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Method for synthesizing high-stability gamma-Pr2S3 powder

A high-stability, -pr2s3 technology, applied in chemical instruments and methods, rare earth metal compounds, inorganic chemistry, etc., can solve the problems of low purity, high cost, and low product stability, and achieve simple process, low cost, and broad The effect of applying the foreground

Inactive Publication Date: 2017-03-22
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Apparently existing synthetic preparation of γ-Pr 2 S 3 The powder method has different defects, such as harsh requirements on process equipment and conditions, high vulcanization temperature, long time, high cost, or low product stability and low purity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1 Preparation of precursor powder: Pr according to the ratio of the amount of substance 3+ :Na + =1.0:2.0 Weigh 200 mesh analytical grade praseodymium carbonate (molecular formula: Pr 2 (CO 3 ) 3 ) 11.55 grams of powder and 5.85 grams of NaCl. At 25℃, add the weighed NaCl into 17ml deionized water to make the concentration 6.0mol·L -1 Then inject the prepared NaCl solution into the praseodymium carbonate powder and stir it with a magnetic stirrer until it is uniform; then place the mixture of NaCl and praseodymium carbonate in a vacuum drying oven at 90°C for 12 hours to remove moisture and take it out After grinding into a powder of 200 mesh, 17.4 grams of precursor powder of praseodymium carbonate and NaCl uniformly mixed can be obtained.

[0025] Step 2γ-Pr 2 S 3 Preparation of powder: Put the precursor powder prepared in step 1 in an atmosphere tube furnace, and under the protection of Ar with a flow rate of 50mL / min, heat up at a heating rate of 5℃ / min. When the t...

Embodiment 2

[0027] Step 1 Preparation of precursor powder: Pr according to the ratio of the amount of substance 3+ :Na + =1.0:1.0 Weigh 200 mesh analytical grade praseodymium carbonate (molecular formula: Pr 2 (CO 3 ) 3 ) 16.1 grams of powder and 4.1 grams of NaCl. At 25℃, add the weighed NaCl to 23ml deionized water to make the concentration 3.0mol·L -1 Then inject the NaCl solution into the praseodymium carbonate powder and stir it with a magnetic stirrer until it is uniform; then place the solid-liquid mixture of NaCl and praseodymium carbonate in a vacuum drying oven at 70°C for 12 hours to remove moisture, and take it out After grinding into 300 mesh powder, 20.2 grams of precursor powder of praseodymium carbonate and NaCl uniformly mixed can be obtained.

[0028] Step 2γ-Pr 2 S 3 Preparation of powder: Put the precursor powder prepared in step 1 in an atmosphere tube furnace, under the protection of Ar with a flow rate of 30mL / min, heat up at a heating rate of 5℃ / min, when the tube furn...

Embodiment 3

[0030] Step 1 Preparation of precursor powder: Pr according to the ratio of the amount of substance 3+ :Na + =1.0:1.5 Weigh 250 mesh analytical grade praseodymium carbonate (molecular formula: Pr 2 (CO 3 ) 3 ) 16.9 grams of powder and 6.4 grams of NaCl. At 25℃, add the weighed NaCl into 22.0ml deionized water to make a concentration of 5.0mol·L -1 Inject the NaCl solution into the praseodymium carbonate powder and stir it with a magnetic stirrer until it is uniform; then place the solid-liquid mixture of NaCl and praseodymium carbonate in a vacuum drying oven at 80°C for 12 hours to remove moisture, and take it out After grinding into powder of 250 mesh, 23.3 grams of precursor powder of praseodymium carbonate and NaCl uniformly mixed can be obtained.

[0031] Step 2γ-Pr 2 S 3 Preparation of powder: Put the precursor powder prepared in step 1 in an atmosphere tube furnace, under the protection of Ar with a flow rate of 30-50mL / min, heat up at a heating rate of 5℃ / min, when the tem...

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Abstract

The invention relates to a method for synthesizing high-stability gamma-Pr2S3 powder. By virtue of the method, high-purity gamma-Pr2S3 powder with a cubic structure within a temperature range from the room temperature to 1340 DEG C and stable thermodynamics performance at a relatively low preparation temperature and a relative short temperature maintenance time can be obtained. The problems that the vulcanizing temperature is high, the time is long, the cost is high, or the product stability is low, the purity is low, and carbon pollution and sulfur oxide impurities are easily produced in the prior art are solved. Gamma-phase Pr2S3 belongs to a stable phase at a temperature higher than 1340 DEG C, so that praseodymium sulfide powder prepared by virtue of the method can stably preserve a gamma-phase structure in a whole temperature range. Meanwhile, the method is simple in process, low in cost and applicable to the large-scale preparation of high-stability high-purity gamma-phase praseodymium sulfide, and has wide application prospects.

Description

Technical field [0001] The invention belongs to the technical field of new materials and relates to a synthetic high-stability γ-Pr 2 S 3 The method of powder, specifically relates to a rapid synthesis of high stability γ-phase praseodymium sulfide (γ-Pr 2 S 3 ) Preparation method of powder. Γ-Pr prepared by this method 2 S 3 The powder can be kept in a cubic phase in the whole temperature range, has high thermodynamic stability, and is used to prepare γ-Pr 2 S 3 Polycrystalline materials, thermoelectric materials. Background technique [0002] There are three crystal phase structures of praseodymium sulfide compounds: α phase, β phase and γ phase, among which α-Pr 2 S 3 It belongs to the orthorhombic system, and the space group is (D 2h 16 -Pnma), the stable phase at room temperature; β-Pr 2 S 3 Is a tetragonal structure, and the space group is (D 4h 20 -I4 1 / acd) The molecular formula is written as Pr 10 S 15-x O x (0≤x≤1), essentially sulfur oxide of praseodymium, β-Pr 2 S 3 T...

Claims

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Application Information

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IPC IPC(8): C01F17/00
CPCC01F17/288C01P2002/30
Inventor 李焕勇朱娜娜
Owner NORTHWESTERN POLYTECHNICAL UNIV
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