CN115676830A - Preparation method of zirconium carbide powder - Google Patents
Preparation method of zirconium carbide powder Download PDFInfo
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- CN115676830A CN115676830A CN202211116556.8A CN202211116556A CN115676830A CN 115676830 A CN115676830 A CN 115676830A CN 202211116556 A CN202211116556 A CN 202211116556A CN 115676830 A CN115676830 A CN 115676830A
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Abstract
The invention relates to the technical field of application, in particular to a preparation method of zirconium carbide powder, which specifically comprises the following steps: with zirconium nitrate (Zr (NO) 3 ) 4 ·5H 2 O) as a zirconium source, sucrose as a carbon source and the mol number of the zirconium source is calculated by the mol number of the zirconium element in the zirconium source; the mol number of the carbon source is calculated by the mol number of carbon elements in the carbon source, the mixture is prepared into aqueous solution according to the mol ratio of 1:3, 1:4 and 1:5 of the zirconium source and the carbon source, the aqueous solution is placed into a high-pressure reaction kettle for hydrothermal reaction, then the hydrothermal product is obtained by drying, the hydrothermal product is heated, the heating temperature is 1300-1600 ℃, the heat preservation time is 1-2 h, and furnace cooling is carried out, thus finally obtaining the zirconium carbide powder. The invention has the beneficial effects that: the method has the advantages of low implementation cost, simple synthesis process and easy control of the process, and the prepared ZrC powder particles are fine and reach the nanometer level, have good powder particle dispersibility and uniform particle size distribution, have good social benefit and are suitable for popularization and use.
Description
Technical Field
The invention relates to the technical field of preparation and application of zirconium carbide powder, in particular to a preparation method of zirconium carbide powder.
Background
ZrC has high melting point (3550 ℃), high hardness (25 GPa), strong wear resistance and corrosion resistance and excellent electric and heat conducting properties, and is widely applied to the fields of cutter cutting, electronic components, high-temperature structural materials and the like. In addition, the ZrC has a low neutron absorption cross section and good radiation resistance, so that the ZrC also has important application in the field of nuclear reactor core materials.
Chinese patent with publication number CN102491327B discloses zirconium carbide powder and a preparation method thereof. The technical scheme is as follows: firstly, 8 to 22 weight percent of zirconium dioxide or zirconium oxychloride, 65 to 80 weight percent of alkali metal sulfate, 1 to 3 weight percent of carbon black and 10 to 20 weight percent of aluminum powder are taken as raw materials and are uniformly mixed; then the evenly mixed raw materials are placed in a tubular electric furnace, the temperature is raised to 950-1150 ℃ at the heating rate of 2-8 ℃/min under the atmosphere of inert gas, and the temperature is kept for 1-6 hours; then putting the obtained product into H with the concentration of 0.5-3 mol/L 2 SO 4 Soaking the zirconium carbide powder in the solution for 2 to 8 hours, filtering, washing the zirconium carbide powder by using deionized water until the pH value of a washing liquid is 7.0, and finally drying the zirconium carbide powder for 10 to 24 hours at the temperature of 110 ℃ to obtain the zirconium carbide powder. The invention has the characteristics of low raw material price, simple synthesis process, easy control of the synthesis process and great industrialization prospect; the prepared zirconium carbide powder has high activity and purity, and the particle size distribution of the powder particles is uniform and is 80-300 nm. The patent has the defects of high cost for preparing zirconium carbide powder, large particle size of the prepared zirconium carbide powder and poor dispersibility of the powder particles.
