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Preparation method of gadolinium oxysulfide powder

A technology of gadolinium oxysulfide and powder is applied in the field of preparation of infrared materials, which can solve the problems of long reaction time, uneven particle size distribution of powder, agglomeration and the like, and achieve the effect of avoiding the discharge of harmful by-products.

Pending Publication Date: 2022-03-11
安徽光智科技有限公司
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Problems solved by technology

However, this method has defects such as high reaction temperature, long reaction time, uneven powder particle size distribution, more impurities, harsh reaction conditions, and easy generation of more pollutants and chemical waste.
The vulcanization method can make rare earth oxides or specific precursors in a certain S steam or H 2 S, CS 2 Vulcanize into sulfur oxides under the same atmosphere. If the sulfur source is sufficient and stable, its phase formation and annealing will proceed simultaneously, and the size of the particles can be adjusted, but the vulcanization medium is polluting gas, which is harmful to the environment.
The combustion method can achieve batch synthesis of high-purity nano-scale rare earth sulfur oxides in a short reaction time at low temperature, but there is agglomeration phenomenon

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  • Preparation method of gadolinium oxysulfide powder

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[0022] Aiming at the problem of environmental pollution in the preparation of gadolinium oxysulfide powder by vulcanization method in the prior art, this application provides a preparation method for preparing gadolinium oxysulfide powder, the preparation method is green and environmentally friendly, and the gadolinium oxysulfide powder has The particle size is small. The preparation process of the application gadolinium oxysulfide powder is as follows figure 1 As shown, the embodiment of the present invention specifically discloses a preparation method of gadolinium oxysulfide powder, comprising the following steps:

[0023] A) will Gd 2 o 3 , activator, flux and sulfur are mixed in a stoichiometric ratio to obtain a mixed powder;

[0024] B) ball milling the mixed powder and the mineralizer to obtain a precursor powder;

[0025] C) Calcining the precursor powder to obtain a primary powder, pickling the primary powder, and drying in a vacuum to obtain a gadolinium oxysulf...

Embodiment 1

[0033] A preparation method of ideal matrix material ultrafine gadolinium oxysulfide powder, the Gd 2 o 2 The preparation method of S powder comprises the steps:

[0034] (1) 181.3g Gd 2 o 3 , 15.312g Tb 4 o 7 or 20.428g Pr 6 o 11 One of the flux Na 2 CO 3 , 128.24g S is proportioned according to stoichiometry, and is initially mixed to obtain a mixed powder; the addition of flux is 0.5wt%;

[0035] (2) Add a certain proportion of mineralizers KF and KCl to the mixed powder, the addition amount is 0.5wt%, and add it into the planetary ball mill according to a certain ball-to-material ratio and mix evenly, and the ball-mill ratio is 2:1 to obtain the precursor powder;

[0036] (3) Calcining the obtained precursor powder at 1100°C for 1 h in a reducing atmosphere to obtain a primary powder; the SO produced during the calcination process 2 The gas can be recovered SO by activated carbon dry method 2 ; The reducing atmosphere is N 2 +H 2 Mix in proportion, where N 2...

Embodiment 2

[0040] A preparation method of ideal matrix material ultrafine gadolinium oxysulfide powder, the Gd 2 o 2 The preparation method of S powder comprises the steps:

[0041] (1) 181.3g Gd 2 o 3 , 15.312g Tb 4 o 7 or 20.428g Pr 6 o 11 One of the flux Li 2 CO 3 , 128.24g S is proportioned according to stoichiometry, and is initially mixed to obtain a mixed powder; the addition of flux is 0.5wt%;

[0042] (2) Add a certain proportion of mineralizers KF and KCl to the mixed powder, the addition amount is 0.5wt%, and add it into the planetary ball mill according to a certain ball-to-material ratio and mix evenly, and the ball-mill ratio is 8:1 to obtain the precursor powder;

[0043] (3) Calcining the obtained precursor powder at 1100°C for 1 h in a reducing atmosphere to obtain a primary powder; the SO produced during the calcination process 2 The gas can be recovered SO by activated carbon dry method 2 ; The reducing atmosphere is N 2 +H 2 Mix in proportion, where N 2...

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Abstract

The invention provides a preparation method of gadolinium oxysulfide powder, which comprises the following steps: A) mixing Gd2O3, an activating agent, a fluxing agent and sulfur according to a stoichiometric ratio to obtain mixed powder; b) carrying out ball milling on the mixed powder and a mineralizing agent to obtain precursor powder; and C) calcining the precursor powder to obtain primary powder, and performing acid pickling and vacuum drying on the primary powder to obtain the gadolinium oxysulfide powder. The preparation method of the gadolinium oxysulfide powder provided by the invention is green and environment-friendly, and the gadolinium oxysulfide powder with fine and uniform particle size can be prepared.

Description

technical field [0001] The invention relates to the technical field of preparation of infrared materials, in particular to a preparation method of gadolinium oxysulfide powder. Background technique [0002] Rare earth sulfur oxides have a hexagonal crystal structure, that is, space group P3m1, are insoluble in water, and have a chemical formula of RE 2 o 2 S, where RE=Y, La, Gd and Lu, are the hosts of luminescent materials, which are white. Gd 2 o 2 S, namely GOS, high melting point (2070°C-2200°C), lattice constant Large band gap (4.6eV), high density (7.34g / cm 3 ), wherein the atomic number of Gd is 60, which has high resistance to X-rays, high luminous efficiency, strong oxidation resistance, high light absorption rate and transmission efficiency, and is non-toxic. Due to the existence of anisotropy, there is birefringence on the grain boundary, and it is not easy to prepare transparent ceramics. Phonons have low energy and good physical and chemical stability, s...

Claims

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Application Information

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IPC IPC(8): C01F17/294C01F17/10C09K11/84
CPCC01F17/294C01F17/10C09K11/7701C01P2004/61
Inventor 安宁于金凤
Owner 安徽光智科技有限公司
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