CN111003696B - Preparation method of nano zirconium nitride powder - Google Patents
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Abstract
A preparation method of nano zirconium nitride powder relates to the technical field of preparation of high-melting-point nitride powder. Pretreating zirconium dioxide, preparing zirconium nitride by a chemical vapor deposition method, and finally grinding and grading to obtain the nano zirconium nitride powder. Zirconium dioxide is required to be pretreated before preparing zirconium nitride, and the silica sol obtained through reaction is used for polishing the surface of zirconium dioxide powder, so that a relatively smooth surface can be obtained, the reaction activity of the zirconium dioxide powder is improved, and the subsequent generation of high-purity zirconium nitride powder is facilitated. The invention realizes the preparation of the high-purity nano zirconium nitride powder, has the advantages of simple and convenient process, low cost, uniform particle size distribution of the product, high product purity and the like, and can be used for large-scale production.
Description
Technical Field
The invention relates to the technical field of preparation of high-melting-point nitride powder, in particular to a preparation method of nano zirconium nitride powder.
Background
Nitride powders having high melting point, high hardness, high chemical stability, and excellent electrical and optical properties have attracted general attention. The unique physical and chemical properties make the nitride have wide application in the fields of semiconductor devices, microelectronics, porous ceramics and the like.
ZrN is a refractory hard compound, has high decomposition temperature and good chemical stability, so the ZrN has good high temperature resistance, corrosion resistance and wear resistance, is a good high-temperature structural material, a superhard tool material and a surface protection material, has a golden yellow color with lower brightness which is popular among people, is suitable for the field of titanium nitride which is not suitable for coating, and has high corrosion resistance, good smooth surface and ductility. The method is widely applied to daily hardware workpieces such as hardware, building materials, bathrooms and the like. The method is widely applied to the fields of building decoration, household appliances, watches, jewelry, mobile phones and the like, thereby becoming a research object with high importance in the decoration coating industry.
Currently, zirconium nitride powder is prepared mainly by conventional methods for synthesizing nitrides, such as solid-phase reaction synthesis and gas-phase reaction synthesis, among which the reductive nitridation method and the Chemical Vapor Deposition (CVD) method are commonly used. The reduction nitridation method uses ammonia gas and metal oxide as main raw materials to prepare nitride powder. Chemical Vapor Deposition (CVD) is carried out by reacting a metal and a volatile compound (halide or alkyl compound) of the metal with N 2 Atmosphere is introduced into the reaction chamber with NH 3 The reaction deposits the crystal grains of the nitride from the gas phase, and then the crystal grains are aggregated into nitride powder. However, the zirconium nitride powder prepared by the above method also has many disadvantages and defects, such as the need to prepare a reactant precursor with a suitable size and structure, low purity of the powder obtained by the reaction, and easy generation of environmental problems.
Disclosure of Invention
Aiming at the defects of impure products, difficult control of reaction, uneven particle size distribution and the like in the preparation of the zirconium nitride powder, the invention provides the preparation method of the nano zirconium nitride powder, and the preparation method has the advantages of simple and convenient operation, controllable particle size distribution of the products, higher purity and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the preparation process of nanometer zirconium nitride powder includes pre-treatment of zirconium dioxide, chemical vapor deposition to prepare zirconium nitride, and final grinding to obtain nanometer zirconium nitride powder.
As a preferred technical solution of the present invention, the step of pretreating zirconium dioxide comprises:
firstly, adding absolute ethyl alcohol into zirconium dioxide, and performing ultrasonic dispersion; the weight ratio of the added zirconium dioxide to the absolute ethyl alcohol is 1: 15-25; then adding a silane coupling agent KH-792 and polyvinyl alcohol, heating to 40-80 ℃, and stirring for reaction for 10-30 hours; wherein the adding weight ratio of the zirconium dioxide to the silane coupling agent KH-792 to the polyvinyl alcohol is 1: 2-5: 1-3; standing and aging for 10-30 h after the reaction is finished, and drying after solid-liquid separation to obtain the pretreated zirconium dioxide.