At present, the traditional method for preparing ZrC at home and abroad comprises the following steps: direct synthesis, self-propagating high temperature synthesis, high energy ball milling, sol-gel, carbothermic, and the like. ZrC powder particles prepared by the direct synthesis method are large in size, the synthesis process of the self-propagating high-temperature synthesis method is not easy to control, the product performance is easily influenced, impurities are easily introduced in the high-energy ball milling process, powder particles produced by the sol-gel method are fine, but the production process is complex and not suitable for mass production, the production process of the carbothermic method is simple, and the purity of the produced product is not high.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of zirconium carbide powder, which has the advantages of low implementation cost, simple synthesis process and easily controlled process, and the prepared ZrC powder has fine particles reaching the nanometer level, good powder particle dispersibility and uniform particle size distribution.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of zirconium carbide powder comprises the following steps:
the method comprises the following steps: with zirconium nitrate (Zr (NO) 3 ) 4 ·5H 2 O) as a zirconium source, sucrose as a carbon source and the mol number of the zirconium source is calculated by the mol number of the zirconium element in the zirconium source; the mol number of the carbon source is calculated by the mol number of carbon elements in the carbon source, and the mixture is prepared into aqueous solution according to the mol ratio of the zirconium source to the carbon source of 1:3, 1:4 and 1:5;
step two: putting the aqueous solution into a high-pressure reaction kettle for hydrothermal reaction at the temperature of 170-250 ℃ for 15-25 h, and then drying to obtain a hydrothermal product;
step three: heating the hydrothermal product at 1300-1600 ℃ for 1-2 h, cooling along with the furnace under the protection of inert gas in the heating process, and finally grinding to obtain zirconium carbide powder. The method has the advantages of low implementation cost, simple synthesis process and easy control of the process, and the prepared ZrC powder has fine particles.
The invention has further technical improvements that: and step two, putting the aqueous solution into a high-pressure reaction kettle for hydrothermal reaction, wherein the reaction temperature is 200 ℃, the reaction time is 20 hours, the powder particles have good dispersibility, and the uniform particle size distribution reaches the nanometer level.
The invention has further technical improvements that: and in the second step, after the hydrothermal reaction of the aqueous solution, drying is carried out in a vacuum drying mode at the temperature of 60 ℃ for 9 hours.
The invention has further technical improvements that: heating the hydrothermal product in the third step, wherein the heating temperature is 1500 ℃, and the heat preservation time is as follows: and (5) h.
The invention has the beneficial effects that:
the method has the advantages of low implementation cost, simple synthesis process and easy control of the process, and the prepared ZrC powder has fine particles, good dispersibility of the powder particles and uniform particle size distribution.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
A preparation method of zirconium carbide powder specifically comprises the following steps:
the method comprises the following steps: with zirconium nitrate (Zr (NO) 3 ) 4 ·5H 2 O) as a zirconium source, sucrose as a carbon source and the mol number of the zirconium source is calculated by the mol number of the zirconium element in the zirconium source; the mol number of the carbon source is calculated by the mol number of carbon elements in the carbon source, and the mixture is prepared into aqueous solution according to the mol ratio of the zirconium source to the carbon source of 1:3, 1:4 and 1:5;
step two: placing the aqueous solution into a high-pressure reaction kettle for hydrothermal reaction at the reaction temperature of 200 ℃ for 20 hours, and then carrying out vacuum drying at the temperature of 60 ℃ for 9 hours to obtain a hydrothermal product, wherein the powder particles have good dispersibility and uniform particle size distribution;
step three: and heating the hydrothermal product at 1500 ℃, keeping the temperature for 1.5h, cooling along with the furnace, protecting by inert gas in the heating process, and finally grinding to obtain zirconium carbide powder.
Example 2
A preparation method of zirconium carbide powder specifically comprises the following steps:
the method comprises the following steps: with zirconium nitrate (Zr (NO) 3 ) 4 ·5H 2 O) as a zirconium source, sucrose as a carbon source and the mol number of the zirconium source is calculated by the mol number of the zirconium element in the zirconium source; the mol number of the carbon source is calculated by the mol number of carbon elements in the carbon source according to the zirconium source and the carbonMixing the raw materials according to the molar ratio of 1:3, 1:4 and 1:5 to prepare an aqueous solution;
step two: putting the aqueous solution into a high-pressure reaction kettle for hydrothermal reaction at 180 ℃ for 19h, and drying to obtain a hydrothermal product;
step three: and heating the hydrothermal product at 1400 ℃, keeping the temperature for 1h, cooling along with the furnace, protecting by inert gas in the heating process, and finally grinding to obtain the zirconium carbide powder.
