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Novel method for in situ preparing nano-zinc borate crystal whisker in normal pressure normal pressure liquid phase

A nano-zinc borate, in-situ preparation technology, applied in chemical instruments and methods, solutions from room temperature liquid solvents, single crystal growth, etc. Complex operation and other problems, to achieve high economic value and social value, improve market competitiveness, simple preparation process effect

Inactive Publication Date: 2008-11-05
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Some whisker preparation methods in China mainly include hydrothermal method and solid-phase method, both of which have limitations. The former has higher requirements for experimental equipment, and needs to use a reactor to complete the experiment, and the output is low. It is complex and virtually increases the cost; while the latter requires high-temperature calcination, which will inevitably increase the particle size of the product, and the high-temperature calcination consumes a lot of energy, the production cycle is long, and the use of flux increases the cost. At the same time The emitted gas is easy to pollute the environment, and the quality of the obtained whiskers is not as good as that of the hydrothermal method
Therefore, these unfavorable factors will cause the economic and social benefits of the product to be lost
[0005] So far, there are no literature and patent reports on the synthesis of nano-zinc borate whiskers as a reinforcing agent at home and abroad, especially there is no research report on the synthesis of nano-zinc borate whiskers by in-situ one-step precipitation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] 1. Add 50ml of Na with a molar content of 0.1mol / l to the three-necked flask 2 B 4 o 7 10H 2 O placed in a 70°C water bath;

[0012] 2. Under stirring, add 10ml of 2mol / l Zn(NO 3 ) 2 ·6H 2 O solution;

[0013] 3. Use alkali to adjust the pH value of the solution;

[0014] 4. Keep the temperature and continue to stir for 7 hours;

[0015] 5. Filter and wash the above precipitate;

[0016] 6. Dehydration and drying at 60°C, and grinding to obtain zinc borate crystal powder with irregular morphology.

Embodiment 2

[0018] 1. Add 50ml of Na with a molar content of 0.1mol / l to the three-necked flask 2 B 4 o 7 10H 2 O was placed in a water bath at 50°C, and the cationic surfactant was added and stirred evenly.

[0019] 2. Under stirring, add 10ml of 2mol / l Zn(NO 3 ) 2 ·6H 2 O solution;

[0020] 3. Use alkali to adjust the pH value of the solution;

[0021] 4. Keep the temperature and continue to stir for 7 hours;

[0022] 5. Filter and wash the above precipitate;

[0023] 6. Dehydration and drying at 60°C, and grinding to obtain flaky zinc borate crystal powder.

Embodiment 3

[0025] 1. Add 50ml of Na with a molar content of 0.1mol / l to the three-necked flask 2 B 4 o 7 10H 2 O was placed in a 70°C water bath, and the cationic surfactant was added and stirred evenly.

[0026] 2. Under stirring, add 10ml of 2mol / l Zn(NO 3 ) 2 ·6H 2 O solution;

[0027] 3. Use alkali to adjust the pH value of the solution;

[0028] 4. Keep the temperature and continue to stir for 7 hours;

[0029] 5. Filter and wash the above precipitate;

[0030] 6. Dehydrate and dry at 60°C, and grind to obtain nano-zinc borate whisker powder with a diameter of 20nm-40nm, a length of 500nm-1μm, and an aspect ratio of 25-50.

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Abstract

The invention relates to a liquidoid in situ method for preparing a nano zinc borate crystal whisker under normal pressure and low temperature, which comprises following steps: 50 milliliter of a borax solution with the concentration of 0.05 to 0.2 mol per liter is placed into a three-necked bottle, an aqueous solution of a cation surfactant is added and agitated evenly, 10 milliliter of a zinc salt with the concentration of 1 to 2 mol per liter is then added, temperature is heated until 50 to 90 DEG C, and crystallization is implemented by 7 to 10 hours of agitation at constant temperature; a white deposition that is obtained is filtered, washed and dried at the temperature of 50 to 90 DEG C, thus obtaining powder of the nano zinc borate crystal whisker with the diameter of 20 nm to 40 nm, the length of 500 nm to 1 um and the slenderness ratio of 25 to 50. The liquidoid in situ method for preparing the nano zinc borate crystal whisker is characterized in that the method has simple preparation techniques, does not use a fluxing agent and a high-pressure reaction kettle, does not need high-temperature calcinations, does not generate pollution, and has low cost, high productivity and higher economical and social values.

Description

technical field [0001] The invention relates to a method for preparing zinc borate whiskers, in particular to a new method for preparing nano-sized zinc borate whiskers in situ in a normal-pressure low-temperature liquid phase. Background technique [0002] Whiskers refer to a fiber grown in the form of a single crystal under artificially controlled conditions. Its diameter is very small (on the order of nanometers or micrometers), and it does not contain defects (grain boundaries, dislocations, holes, etc.) that usually exist in materials. , its atomic arrangement is highly ordered, so its strength is close to the theoretical value of a complete crystal. Due to the potential of achieving high strength in composites reinforced with whiskers, the research and development of whiskers has received high attention. Although nearly a hundred experimental products of whiskers of different materials have been developed in the 1960s, they are rarely of practical value due to the com...

Claims

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Application Information

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IPC IPC(8): C30B29/22C30B29/62C30B7/14
Inventor 田玉美郑云辉赵旭刘艳华郭玉鹏周兵王子忱
Owner JILIN UNIV
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