As a preferred technical scheme of the invention, the step of preparing the zirconium nitride by the chemical vapor deposition method comprises the following steps:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 200-500 ℃ and 800-1100 ℃; continuously introducing argon into the heating area, the high-temperature area and the cooling area, and simultaneously introducing ammonia into the high-temperature area; enabling the mixed powder of zirconium dioxide and magnesium powder to enter a heating area of a reactor through automatic feeding equipment, staying for 1-5 minutes, then continuing to advance to a high-temperature area, and staying for 10-30 minutes; leaving the high-temperature area after the reaction is finished, and entering a cooling area for cooling; cooling to room temperature to obtain a mixture of zirconium nitride and magnesium nitride; and removing magnesium nitride from the mixture through acid washing and alcohol washing, and then drying to obtain zirconium nitride powder.
Further, the weight ratio of the ammonia gas to the zirconium dioxide is 4-10: 1.
further, the weight ratio of zirconium dioxide to magnesium powder is 1: 2 to 5.
As a preferred technical scheme of the invention, the step of obtaining the nano zirconium nitride powder by grinding and grading comprises the following steps:
adding zirconium nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid; firstly, controlling a stirring shaft of a stirring mill to keep high-speed running for 10-20 minutes in the same direction to generate violent collision among materials, then changing the rotating direction of the stirring shaft, reversely running for 15-25 minutes at high speed to further grind zirconium nitride powder, and then grading to obtain the nano zirconium nitride powder with uniform particle size distribution.
Further, the solvent and the grinding aid added in the grinding machine are ethanol and quartz sand respectively.
Further, the weight ratio of the material balls in the grinding machine is 1: 3-5, wherein the weight ratio of the zirconium nitride powder, the solvent and the grinding aid is 1: 3-5: 2 to 6.
Compared with the prior art, the invention has the beneficial effects that:
1) the method realizes the preparation of the high-purity nano zirconium nitride powder, has the advantages of simple and convenient process, low cost, uniform particle size distribution of the product, high product purity and the like, and can be used for large-scale production.
2) The zirconium dioxide is required to be pretreated before the zirconium nitride is prepared, and the surface of the zirconium dioxide powder is polished by the silica sol obtained through reaction, so that a relatively smooth surface can be obtained, the reaction activity of the zirconium dioxide powder is improved, and the subsequent generation of high-purity zirconium nitride powder is facilitated. The nitridation reduction reaction is completed in an inert atmosphere, so that the influence of oxygen or air on the reaction process can be completely eliminated, and the ammonia gas is enough to ensure that the zirconium dioxide can be completely reacted.
Drawings
FIG. 1 is an XRD pattern (a) and an SEM pattern (b) before grinding for preparing zirconium nitride;
FIG. 2 is an SEM image of zirconium nitride after grinding.
Detailed Description
The invention provides a preparation method of nano zirconium nitride powder, which comprises the steps of pretreating zirconium dioxide, preparing zirconium nitride by a chemical vapor deposition method, and finally grinding and grading to obtain the zirconium nitride powder. The steps are respectively as follows:
firstly, the step of pretreating zirconium dioxide comprises the following steps:
firstly, adding absolute ethyl alcohol into zirconium dioxide, and carrying out ultrasonic dispersion. The weight ratio of the added zirconium dioxide to the absolute ethyl alcohol is 1: 15 to 25. And then adding a silane coupling agent KH-792 and polyvinyl alcohol, heating to 40-80 ℃, and stirring for reaction for 10-30 hours. Wherein the adding weight ratio of the zirconium dioxide to the silane coupling agent KH-792 to the polyvinyl alcohol is 1: 2-5: 1 to 3. Standing and aging for 10-30 h after the reaction is finished, and drying after solid-liquid separation to obtain the pretreated zirconium dioxide.
In order to improve the quality of zirconium nitride preparation, zirconium dioxide, which is a raw material, needs to be pretreated before zirconium nitride preparation, and the silica sol obtained through reaction is used for polishing the surface of zirconium dioxide powder, so that a relatively smooth surface can be obtained, the reaction activity of the zirconium dioxide powder is improved, and the subsequent high-purity zirconium nitride powder is more favorably generated.
Secondly, the step of preparing zirconium nitride by chemical vapor deposition comprises:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 200-500 ℃ and 800-1100 ℃. Argon is continuously introduced into the heating area, the high-temperature area and the cooling area, and meanwhile, ammonia is introduced into the high-temperature area.
And (3) enabling the mixed powder of zirconium dioxide and magnesium powder to enter an elevated temperature zone of the reactor through automatic feeding equipment, staying for 1-5 minutes, then continuing to advance to a high temperature zone, and staying for 10-30 minutes. The weight ratio of the ammonia gas to the zirconium dioxide is 4-10: 1. the weight ratio of zirconium dioxide to magnesium powder is 1: 2 to 5.
