Preparation method of controllable yttrium silicate nano-rod

A technology of yttrium silicate and nanorods is applied in the field of preparation of yttrium silicate nanorods, which can solve the problems of reports that have no influence on the process structure, complicated preparation methods and less involved in the morphology of yttrium silicate, etc. The effect of controllable particle morphology, simple process preparation and easy availability of raw materials

Inactive Publication Date: 2009-10-14
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, and its application is limited due to its large volume
YCl 3 , PrOH, TEOS, etc. as raw materials, Y was prepared by the sol-gel method 2 SiO 5 , the process is complex, the cycle is long, and there are impurities. There is no more detailed report on the impact of the process on the structure
Ana I.Becerro et al. (Ana I.Becerro, Moise's Naranjo, Ana C.Perdigo'n, and Jose'M.Trillo Hydrothermal

Method used

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  • Preparation method of controllable yttrium silicate nano-rod
  • Preparation method of controllable yttrium silicate nano-rod

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Embodiment 1

[0016] Embodiment 1: at first, analytically pure Y (NO 3 ) 3 ·6H 2 O, Na 2 SiO 3 9H 2 Add O and NaOH into distilled water respectively, and keep stirring to prepare a transparent solution with a concentration of 0.5mol / L, in which Y(NO 3 ) 3 :Na 2 SiO 3 : The mol ratio of NaOH is 2: 1: 4, utilizes the nitric acid that mass concentration is 20% and the ammoniacal liquor of 0.1mol / L to adjust its pH value to be 10.01, and the gained solution is denoted as A; Secondly, the A solution of above-mentioned preparation is poured into In the hydrothermal reaction kettle, the filling degree is controlled at 60%, and then the hydrothermal reaction kettle is sealed, and it is placed in a temperature-pressure dual-control microwave hydrothermal reactor, and the hydrothermal temperature is controlled at 180°C for 25 minutes. After the reaction, it will naturally After cooling to room temperature, the resulting solution was designated as B; then, the hydrothermal reaction vessel was ...

Embodiment 2

[0018] Embodiment 2: at first, analytically pure Y (NO 3 ) 3 ·6H 2 O, Na 2 SiO 3 9H 2 Add O and NaOH into distilled water respectively, 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 mol ratio of NaOH is 2: 2: 2, utilizes mass concentration to be that the nitric acid of 20% and the ammoniacal liquor of 0.1mol / L regulate its pH value to be 6.40, and the gained solution is denoted as A; Secondly, the A solution of above-mentioned preparation is poured into In the hydrothermal reaction kettle, the filling degree is controlled at 80%, and then the hydrothermal reaction kettle is sealed, and it is placed in a temperature-pressure dual-control microwave hydrothermal reaction instrument, and the hydrothermal temperature is controlled at 120°C for 60 minutes. After the reaction, it will naturally After cooling to room temperature, the resulting solution was denoted as B; then, the hydrothermal reactio...

Embodiment 3

[0019] Embodiment 3: at first, analytically pure Y (NO 3 ) 3 ·6H 2 O, Na 2 SiO 3 9H 2 Add O and NaOH to distilled water respectively, and keep stirring to prepare a transparent solution with a concentration of 0.6mol / L, in which Y(NO 3 ) 3 :Na 2 SiO 3: The mol ratio of NaOH is 2: 1.3: 6, utilizes mass concentration to be that the nitric acid of 20% and the ammoniacal liquor of 0.1mol / L regulate its pH value to be 4, and the gained solution is denoted as A; Next, the A solution of above-mentioned preparation is poured into In the hydrothermal reaction kettle, the filling degree is controlled at 40%, then the hydrothermal reaction kettle is sealed, and it is placed in a microwave hydrothermal reaction instrument with dual temperature and pressure control, and the hydrothermal temperature is controlled at 210°C for 10 minutes. After cooling to room temperature, the resulting solution was designated as B; then, the hydrothermal reaction vessel was opened, and the product w...

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Abstract

The invention relates to a preparation method of a controllable yttrium silicate nano-rod. The preparation method comprises the following steps: respectively adding NaOH and analytically pure (NO3)3.6H2O and Na2SiO3.9H2O into distilled water, adjusting the pH to 4-13 and obtaining a solution A; adding the solution A into a hydro-thermal reaction kettle, sealing the hydro-thermal reaction kettle, placing the hydro-thermal reaction kettle into a temperature and pressure double-control microwave hydro-thermal reaction instrument, naturally cooling to room temperature after reaction, and obtaining a solution B; opening the hydro-thermal reaction kettle, collecting the product through filtering, washing the product by respectively adopting de-ionized water and absolute ethyl alcohol or isopropanol, drying the product in an electrothermal blowing dry box and obtaining a final product, i.e. yttrium silicate nano-powder. The invention adopts microwave hydro-thermal method to synthesize yttrium silicate nano-crystal, and then controls the yttrium silicate nano-structure through processes of anneal, and the like. The invention has the advantages of simple process preparation, convenient operation, easily obtained materials, low preparation cost, short reaction period, low temperature and good repetitiveness. The yttrium silicate nano-powder prepared by the method has narrow distribution of grain diameter, controllable crystal grain shape and higher purity.

Description

technical field [0001] The invention relates to a preparation method of yttrium silicate, in particular to a preparation method of controlled yttrium silicate nanorods. Background technique [0002] The structural characteristics and a series of excellent physical and chemical properties of yttrium silicate materials make it possible to be used as high-temperature anti-oxidation coating materials, optical matrix materials and Dielectric materials, etc. At present, the methods for preparing yttrium silicate crystals mainly include solid-state reaction method, hydrothermal method and sol-gel method. However, due to the many crystal forms and complex structures of yttrium silicate, the above-mentioned methods generally require high temperature (such as 1500-1700°C for solid-state reaction method) or long time (such as 24-200h for hydrothermal method) to obtain silicic acid with expected structure. Yttrium crystals, and the microscopic morphology of the prepared yttrium silica...

Claims

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Application Information

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IPC IPC(8): C30B7/10C30B29/34C30B29/62C30B33/02C01B33/20C01F17/00
Inventor 曹丽云许斌生黄剑锋
Owner SHAANXI UNIV OF SCI & TECH
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