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Preparation method of Y2SiO5 crystal whiskers

A whisker and 3·6H2O technology, applied in the field of Y2SiO5 material preparation, can solve the problems of complex preparation process, harsh reaction conditions, long reaction cycle, etc., and achieve the effect of simple process, avoiding grain growth and low cost

Active Publication Date: 2012-09-19
李建伟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These preparation methods have their unique advantages, but most of the disadvantages are that the preparation process is complex, the reaction cycle is long, the reaction conditions are relatively harsh, and late crystallization treatment is required, and most of them are related to Y 2 SiO 5 There is no report on powder preparation, but there is no report on Y 2 SiO 5 Whisker preparation reports

Method used

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  • Preparation method of Y2SiO5 crystal whiskers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1) Take analytically pure Y(NO) 3 ·6H 2 O, Na 2 SiO 3 9H 2 O, follow Y (NO) 3 ·6H 2 O:Na 2 SiO 3 9H 2 The molar ratio of O=2:0.8 is dissolved in absolute ethanol and prepared as Y 3+ A solution with a concentration of 0.01mol / L is adjusted to pH=2 with a NaOH solution with a concentration of 3mol / L to obtain solution A;

[0018] 2) Press Y into Solution A 3+ : citric acid=1:0.4 molar ratio, add analytically pure citric acid as a template, stir magnetically at room temperature for 1h, mix well, and obtain solution B;

[0019] 3) Put solution B in a polytetrafluoroethylene-lined hydrothermal kettle, control the filling ratio to 60%, then put the reaction kettle into a constant temperature reactor, and react at 400°C for 30h;

[0020] 4) The reaction system was naturally cooled to room temperature, centrifuged, washed three times with distilled water and absolute ethanol, and finally dried in an electric blast drying oven at 50°C to obtain Y 2 SiO 5 whiskers. ...

Embodiment 2

[0022] 1) Take analytically pure Y(NO) 3 ·6H 2 O, Na 2 SiO 3 9H 2 O, follow Y (NO) 3 ·6H 2 O:Na 2 SiO 3 9H 2 The molar ratio of O=2:1.4 is dissolved in absolute ethanol and formulated as Y 3+ A solution with a concentration of 0.2mol / L is adjusted to pH=4 with a NaOH solution with a concentration of 3mol / L to obtain solution A;

[0023] 2) Press Y into Solution A 3+: The mol ratio of citric acid=1:1.5 was added analytically pure citric acid as template agent, magnetically stirred at room temperature for 3h, mixed evenly, and obtained solution B;

[0024] 3) Put solution B in a polytetrafluoroethylene-lined hydrothermal kettle, control the filling ratio to 70%, then put the reaction kettle into a constant temperature reactor, and react at 280°C for 24 hours;

[0025] 4) The reaction system was naturally cooled to room temperature, centrifuged, washed with distilled water and absolute ethanol for 5 times, and finally dried in an electric blast drying oven at 80°C to o...

Embodiment 3

[0028] 1) Take analytically pure Y(NO) 3 ·6H 2 O, Na 2 SiO 3 9H 2 O, follow Y (NO) 3 ·6H 2 O:Na 2 SiO 3 9H 2 The molar ratio of O=2:1.1 is dissolved in absolute ethanol and formulated as Y 3+ A solution with a concentration of 0.1mol / L is adjusted to pH=3 with a NaOH solution with a concentration of 3mol / L to obtain solution A;

[0029] 2) Press Y into Solution A 3+ : citric acid=1:0.9 molar ratio is added analytically pure citric acid as a template, magnetically stirred at room temperature for 2h, mixed evenly, and obtained solution B;

[0030] 3) Put solution B in a polytetrafluoroethylene-lined hydrothermal kettle, control the filling ratio to 65%, then put the reaction kettle into a constant temperature reactor, and react at 340°C for 18 hours;

[0031] 4) The reaction system was naturally cooled to room temperature, centrifuged, washed with distilled water and absolute ethanol for 4 times, and finally dried in an electric blast drying oven at 65°C to obtain Y ...

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Abstract

The invention relates to a preparation method of Y2SiO5 crystal whiskers, which comprises the steps of: dissolving Y (NO)3.6H2O and Na2SiO3.9H2O in anhydrous ethanol to obtain solution A; adding citric acid in the solution A and magnetically stirring at room temperature to obtain solution B; and placing the solution B in a hydrothermal reaction kettle for constant-temperature reaction, conducting centrifugal separation after a reaction system is naturally cooled to room temperature, successively washing with distilled water and anhydrous ethanol and finally drying to obtain the Y2SiO5 crystal whiskers. Compared with the traditional method, the preparation method of the Y2SiO5 crystal whiskers has the advantages that the purity of the Y2SiO5 crystal whiskers prepared through a solvent hydrothermal synthesis method is high, the fineness is ultrahigh, the grain size distribution range is narrow, the extent of particle aggregation is low, the crystal is fully developed, the process is relatively simple, the appearance and the size are controllable, the process is simple and high-efficiency, the cost is lower, the preparation temperature is low, the later-stage crystallization is not required, the possible defects that the crystal grains grow up, are coarsened or are curled and the like in the later-stage heat treatment process are avoided to some extent, and the like. By adopting the solvent hydrothermal synthesis method, high-purity Y2SiO5 crystal whiskers with controllable appearance are prepared under low-temperature condition.

Description

technical field [0001] The invention relates to a shape-controllable Y 2 SiO 5 The preparation method of material, specifically relates to a kind of Y 2 SiO 5 Whisker preparation method. Background technique [0002] Y 2 SiO 5 Also known as yttrium orthosilicate, it belongs to monoclinic biaxial crystal system and belongs to C 6 2h space group, which (C 2 / c) The lattice constant is a=1.250nm, b=0.972nm, c=1.042nm, and the angle between the crystal planes is β=102.68°, with X 1 -Y 2 SiO 5 (low temperature phase) and X 2 -Y 2 SiO 5 (High temperature phase) Two different monoclinic structures. [Deng Fei, Huang Jianfeng, Cao Liyun, et al. Research progress of yttrium silicate materials [J]. Aerospace Materials Technology, 2006,4(6):1-4.]. [0003] Yttrium orthosilicate (Y 2 SiO 5 ) The structural characteristics of the material itself and a series of excellent physical and chemical properties, such as low elastic modulus, low high temperature oxygen permeabilit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/10C30B29/62C30B29/34
Inventor 黄剑锋杨柳青曹丽云王雅琴
Owner 李建伟
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