According to (Lu 0.999 Tb 0.001 ) 2 o 3 The stoichiometric ratio of each element in is weighed Lu respectively 2 o 3 and Tb 4 o 7 Powder as reaction raw material;

[0028] Dilute citric acid with distilled water to a concentration of 0.05g / ml, add citric acid and ethylene glycol solution (the mol ratio of metal ion and citric acid is 0.2, and the mass ratio of citric acid and ethylene glycol is 1 ), and stir evenly to obtain a precursor solution;

[0029] Heat the precursor solution to 70 ° C for 24 hours to remove excess water, cool it to room temperature, and then place it in a mortar for grinding to obtain a precursor powder; then pre-prepared the ground precursor powder at 500 ° C Calcined for 5 h to remove excess organic matter, and then the pre-calcined precursor powder was placed in a muffle furnace and calcined at 800°C for 1 h.

[0030] Add 0.05g / ml of binder polyvinyl alcohol (...

Embodiment 2

[0033] Embodiment 2: (Lu 0.995 Tb 0.005 ) 2 o 3 transparent ceramic

[0034] According to (Lu 0.995 Tb 0.005 ) 2 o 3 The stoichiometric ratio of each element in the 3 ) 3 ·6H 2 O and Tb(NO 3 ) 3 ·5H 2 O powder as a reaction raw material;

[0035] Dilute citric acid with distilled water to a concentration of 0.1g / ml, add citric acid and ethylene glycol solution (the mol ratio of metal ion and citric acid is 0.3, and the mass ratio of citric acid and ethylene glycol is 1.5) in the mixed raw materials ), and stir evenly to obtain a precursor solution;

[0036] Heat the precursor solution to 75 ° C for 24 hours to remove excess water, cool it to room temperature, and then place it in a mortar for grinding to obtain a precursor powder; then pre-prepared the ground precursor powder at 700 ° C Calcined for 5 h to remove excess organic matter, and then the pre-calcined precursor powder was placed in a muffle furnace for calcination at 1000° C. for 2 h.

[0037] Add 0.1...

Embodiment 3

[0040] Embodiment 3: (Lu 0.98 Tb 0.02 ) 2 o 3 transparent ceramic

[0041] According to (Lu 0.98 Tb 0.02 ) 2 o 3 The stoichiometric ratio of each element in the 3 ) 3 ·6H 2 O and TbCl 3 ·6H 2 O powder as a reaction raw material;

[0042] Dilute citric acid with distilled water to a concentration of 0.2g / ml, add citric acid and ethylene glycol solution (the mol ratio of metal ion and citric acid is 0.5, and the mass ratio of citric acid and ethylene glycol is 2 ), and stir evenly to obtain a precursor solution;

[0043] Heat the precursor solution to 80°C for 24 hours to remove excess water, cool it to room temperature, and then place it in a mortar for grinding to obtain a precursor powder; Calcined for 7 hours to remove excess organic matter, and then placed the precalcined precursor powder in a muffle furnace for calcination at 1200°C for 3 hours.

[0044] Add 0.2g / ml of binder polyvinyl alcohol (polymerization degree: 1600-1900) solution to the calcined powde...

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Abstract

The invention discloses a method for preparing Tb:Lu2O3 ceramic by laser sintering. The method comprises the following specific steps: separately weighing reaction raw material powder according to thestoichiometric ratio of each element in the chemical structural formula (Lu<1-x>Tbx)2O3, adding citric acid and ethylene glycol into the material mixture, and stirring uniformly to obtain a precursor; then heating the precursor powder, grinding, and calcining by stages; adding a binder, a polyvinyl alcohol solution, into the calcined powder and carrying out dry pressing to obtain a disc-shaped primed piece; placing the primed piece on a Lu2O3 pad, and sintering the both sides of the primed piece by a laser; and finally, grinding and polishing to obtain the Tb:Lu2O3 ceramic. The method provided by the invention can effectively inhibit the conversion of Tb<3+> ions to Tb<4+> ions so as to improve the content of Tb<3+> ions in the ceramic, and realizes high-intensity green light emission under the excitation of 323nm ultraviolet light, the preparation process is simple, energy-saving and environmentally friendly, and the ceramic samples have a relative density of 99.9% and are of high transmittance and good compactness.

Description

technical field [0001] The invention belongs to the technical field of preparation of ceramic materials, in particular to a kind of laser sintering preparation of Tb:Lu 2 o 3 ceramic method. Background technique [0002] Lutetium oxide (Lu 2 o 3 ) has high transmittance under visible light and infrared light, large emission cross-section, low phonon energy, high density, and good mechanical and thermal properties. Therefore, lutetium oxide is an excellent laser dielectric material and scintillator material, and has broad application prospects. Lu 2 o 3 It has a cubic crystal structure, optical isotropy, and the refractive index does not depend on directionality. The powder can be made into transparent ceramics through nanocrystal technology and high-temperature sintering technology. At the same time, Lu 2 o 3 Transparent ceramics can be easily doped with different types and concentrations of rare earth ions, thus having a wide range of optical applications. [0003...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/50C04B35/64
CPCC04B35/50C04B35/64C04B2235/3224C04B2235/665C04B2235/77C04B2235/786C04B2235/9653
Inventor 张乐侯晨蒋志刚陈浩
Owner 徐州华焰特种陶瓷有限公司
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