Leaving the high-temperature area after the reaction is finished, entering a cooling area for cooling. And cooling to room temperature to obtain a mixture of zirconium nitride and magnesium nitride. And removing magnesium nitride from the mixture through acid washing and alcohol washing, and then drying to obtain zirconium nitride powder.
It is particularly noted that the reaction is a nitridation reduction reaction carried out in an inert atmosphere, and the influence of oxygen or air on the reaction process can be completely eliminated, and the ammonia gas is sufficient to allow the zirconium dioxide to be completely reacted.
FIG. 1a is an XRD spectrum of the prepared zirconium nitride powder, and the analysis shows that the reaction product is ZrN (XRD standard spectrum: ZrN standard spectrum). FIG. 1b is an overall SEM morphology of zirconium nitride powder, which shows that the powder exists in bulk form, the particle size is over 100nm and the distribution is not uniform.
Thirdly, the step of obtaining the nano zirconium nitride powder by grinding and grading comprises the following steps:
adding zirconium nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid. Firstly, controlling a stirring shaft of a stirring mill to keep high-speed running for 10-20 minutes in the same direction to generate violent collision among materials, then changing the rotating direction of the stirring shaft, reversely running for 15-25 minutes at high speed to further grind zirconium nitride powder, and then grading to obtain the nano zirconium nitride powder with uniform particle size distribution.
The solvent and the grinding aid added in the grinding machine are respectively ethanol and quartz sand. The weight ratio of the material balls in the grinding machine is 1: 3-5, wherein the weight ratio of the zirconium nitride powder, the solvent and the grinding aid is 1: 3-5: 2 to 6.
FIG. 2 is an SEM image of the zirconium nitride powder after grinding, which shows that the zirconium nitride powder after grinding has a uniform particle size distribution with an average particle size of about 30 nm. Through detection, the purity of the prepared nano zirconium nitride powder reaches more than 99%.
The preparation method of the zirconium nitride nanopowder of the present invention is further illustrated by the following examples.
Example 1
The preparation method of the nano zirconium nitride powder comprises the following steps:
firstly, the step of pretreating zirconium dioxide comprises the following steps:
firstly, adding absolute ethyl alcohol into zirconium dioxide, and carrying out ultrasonic dispersion. The weight ratio of the added zirconium dioxide to the absolute ethyl alcohol is 1: 18. then adding a silane coupling agent KH-792 and polyvinyl alcohol, heating to 75 ℃, and stirring for reaction for 15 hours. Wherein the adding weight ratio of the zirconium dioxide to the silane coupling agent KH-792 to the polyvinyl alcohol is 1: 3: 3. standing and aging for 15h after the reaction is finished, and drying after solid-liquid separation to obtain the pretreated zirconium dioxide.
Secondly, the step of preparing zirconium nitride by chemical vapor deposition comprises:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 500 ℃ and 1000 ℃. Argon is continuously introduced into the heating area, the high-temperature area and the cooling area, and meanwhile, ammonia is introduced into the high-temperature area. The mixed powder of zirconium dioxide and magnesium powder enters the heating zone of the reactor through automatic feeding equipment and stays for 3 minutes, and then continues to move to the high-temperature zone and stays for 10 minutes. The weight ratio of the ammonia gas to the zirconium dioxide is 8: 1. the weight ratio of zirconium dioxide to magnesium powder is 1: 3. leaving the high-temperature area after the reaction is finished, entering a cooling area for cooling. And cooling to room temperature to obtain a mixture of zirconium nitride and magnesium nitride. And removing magnesium nitride from the mixture through acid washing and alcohol washing, and then drying to obtain zirconium nitride powder.
The step of obtaining zirconium nitride powder by grinding and grading comprises the following steps:
adding zirconium nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid. Firstly, controlling a stirring shaft of a stirring mill to keep high-speed running for 15 minutes in the same direction to generate violent collision among materials, then changing the rotating direction of the stirring shaft, reversely running for 15 minutes at high speed to further grind zirconium nitride powder, and then grading to obtain the zirconium nitride powder with uniform particle size distribution. The solvent and the grinding aid added in the grinding machine are respectively ethanol and quartz sand. The weight ratio of the material balls in the grinding machine is 1: 4, the weight ratio of the zirconium nitride powder, the solvent and the grinding aid is 1: 5: 3.
