Method for preparing nano nickel borate whiskers

A nano-boric acid and whisker technology is applied in the field of preparation of nano-nickel borate whiskers. Effect

Active Publication Date: 2010-09-29
海宁市黄湾镇资产经营有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are many defects in these methods: complex equipment, harsh preparation conditions (must be carried out under the protection of inert gas), low yield, inconsistent product morphology (dispersion of dimension distribution)
Japanese patent JP4280899A uses nickel sulfate, boric acid and alkali metal sulfate double salt as raw materials, and can obtain whiskers with a diameter of 0.2 to 0.3 μm and an aspect ratio of 10 to 100 by using the molten salt method, but there are still complex formulas and roasting problems. Due to the disadvantages of high temperature and low yield, industrialization cannot be realized

Method used

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  • Method for preparing nano nickel borate whiskers
  • Method for preparing nano nickel borate whiskers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 0.7269gNi(NO 3 ) 3 ·6H 2 O, 0.4637g H 3 BO 3 Dissolve in 50ml of distilled water, then add 2.6268g of citric acid, stir the solution evenly with magnetic stirring, after stirring at room temperature for 4 hours, dry the mixture in an oven at 120°C to obtain a brown gel, and heat the gel at 750°C Roasting for 4 hours, the green powder was obtained, washed 4 times with 0.1mol / L hydrochloric acid, and the washing liquid was characterized by XRD, and the spectrum showed only Ni 3 B 2 o 6 Crystal diffraction peaks, no impurities such as diboron trioxide, then washed once with deionized water, filtered, and the filter cake was dried at 100°C to obtain Ni 3 (BO 3 ) 2 whiskers. Detected by XRD, as attached figure 1 As shown, the resulting Ni 3 (BO 3 ) 2 It is a pure substance without impurities such as diboron trioxide; after TEM detection, if attached figure 2 As shown, the whiskers are uniformly distributed in size, with a diameter of 150-250 nm and a len...

Embodiment 2

[0022] Weigh 0.7281gNi(NO 3 ) 3 ·6H 2 O, 0.3092g H 3 BO 3 Dissolve in 50ml of distilled water, then add 2.6159g of citric acid, stir the solution evenly at room temperature, and after stirring at room temperature for 8 hours, dry the mixture in an oven at 150°C to obtain a brown gel, and heat the gel at 750°C Calcined at low temperature for 10 hours to obtain green powder, which was directly washed with 60°C ionized water for 3 times until the washing liquid was characterized by XRD, and the spectrum showed that only Ni 3 B 2 o 6 Crystal diffraction peaks, no impurities such as diboron trioxide, washed once with deionized water, filtered, and dried at 100°C to obtain Ni 3 (BO 3 ) 2 Whiskers, Ni detected by TEM and XRD 3 (BO 3 ) 2 It is a single crystal structure, and the whiskers are uniformly distributed in size, with a diameter of 50-100nm and a length of 400-800nm.

Embodiment 3

[0024] Weigh 0.6572gNiSO 4 ·6H 2 O, 0.4637g H 3 BO 3 Dissolve in 50ml of distilled water, then add 2.6458g of citric acid, stir the solution evenly with magnetic stirring, and after stirring at room temperature for 16 hours, dry the mixture in an oven at 110°C to obtain a brown gel, and heat the gel at 850°C Calcined for 12 hours to obtain a green powder, washed 3 times with 0.1mol / L hydrochloric acid until the washing liquid was characterized by XRD, and the spectrum showed that only Ni 3 B 2 o 6 Crystal diffraction peaks, no impurities such as diboron trioxide, washed once with deionized water, filtered, and dried at 80°C to obtain Ni 3 (BO 3 ) 2 Whiskers, Ni detected by TEM and XRD 3 (BO 3 ) 2 It is a single crystal structure, and the whiskers are uniformly distributed in size, with a diameter of 200-300nm and a length of 1.5-2.5μm.

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Abstract

The invention relates to a method for preparing nano nickel borate whiskers. The nano nickel borate whiskers are prepared by a sol-gel method, and the method comprises the following steps of: (1) adding water into inorganic nickel salt, boric acid and citric acid in an amount-of-substance ratio of 1:1-10:1-10 to prepare aqueous solution, controlling the concentration of the inorganic nickel salt in the aqueous solution to between 0.1 and 2.0mol / L, stirring at room temperature for 2 to 72 hours, and drying at the temperature of between 40 and 300 DEG C to obtain coffee dried gel; (2) sintering the dried gel obtained by the step (1) at the temperature of between 500 and 1,500 DEG C for 2 to 72 hours in air atmosphere to obtain green powder; and (3) post-treating the green powder obtained by the step (2) to prepare the nano nickel borate whiskers shown as Ni3B2O6. Compared with the traditional molten salt growth method, the method has the advantages of simple formula, easy operation, high yield, low sintering temperature and the like, and is favorable for industrialization.

Description

(1) Technical field [0001] The invention relates to a method for preparing nano-nickel borate whiskers, in particular to a method for preparing nano-nickel borate whiskers by a sol-gel method. (2) Background technology [0002] Inorganic materials play an important role in the national economy and national defense construction. As a single crystal material, whisker has a nearly complete structure, and its strength and modulus are close to theoretical values. At the same time, it has a high aspect ratio, similar to short fibers. , is a very good strengthening and toughening modified material. Among many whisker materials, borate whiskers have the characteristics of abundant raw materials, high cost performance, and wide application. They have broad application prospects in aluminum, magnesium and alloys, plastic composite materials, polymer materials, and engineering plastics to improve Its compression resistance, tensile strength, enhanced bonding ability and corrosion resi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/10C30B29/62
Inventor 陈爱民胡锋超倪哲明
Owner 海宁市黄湾镇资产经营有限公司
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