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Hydrothermal preparation method for potassium plumbite single crystal

A technology of potassium lead acid and single crystal, applied in the field of chemical engineering, can solve the problems of high energy consumption and uneven composition of potassium lead acid, and achieve the effect of reducing energy consumption and environmental pollution, and reducing the preparation process and production cost.

Inactive Publication Date: 2009-11-18
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the problems of high energy consumption and composition inhomogeneity in the preparation process of potassium lead acid

Method used

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  • Hydrothermal preparation method for potassium plumbite single crystal
  • Hydrothermal preparation method for potassium plumbite single crystal
  • Hydrothermal preparation method for potassium plumbite single crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Put lead oxide (PbO) and potassium hydroxide (KOH) into the autoclave after weighing, the molar ratio of lead oxide and potassium hydroxide is 1, and add corresponding volume of deionized Water, adjust the amount of raw materials so that the concentration of potassium hydroxide is 2mol / L, stir slowly with a glass rod to dissolve potassium hydroxide; Raise the heating rate to 160 degrees Celsius, keep it warm for 24 hours, and then cool with the furnace; take out and open the autoclave, pour the reactants into a beaker, and use deionized water to filter and wash repeatedly until the washing liquid becomes neutral, and the obtained single crystal particles are placed Put it into the oven and bake at 60 degrees Celsius for 10 hours. The phase and crystal structure of potassium plumbate were detected by X-ray diffractometer; figure 1 The morphology and size of potassium plumbate were detected by scanning electron microscopy.

Embodiment 2

[0015] Put lead oxide (PbO) and potassium hydroxide (KOH) into the autoclave after weighing, the molar ratio of lead oxide and potassium hydroxide is 5, add the corresponding volume of deionized Water, adjust the amount of raw materials so that the concentration of potassium hydroxide is 4mol / L, stir slowly with a glass rod to dissolve potassium hydroxide; Raise the heating rate to 190 degrees Celsius, keep it warm for 16 hours, and then cool with the furnace; take out and open the autoclave, pour the reactants into a beaker, and use deionized water to filter and wash repeatedly until the washing liquid becomes neutral. Put it into the oven and bake at 60 degrees Celsius for 10 hours. The phase and crystal structure of potassium plumbate were detected by X-ray diffractometer; figure 2 The morphology of the growth tip of the potassium plumbate is examined using a scanning electron microscope.

Embodiment 3

[0017] Put lead oxide (PbO) and potassium hydroxide (KOH) into the autoclave after weighing, the molar ratio of lead oxide and potassium hydroxide is 8, add the corresponding volume of deionized Water, adjust the amount of raw materials so that the concentration of potassium hydroxide is 7mol / L, stir slowly with a glass rod to dissolve potassium hydroxide; Raise the heating rate to 200 degrees Celsius, keep the temperature for 30 hours, and then cool with the furnace; take out and open the autoclave, pour the reactants into a beaker, and use deionized water to filter and wash repeatedly until the washing liquid becomes neutral. Put it into the oven and bake at 60 degrees Celsius for 10 hours. The phase and crystal structure of potassium plumbate were detected by X-ray diffractometer; image 3 The morphology of the potassium plumbate single crystals examined using a polarizing microscope is given.

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Abstract

The invention discloses a hydrothermal preparation method for potassium plumbite single crystal, comprising the following steps of: arranging a lead oxide and a potassium hydroxide with the molar ratio of 0.1-10 into a high-pressure kettle; adding a deioned water into the high-pressure kettle according to a filling rate of 50-80% so that the concentration of the potassium hydroxide is 0.1-10mol / L; sealing the high-pressure kettle and subsequently arranging the high-pressure kettle in a vertical pit furnace or an oven; heating the high-pressure kettle to the temperature of 130-240 DEG C at the temperature increment speed of 1-3 DEG C per minute; keeping the temperature for 4-72 hours; subsequently cooling the high-pressure kettle together with the furnace; taking out and opening the high-pressure kettle; pouring the obtained product into a beaker; repeatedly filtering and washing the obtained product by the deioned water till the cleaning solution is neutral; arranging the obtained single-crystal grains in the oven, and baking the grains at the temperature of 40-100 DEG C for 8-24 hours. The kalium plumbate single crystal prepared by the method has uniform grain and large dimension and can be used for superconductor industries; and the method is simple, energy-saving and exhaust-reducing, has low cost and is suitable for batch production.

Description

technical field [0001] The invention relates to a hydrothermal preparation method of potassium lead acid single crystal, which belongs to the field of chemical engineering. Background technique [0002] Potassium lead acid material is a very potential superconducting material. Literature "Vadim A. Drozd, Alexander M. Gabovich, Marek P k, Valery N. Boychuk, Dmitry P. Moiseevand Sergey A. Nedilko, Transport study of newly synthesized polycrystalline Sr 1-x K x PbO 3-δ solid solutions, Journal of Alloys and Compounds, 346(1-2): 17-23, 2002 "The ceramic bodies of potassium leadate and strontium potassium leadate were prepared by traditional solid-phase synthesis method. Not only the energy consumption is very large, but also in There are grain boundaries and compositional fluctuations in polycrystalline ceramics, which seriously affect the superconducting properties and stability of the material, while the superconducting properties of single crystals are much higher than tho...

Claims

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Application Information

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IPC IPC(8): C30B7/10C30B29/22
Inventor 刘来君方亮胡长征
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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