example 2
The preparation method of the nanometer zirconium nitride powder comprises the following steps:
firstly, the step of pretreating zirconium dioxide comprises the following steps:
firstly, absolute ethyl alcohol is added into zirconium dioxide, and ultrasonic dispersion is carried out. The weight ratio of the added zirconium dioxide to the absolute ethyl alcohol is 1: 22. then adding a silane coupling agent KH-792 and polyvinyl alcohol, heating to 55 ℃, and stirring for reaction for 25 hours. Wherein the adding weight ratio of the zirconium dioxide to the silane coupling agent KH-792 to the polyvinyl alcohol is 1: 2: 1. standing and aging for 20h after the reaction is finished, and drying after solid-liquid separation to obtain the pretreated zirconium dioxide.
Secondly, the step of preparing zirconium nitride by chemical vapor deposition comprises:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 400 ℃ and 800 ℃. Argon is continuously introduced into the heating area, the high-temperature area and the cooling area, and ammonia is introduced into the high-temperature area. The mixed powder of zirconium dioxide and magnesium powder enters the heating zone of the reactor through automatic feeding equipment and stays for 5 minutes, and then continues to move to the high-temperature zone and stays for 30 minutes. The weight ratio of the ammonia gas to the zirconium dioxide is 5: 1. the weight ratio of zirconium dioxide to magnesium powder is 1: 5. leaving the high-temperature area after the reaction is finished, entering a cooling area for cooling. And cooling to room temperature to obtain a mixture of zirconium nitride and magnesium nitride. And removing magnesium nitride from the mixture through acid washing and alcohol washing, and then drying to obtain zirconium nitride powder.
The step of obtaining zirconium nitride powder by grinding and grading comprises the following steps:
adding zirconium nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid. Firstly, controlling a stirring shaft of a stirring mill to keep high-speed running for 10 minutes in the same direction to generate violent collision among materials, then changing the rotating direction of the stirring shaft, reversely running for 20 minutes at high speed to further grind zirconium nitride powder, and then grading to obtain the zirconium nitride powder with uniform particle size distribution. The solvent and the grinding aid added in the grinding machine are respectively ethanol and quartz sand. The weight ratio of the material balls in the grinding machine is 1: 5, the weight ratio of the zirconium nitride powder, the solvent and the grinding aid is 1: 3: 6.
example 3
The preparation method of the nano zirconium nitride powder comprises the following steps:
firstly, the step of pretreating zirconium dioxide comprises the following steps:
firstly, absolute ethyl alcohol is added into zirconium dioxide, and ultrasonic dispersion is carried out. The weight ratio of the added zirconium dioxide to the absolute ethyl alcohol is 1: 20. then adding a silane coupling agent KH-792 and polyvinyl alcohol, heating to 45 ℃, and stirring for reaction for 30 hours. Wherein the adding weight ratio of the zirconium dioxide to the silane coupling agent KH-792 to the polyvinyl alcohol is 1: 5: 1. standing and aging for 30h after the reaction is finished, and drying after solid-liquid separation to obtain the pretreated zirconium dioxide.
Secondly, the step of preparing zirconium nitride by chemical vapor deposition comprises:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 300 ℃ and 900 ℃. Argon is continuously introduced into the heating area, the high-temperature area and the cooling area, and meanwhile, ammonia is introduced into the high-temperature area. The mixed powder of zirconium dioxide and magnesium powder enters the heating zone of the reactor through automatic feeding equipment and stays for 4 minutes, and then continues to move to the high-temperature zone and stays for 25 minutes. The weight ratio of the ammonia gas to the zirconium dioxide is 10: 1. the weight ratio of zirconium dioxide to magnesium powder is 1: 2. leaving the high-temperature area after the reaction is finished, entering a cooling area for cooling. And cooling to room temperature to obtain a mixture of zirconium nitride and magnesium nitride. And removing magnesium nitride from the mixture through acid washing and alcohol washing, and then drying to obtain zirconium nitride powder.