Example 3
A preparation method of zirconium carbide powder specifically comprises the following steps:
the method comprises the following steps: with zirconium nitrate (Zr (NO) 3 ) 4 ·5H 2 O) as a zirconium source, sucrose as a carbon source and the mol number of the zirconium source is calculated by the mol number of the zirconium element in the zirconium source; the mol number of the carbon source is calculated by the mol number of carbon elements in the carbon source, and the mixture is prepared into aqueous solution according to the mol ratio of the zirconium source to the carbon source of 1:3, 1:4 and 1:5;
step two: putting the aqueous solution into a high-pressure reaction kettle for hydrothermal reaction at the temperature of 190 ℃ for 21 hours, and then drying to obtain a hydrothermal product;
step three: heating the hydrothermal product at 1600 ℃ for 2h, cooling along with the furnace, protecting with inert gas in the heating process, and finally grinding to obtain zirconium carbide powder
The method has the advantages of low implementation cost, simple synthesis process and easy control of the process, and the prepared ZrC powder particles are fine and reach the nanometer level, have good powder particle dispersibility and uniform particle size distribution, have good social benefit and are suitable for popularization and use.
Comparative example
With zirconium nitrate (Zr (NO) 3 ) 4 ·5H 2 O) as a zirconium source, sucrose as a carbon source, and the mol number of the zirconium source is the zirconium element in the zirconium sourceMolar basis of the element; the moles of the carbon source are based on the moles of carbon in the carbon source. Mixing a zirconium source and a carbon source according to a molar ratio of 1:3 to prepare an aqueous solution, putting the aqueous solution into a high-pressure reaction kettle for hydrothermal reaction at 200 ℃ for 20 hours, and then drying (drying in a vacuum manner, at 60 ℃ for 12 hours) to obtain a hydrothermal product. Heating the hydrothermal product at the heating temperature: 1200 ℃, heat preservation time: and 2h, cooling along with the furnace, and finally grinding to obtain a final product, wherein the final product is zirconium oxide through XRD detection and analysis.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the embodiments and descriptions given above are only illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A preparation method of zirconium carbide powder is characterized by comprising the following steps: the method specifically comprises the following steps:
the method comprises the following steps: taking zirconium nitrate as a zirconium source, taking cane sugar as a carbon source, and counting the moles of the zirconium source by the moles of a zirconium element in the zirconium source; the mol number of the carbon source is calculated by the mol number of carbon elements in the carbon source, and the mixture is prepared into aqueous solution according to the mol ratio of the zirconium source to the carbon source of 1:3, 1:4 and 1:5;
step two: putting the aqueous solution into a high-pressure reaction kettle for hydrothermal reaction at the temperature of 170-250 ℃ for 15-25 h, and then drying to obtain a hydrothermal product;
step three: heating the hydrothermal product at 1300-1600 ℃ for 1-2 h, cooling along with the furnace under the protection of inert gas in the heating process, and finally grinding to obtain zirconium carbide powder.
2. The method for producing a zirconium carbide powder according to claim 1, characterized in that: and in the second step, the aqueous solution is placed into a high-pressure reaction kettle for hydrothermal reaction, the reaction temperature is 200 ℃, and the reaction time is 25 hours.
3. The method for preparing zirconium carbide powder according to claim 1, characterized in that: and in the second step, after the hydrothermal reaction of the aqueous solution, the drying mode is vacuum drying at the temperature of 60 ℃ for 9 hours.
4. The method for preparing zirconium carbide powder according to claim 1, characterized in that: heating the hydrothermal product in the third step, wherein the heating temperature is 1500 ℃, and the heat preservation time is as follows: and (5) h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515164A (en) * | 2011-11-30 | 2012-06-27 | 北京科技大学 | Preparation method of zirconium carbide ceramic powder |
| CN103626179A (en) * | 2013-11-19 | 2014-03-12 | 陕西科技大学 | Method for preparing nanometer zirconium carbide powder |
| CN107721429A (en) * | 2017-11-15 | 2018-02-23 | 中国科学院福建物质结构研究所 | Zirconium carbide silicon carbide composite powder body material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515164A (en) * | 2011-11-30 | 2012-06-27 | 北京科技大学 | Preparation method of zirconium carbide ceramic powder |
| CN103626179A (en) * | 2013-11-19 | 2014-03-12 | 陕西科技大学 | Method for preparing nanometer zirconium carbide powder |
| CN107721429A (en) * | 2017-11-15 | 2018-02-23 | 中国科学院福建物质结构研究所 | Zirconium carbide silicon carbide composite powder body material and preparation method thereof |
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