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Method for preparing yttrium silicate nano powder

A technology of nano-powder and yttrium silicate, applied in chemical instruments and methods, rare earth metal compounds, inorganic chemistry, etc., can solve the problems of long cycle, high preparation temperature, complicated process, etc., and achieve short reaction cycle and low preparation cost , the effect of easy access to raw materials

Inactive Publication Date: 2009-03-25
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its preparation method is complex and requires high temperature for a long time
YCl 3 , PrOH, TEOS, etc. as raw materials, Y was prepared by the sol-gel method 2 SiO 5 , the process is complicated, the cycle is long, and there are impurities
Ana I.Becerro et al. (Ana I.Becerro, Moise's Naranjo, Ana C.Perdigo'n, and Jose'M.Trillo Hydrothermal Chemistry of Silicates: Low-Temperature Synthesis of y-Yttrium Disilicate.J.Am.Ceram.2003.86 [9]1592-1594.) with Y 2 o 3 , SiO 2 As the main raw material, yttrium silicate is synthesized at high temperature, and its preparation temperature is too high, which is not conducive to mass production
Huang Jianfeng et al. (Huang Jianfeng, Deng Fei, Cao Liyun et al. Controllable synthesis of yttrium silicate nanocrystals by sonochemical method, Journal of Synthetic Crystals [J]. 2007.36(2).463-465.) with Y(NO 3 ) 3 , Na 2 SiO 3 , NaOH is used as raw material, sonochemical method is used to prepare yttrium silicate, which cannot directly prepare yttrium silicate from the liquid phase, and requires annealing at 900 ° C for 2 hours, and as a result, relatively pure yttrium silicate cannot be prepared

Method used

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  • Method for preparing yttrium silicate nano powder
  • Method for preparing yttrium silicate nano powder
  • Method for preparing yttrium silicate nano powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) The analytically pure Y(NO 3 ) 3 ·6H 2 O, Na 2 SiO 3 9H 2 O and NaOH were added into distilled water and stirred continuously to prepare a transparent solution with a concentration of 0.5mol / L, in which Y(NO 3 ) 3 : Na 2 SiO 3 : The molar ratio of NaOH is 2:1:4, and it is stirred continuously to form a precursor solution, and the obtained solution is recorded as A solution;

[0019] 2) Pour the A solution prepared above into the hydrothermal reaction kettle, and the filling degree is controlled at 60%; then seal the hydrothermal reaction kettle, and put it into the MDS-6 type temperature-pressure dual-control microwave hydrothermal reaction apparatus; The hydrothermal temperature is controlled at 180°C, and the reaction time is controlled at 10 minutes. After the reaction is completed, it is naturally cooled to room temperature, and the obtained solution is recorded as B solution;

[0020] 3) Open the hydrothermal reaction kettle, filter B solution through f...

Embodiment 2

[0023] 1) The analytically pure Y(NO 3 ) 3 ·6H 2 O, Na 2 SiO 3 9H 2 Add O and NaOH into distilled water, and keep stirring to prepare a transparent solution with a concentration of 0.7mol / L, in which Y(NO 3 ) 3 : Na 2 SiO 3 : The molar ratio of NaOH is 2:1:4, and it is stirred continuously to form a precursor solution, and the obtained solution is recorded as A solution;

[0024] 2) Pour the above-prepared A solution into the hydrothermal reaction kettle, and the filling degree is controlled at 60%; then seal the hydrothermal reaction kettle, and put it into the MDS-6 type temperature-pressure dual-control microwave hydrothermal reaction apparatus; The hydrothermal temperature is controlled at 180°C, and the reaction time is controlled at 10 minutes. After the reaction is completed, it is naturally cooled to room temperature, and the obtained solution is recorded as B solution;

[0025] 3) Turn on the hydrothermal reaction kettle, filter B solution through filter pape...

Embodiment 3

[0029] 1) The analytically pure Y(NO 3 ) 3 ·6H 2 O, Na 2 SiO 3 9H 2 O and NaOH were added into distilled water and stirred continuously to prepare a transparent solution with a concentration of 0.6mol / L, in which Y(NO 3 ) 3 : Na 2 SiO 3 : The molar ratio of NaOH is 2:1:4, and it is stirred continuously to form a precursor solution, and the obtained solution is recorded as A solution;

[0030] 2) Pour the A solution prepared above into the hydrothermal reaction kettle, and the filling degree is controlled at 60%; then seal the hydrothermal reaction kettle, and put it into the MDS-6 type temperature-pressure dual-control microwave hydrothermal reaction apparatus; The hydrothermal temperature is controlled at 150°C, and the reaction time is controlled at 10 minutes. After the reaction is completed, it is naturally cooled to room temperature, and the obtained solution is recorded as B solution;

[0031] 3) Turn on the hydrothermal reaction kettle, filter B solution throug...

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Abstract

The invention relates to a preparation method of for an yttrium silicate nanopowder is disclosed, comprising the following steps: analytically pure Y(NO3)3 question mark 6H2O, Na2SiO3 question mark 9H2O and NaOH are added into distilled water and then stirred for obtaining solution A; the solution A is poured into a hydrothermal reaction kettle; the hydrothermal temperature is controlled at 120 to 180 DEG C; the reaction time is controlled at 10min to 60min; after the reaction is finished, the solution A is naturally cooled to the room temperature so as to obtain solution B; the products of the solution B are collected by pumping filtration of filter paper, which are then washed and dried for 0.5 to 1h, finally product C which contains yttrium silicate nanopowder is obtained. By using a microwave hydrothermal method, the invnetion can rapidly prepare yttrium silicate nanopowder with controllable crystal form and size. The controllable yttrium silicate nanopowder prepared by the process has the advantages of short reaction cycle, good reproducibility, simple process, convenient operation, easy obtaining of raw materials, and lower preparation cost.

Description

technical field [0001] The invention belongs to the field of material chemical industry, and in particular relates to a preparation method of yttrium silicate nanopowder. Background technique [0002] Yttrium silicate material has a high melting point (Y 2 SiO 5 , Y 2 Si 2 o 7 and Y 4 Si 3 o 12 The melting points are 1980°C, 1775°C and 1950°C, respectively), low high temperature oxygen permeability, low thermal expansion coefficient, low Young's modulus, low thermal conductivity, low high temperature volatility, chemical corrosion resistance, and chemical and thermodynamic stability. characteristic. It can be used as high-temperature anti-oxidation coating materials, optical matrix materials and dielectric materials for high-performance structural materials (such as graphite, C / C composite materials and SiC structural ceramics, etc.). [0003] At present, the methods for preparing yttrium silicate crystals mainly include solid-state reaction method, hydrothermal met...

Claims

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Application Information

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IPC IPC(8): C01F17/00
Inventor 黄剑锋曹丽云许斌生
Owner SHAANXI UNIV OF SCI & TECH
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