The step of obtaining zirconium nitride powder by grinding and grading comprises the following steps:
adding zirconium nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid. Firstly, controlling a stirring shaft of a stirring mill to keep high-speed running for 10 minutes in the same direction to generate violent collision among materials, then changing the rotating direction of the stirring shaft, reversely running for 25 minutes at high speed to further grind zirconium nitride powder, and then grading to obtain the zirconium nitride powder with uniform particle size distribution. The solvent and the grinding aid added in the grinding machine are respectively ethanol and quartz sand. The weight ratio of the material balls in the grinding machine is 1: 3, the weight ratio of the zirconium nitride powder, the solvent and the grinding aid is 1: 4: 4.
the foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (1)
1. A process for preparing zirconium nitride nanoparticles includes such steps as pretreating zirconium dioxide, preparing zirconium nitride by chemical gas-phase deposition, grinding and classifying,
the pretreatment of zirconium dioxide comprises the following steps:
firstly, adding absolute ethyl alcohol into zirconium dioxide, and performing ultrasonic dispersion; the weight ratio of the added zirconium dioxide to the absolute ethyl alcohol is 1: 15-25; then adding a silane coupling agent KH-792 and polyvinyl alcohol, heating to 40-80 ℃, and stirring for reaction for 10-30 hours; wherein the adding weight ratio of the zirconium dioxide to the silane coupling agent KH-792 to the polyvinyl alcohol is 1: 2-5: 1-3; standing and aging for 10-30 h after the reaction is finished, and drying after solid-liquid separation to obtain pretreated zirconium dioxide;
preparing zirconium nitride by a chemical vapor deposition method, which comprises the following steps:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 200-500 ℃ and 800-1100 ℃; continuously introducing argon into the heating area, the high-temperature area and the cooling area, and simultaneously introducing ammonia gas into the high-temperature area; enabling the mixed powder of zirconium dioxide and magnesium powder to enter a heating area of a reactor through automatic feeding equipment, staying for 1-5 minutes, then continuing to advance to a high-temperature area, and staying for 10-30 minutes; leaving the high-temperature area after the reaction is finished, and entering a cooling area for cooling; cooling to room temperature to obtain a mixture of zirconium nitride and magnesium nitride; removing magnesium nitride from the mixture through acid washing and alcohol washing, and then drying to obtain zirconium nitride powder;
the weight ratio of the ammonia gas to the zirconium dioxide is 4-10: 1, the weight ratio of zirconium dioxide to magnesium powder is 1: 2-5;
the step of obtaining the nano zirconium nitride powder by grinding and grading comprises the following steps:
adding zirconium nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid; firstly, controlling a stirring shaft of a stirring mill to keep high-speed running for 10-20 minutes in the same direction, so that violent collision is generated between materials, then changing the rotating direction of the stirring shaft, reversely running for 15-25 minutes at high speed, further grinding zirconium nitride powder, and then grading to obtain nano zirconium nitride powder with uniform particle size distribution;
the solvent and the grinding aid added into the grinding machine are respectively ethanol and quartz sand, and the weight ratio of material balls in the grinding machine is 1: 3-5, wherein the weight ratio of the zirconium nitride powder, the solvent and the grinding aid is 1: 3-5: 2 to 6.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546370A (en) * | 2003-11-28 | 2004-11-17 | 中国科学院上海硅酸盐研究所 | Method for reduction nitridation preparation of nano cubic zirconium nitride powders |
| JP2009091205A (en) * | 2007-10-10 | 2009-04-30 | Tayca Corp | Fine particle lower zirconium oxide-zirconium nitride composite and method of manufacturing the same |
| CN104176716A (en) * | 2013-05-22 | 2014-12-03 | 安徽港铭新材料科技有限公司 | Preparation method of zirconium nitride |
| CN109923062A (en) * | 2016-09-29 | 2019-06-21 | 三菱综合材料电子化成株式会社 | Zirconium nitride powder and its manufacturing method |
| CN110891898A (en) * | 2017-06-09 | 2020-03-17 | 三菱综合材料电子化成株式会社 | Zirconium nitride powder and method for producing same |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546370A (en) * | 2003-11-28 | 2004-11-17 | 中国科学院上海硅酸盐研究所 | Method for reduction nitridation preparation of nano cubic zirconium nitride powders |
| JP2009091205A (en) * | 2007-10-10 | 2009-04-30 | Tayca Corp | Fine particle lower zirconium oxide-zirconium nitride composite and method of manufacturing the same |
| CN104176716A (en) * | 2013-05-22 | 2014-12-03 | 安徽港铭新材料科技有限公司 | Preparation method of zirconium nitride |
| CN109923062A (en) * | 2016-09-29 | 2019-06-21 | 三菱综合材料电子化成株式会社 | Zirconium nitride powder and its manufacturing method |
| CN110891898A (en) * | 2017-06-09 | 2020-03-17 | 三菱综合材料电子化成株式会社 | Zirconium nitride powder and method for producing same |
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