Process method of rare earth oxysulfide by using alkali chloride

A technology of rare earth sulfur oxides and alkali metal chlorides, applied in rare earth metal compounds, rare earth metal sulfides, chemical instruments and methods, etc., can solve the problems of large particles, reduced luminescence performance, etc., and achieves simple preparation and synthesis methods. Production cost, effect of reducing particle distribution range

Active Publication Date: 2015-01-28
南通捷事达新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the rare earth sulfur oxides prepared by the sulfur melting method have large particles and require ball mil...

Method used

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  • Process method of rare earth oxysulfide by using alkali chloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Raw material composition is as in table 1 1 # Shown, specific preparation method comprises the following steps:

[0021] ① Weigh 18.672g Y by weight 2 o 3 , 13.146g Na 2 CO 3 (mol(Na 2 CO 3 ):mol(Y 2 o 3 )=1.5), 9.280g sublimation sulfur (mol (sublimation sulfur): mol (Y 2 o 3 )=3.5) and 0.876gLiCl(mol(LiCl):mol(Y 2 o 3 )=0.25), mix the weighed materials evenly;

[0022] ②Put the uniformly mixed material into a crucible with a cover inside and outside, fill the gap between the two crucibles with high-temperature resistant powder and compact it;

[0023] ③Raise the temperature of the crucible containing the mixture to 300°C at a heating rate of 2°C / min, and keep it warm for 1h, then raise the temperature to 1100°C at a heating rate of 3°C / min, sinter for 3h, and then cool down to room temperature with the furnace;

[0024] ④ The sintered product is washed with hot water and stirred, and suction filtered;

[0025] ⑤Put the washed product into a constant temp...

Embodiment 2

[0029] ① Weigh 19.060g La by weight 2 o 3 , 10.541g Na 2 CO 3 (mol(Na 2 CO 3 ): mol (La 2 o 3 )=1.7), 7.034g sublimation sulfur (mol (sublimation sulfur): mol (La 2 o 3 )=3.75) and 1.709gNaCl(mol(NaCl):mol(La 2 o 3 )=0.5), mix the weighed materials evenly;

[0030] ②Put the uniformly mixed material into a crucible with a cover inside and outside, fill the gap between the two crucibles with high-temperature resistant powder and compact it;

[0031] ③Raise the temperature of the crucible containing the mixture to 330°C at a heating rate of 2.5°C / min, and keep it warm for 1.5h, then raise the temperature to 1150°C at a heating rate of 3.5°C / min, sinter for 4h, and then cool down to room temperature with the furnace;

[0032] ④ The sintered product is washed with hot water and stirred, and suction filtered;

[0033] ⑤Put the washed product into a constant temperature blast drying oven to dry to obtain rare earth sulfur oxides.

[0034] The test results of this rare ea...

Embodiment 3

[0037] Composition as in Table 1 3 # Shown, specific preparation method comprises the following steps:

[0038] ①Weigh 19.151gGd by weight 2 o 3 , 10.639g Na 2 CO 3 (mol(Na 2 CO 3 ): mol (Gd 2 o 3 )=1.9), 7.200g sublimated sulfur (mol (sublimed sulfur): mol (Gd 2 o 3 )=4.25) and 2.954gKCl(mol(KCl):mol(Gd 2 o 3 )=0.75), mix the weighed materials evenly;

[0039] ②Put the uniformly mixed material into a crucible with a cover inside and outside, fill the gap between the two crucibles with high-temperature resistant powder and compact it;

[0040] ③Raise the temperature of the crucible containing the mixture to 360°C at a heating rate of 3°C / min, and keep it warm for 2h, then raise the temperature to 1200°C at a heating rate of 4°C / min, sinter for 5h, and then cool down to room temperature with the furnace;

[0041] ④ The sintered product is washed with hot water and stirred, and suction filtered;

[0042] ⑤Put the washed product into a constant temperature blast dry...

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Abstract

The invention discloses a process method of rare earth oxysulfide by using an alkali chloride. The method comprises the following steps: (1) weighing required materials RE2O2S (wherein RE is one of rare earth elements Y, La, Gd and Sm), Na2CO3, sublimed sulfur and alkali chloride AMCl (wherein AM is one of alkali metal elements Li, Na or K) according to a stoichiometric ratio and uniformly mixing the weighed materials; (2) putting the uniformly mixed materials into inner and outer crucibles, and filling high-temperature powder in the gap between the two crucibles and compacting, where each of the two crucibles has a cover; (3) raising the temperature of the crucibles with the mixed material to 1100-1250 DEG C in a gradient way, sintering for 3-5 hours and then cooling to room temperature along with a furnace; (4) washing the sintered product with hot water, stirring, and carrying out suction filtration; and (5) drying the washed product into a constant-temperature blowing drying box to obtain the rare earth oxysulfide. By taking RE2O3, Na2CO3, sublimed sulfur and alkali chloride AMCl as raw materials, the rare earth oxysulfide is prepared by using a sulfur melting method. The preparation method of the rare earth oxysulfide is simple and easy to operate and the rare earth oxysulfide can be used in the fields of light-emitting materials and photoabsorption materials and the like.

Description

technical field [0001] The invention relates to a process for preparing rare earth sulfur oxides from alkali metal chlorides, in particular to the preparation and modification of rare earth sulfur oxides by sulfur melting, and the preparation and optimization of rare earth sulfur oxides with narrow particle distribution. Background technique [0002] Rare earth sulfur oxides have high chemical stability and thermal stability, are insoluble in water, and have a melting point as high as 2000-2200°C; the band gap is 4.6-4.8eV, which is suitable for doping ions; its maximum phonon energy is 520cm -1 , is suitable as a host material for luminescent materials, and has very high light absorption and energy transfer efficiency. Hex Ln 2 o 2 The biggest feature of the S crystal structure is that it has a relatively spacious space structure, allowing a certain amount of cation and anion vacancies to form and a certain amount of interstitial ions to enter, while the crystal structure...

Claims

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Application Information

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IPC IPC(8): C01F17/00
CPCC01F17/294C01P2002/72C01P2004/61
Inventor 韩朋德姜晓萍张林涛张长森张其土
Owner 南通捷事达新材料有限公司
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