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Method for preparing single-phase ZrB2 powder employing triethyl borate as boron source through sol-gel method

A technology of triethyl borate and gel method, applied in boron/boride, metal boride and other directions, can solve problems such as unfavorable preparation process and subsequent material processing and development, and achieves low production cost, simple equipment and reaction conditions. mild effect

Inactive Publication Date: 2015-09-02
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the above methods, the inorganic acid—boric acid is selected as the boron source, which increases the acidity of the system, which is not conducive to the preparation process and the processing and development of subsequent materials.

Method used

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  • Method for preparing single-phase ZrB2 powder employing triethyl borate as boron source through sol-gel method
  • Method for preparing single-phase ZrB2 powder employing triethyl borate as boron source through sol-gel method
  • Method for preparing single-phase ZrB2 powder employing triethyl borate as boron source through sol-gel method

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Experimental program
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Effect test

Embodiment 1

[0060] The present invention proposes a single-phase ZrB prepared by a sol-gel method using triethyl borate as a boron source 2 The method of powder, this method comprises the following steps:

[0061] Step 1: Dissolve D-fructose in acetic acid CH 3 In COOH (mass percentage concentration 99.9%), magnetically stir in a water bath at 80°C until the first solution is formed; the stirring speed is 200r / min;

[0062] Step 2: Place the first solution in cooling water, and cool it down to 60°C at a cooling rate of 3°C / min to form a second solution;

[0063] Step 3: Mix triethyl borate (97% by mass concentration) with zirconium n-propoxide (70% by mass percent) to form a third solution; the mixing conditions are: mixing temperature 20°C, stirring speed 200r / min ;

[0064] Step 4: at a stirring speed of 200r / min, the third solution is added to the second solution to form a homogeneous solution;

[0065] Dosage: Add 1.85g of D-fructose, 4.09g of zirconium n-propoxide, and 10ml of ac...

Embodiment 2

[0074] The present invention proposes a single-phase ZrB prepared by a sol-gel method using triethyl borate as a boron source 2 The method of powder, this method comprises the following steps:

[0075] Step 1: Dissolve D-fructose in acetic acid CH 3 In COOH (mass percentage concentration 99.9%), magnetically stir in a water bath at 75°C until the first solution is formed; the stirring speed is 400r / min;

[0076] Step 2: Place the first solution in cooling water, and cool it down to 60°C at a cooling rate of 6°C / min to form a second solution;

[0077] Step 3: triethyl borate (mass percentage concentration 97%) is mixed with n-propoxide zirconium (mass percentage concentration 70%) to form a third solution; the mixing conditions are: mixing temperature 25°C, stirring speed 400r / min ;

[0078] Step 4: at a stirring speed of 200r / min, the third solution is added to the second solution to form a homogeneous solution;

[0079] Dosage: Add 2.5g of D-fructose, 5.3g of zirconium n-...

Embodiment 3

[0088] The present invention proposes a single-phase ZrB prepared by a sol-gel method using triethyl borate as a boron source 2 The method of powder, this method comprises the following steps:

[0089] Step 1: Dissolve D-fructose in acetic acid CH 3 In COOH (mass percentage concentration 99.9%), magnetically stir in a water bath at 82°C until the first solution is formed; the stirring speed is 300r / min;

[0090] Step 2: Place the first solution in cooling water, and cool it down to 65°C at a cooling rate of 5°C / min to form a second solution;

[0091] Step 3: triethyl borate (mass percentage concentration 97%) is mixed with n-propoxide (mass percentage concentration 70%) to form a third solution; the mixing conditions are: mixing temperature 20°C, stirring speed 300r / min ;

[0092] Step 4: at a stirring speed of 200r / min, the third solution is added to the second solution to form a homogeneous solution;

[0093] Dosage: Add 1.4g of D-fructose, 3.2g of zirconium n-propoxide, a...

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Abstract

The invention discloses a method for preparing single-phase ZrB2 powder employing triethyl borate as a boron source through a sol-gel method. The method comprises the following steps: by virtue of the sol-gel method, with D-fructose, triethyl borate and zirconium n-propoxide as raw materials, obtaining precursor gel powder of ZrB2 by adjusting the molar ratio of B to Zr; and carrying out preheating and burning at different heating and cooling rates under protection of argon and cooling along with a furnace, so as to obtain the single-phase pure ZrB2 powder. The precursor gel powder obtained by reaction can reach uniform atomic scale and molecular scale; and the components of a final synthetic material can be strictly controlled by calculating the components of reactants. In addition, through simple process and cheap equipment, the gel or powder with large specific surface area can be obtained; and the purity of the product is high.

Description

technical field [0001] The invention relates to a method for preparing ZrB by sol-gel method 2 Powder, more specifically, refers to a liquid organic ester as a boron source, D-fructose as a carbon source, organic alkoxide as a zirconium source, and obtains ZrO through hydrolysis and polycondensation. 2 Preparation of ZrB from Precursor by Sol-Gel Method 2 powder method. Background technique [0002] ZrB 2 Ceramics are widely used in high-temperature structural ceramic materials, composite materials, refractory materials and It has been widely developed and utilized in nuclear control materials and other fields, and is one of the most promising ultra-high temperature ceramic materials. [0003] The basic principle of the sol-gel method is: the metal alkoxide or inorganic salt is hydrolyzed to directly form a sol or a sol is formed by degelation, then the solute is polymerized and gelled, and then the gel is dried and roasted to remove the organic components, and finally o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/04
Inventor 李锐星赵月
Owner BEIHANG UNIV
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