CN112408473A - Method for preparing nano zirconium dioxide powder by using plasma arc - Google Patents
Method for preparing nano zirconium dioxide powder by using plasma arc Download PDFInfo
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- CN112408473A CN112408473A CN202011435214.3A CN202011435214A CN112408473A CN 112408473 A CN112408473 A CN 112408473A CN 202011435214 A CN202011435214 A CN 202011435214A CN 112408473 A CN112408473 A CN 112408473A
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
A method for preparing nano zirconium dioxide powder by using plasma arc relates to the technical field of nano oxide powder preparation. Grinding zirconium hydroxide powder, and preparing the nano zirconium dioxide powder by a plasma arc flame combustion method. Firstly, starting a plasma power supply, and starting a generator at the top of a plasma arc reaction chamber to work to form plasma arc flame flow; and then conveying the ground zirconium hydroxide powder to the top end inside the plasma arc reaction chamber through a feeder, and quickly reacting the zirconium hydroxide powder through plasma arc flame flow to obtain zirconium dioxide powder. Can realize the rapid preparation of the zirconium dioxide nano powder, and rapidly synthesize the nano zirconium dioxide with high purity and large powder specific surface area by one-step ionic arc combustion. The ion arc reaction is completed instantly, the millisecond level can be reached, the prepared product has small particles, no hard agglomeration and easy ultrasonic dispersion and depolymerization, and has positive guiding significance for the preparation field of oxide nano powder.
Description
Technical Field
The invention relates to the technical field of nano oxide powder preparation, in particular to a method for preparing nano zirconium dioxide powder by using plasma arc.
Background
The zirconium dioxide powder has high melting point, high hardness, high chemical stability and excellent electrical and optical properties, and has wide application in the fields of semiconductor devices, porous ceramics and the like due to the unique physical and chemical properties.
At present, the preparation of zirconium dioxide powder mainly comprises methods such as solid-phase reaction synthesis, liquid-phase synthesis and the like, but the biggest defects of the synthesis methods are that the prepared product has large particles and serious agglomeration imagination, and even partial processes can not realize the preparation of nano-grade powder. Meanwhile, the synthesis method generally has the defects of long reaction time, high energy consumption and the like.
The plasma arc combustion method is a novel preparation method which has attracted attention in recent years, and has advantages which are incomparable with conventional preparation methods, such as short reaction time, high product purity, small particle size and the like. At present, no relevant literature reports that the plasma arc combustion method is applied to the preparation of the zirconium dioxide nano powder.
Disclosure of Invention
Aiming at the technical problems existing in the preparation of the zirconium dioxide powder, the invention provides the method for preparing the nano zirconium dioxide powder by using the plasma arc, which has the advantages of simple and convenient operation, higher purity and the like, and simultaneously overcomes the technical difficulties existing in the zirconium dioxide powder prepared by the existing preparation method.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a process for preparing nano zirconium dioxide powder by plasma arc includes such steps as grinding zirconium hydroxide powder, and plasma arc flame combustion.
As a preferred technical scheme of the invention, the step of grinding zirconium hydroxide powder comprises the following steps:
adding zirconium hydroxide powder into a ball mill for coarse crushing, and then carrying out ultrafine crushing by using a disc jet mill.
As a preferred technical scheme of the invention, the steps for preparing the nano zirconium dioxide powder by a plasma arc flame combustion method comprise:
firstly, plasma arc flame combustion method reaction
Firstly, starting a plasma power supply, and starting a generator at the top of a plasma arc reaction chamber to work to form plasma arc flame flow; then delivering the ground zirconium hydroxide powder to the top end inside the plasma arc reaction chamber through a feeder, and allowing the zirconium hydroxide powder to rapidly react through plasma arc flame flow to obtain zirconium dioxide powder and fall to the bottom of the plasma arc reaction chamber;
② multistage separation and collection of zirconium dioxide powder
Under the action of airflow, zirconium dioxide powder at the bottom of the plasma arc reaction chamber enters a multistage separator, and is stored by a collector after multistage separation;
thirdly, air current circulation
The air pump is arranged between the collector and the purifier, air flow enters the multistage separator, the collector, the air pump and the purifier from the plasma arc reaction chamber in sequence, and the gas after purification treatment is stored and pressurized by the compressor and then is introduced into the top of the plasma arc reaction chamber again to form air flow circulation; and a valve is arranged on an airflow pipeline between the purifier and the compressor and is used for inputting fresh air, high-purity oxygen and exhaust gas.
Furthermore, the flame flow temperature at the top of the plasma arc reaction chamber is 1500-2500 ℃ adjustable, and the reaction time is less than 1 s. The power of the plasma power supply is adjustable within 30-70 kW.
Compared with the prior art, the invention has the beneficial effects that:
1) the method realizes the preparation of the high-purity nano zirconium dioxide powder, has the advantages of simple and convenient process, low cost, high product purity and the like, can be used for large-scale production, and can obviously reduce the reaction temperature and the production energy consumption.
2) The rapid preparation of the zirconium dioxide nano powder can be realized through a plasma arc flame combustion reaction system with novel design, the nano zirconium dioxide with high purity and large powder specific surface area is rapidly synthesized through one-step ionic arc combustion, the productivity can reach a higher level, and the production process is free from three wastes and is environment-friendly.
3) In a plasma arc flame combustion reaction system, the ion arc reaction is instantly finished and can reach the millisecond level, and the prepared product has small particles, no hard agglomeration and easy ultrasonic dispersion depolymerization, thereby having positive guiding significance for the preparation field of oxide nano powder.
Drawings
FIG. 1 is a schematic diagram of a plasma arc flame combustion reaction system.
FIG. 2 is an XRD pattern of nano zirconium dioxide powder prepared in example 1.
FIG. 3 is SEM images of the nano zirconium dioxide powder prepared in example 1 (a and b represent high and low magnifications, respectively).
Detailed Description
The invention provides a method for preparing nano zirconium dioxide powder by using plasma arc, which comprises the steps of firstly grinding zirconium hydroxide powder, then preparing the nano zirconium dioxide powder by using a plasma arc flame combustion method, and further detailing the method by using an embodiment and an attached drawing.
Example 1
Firstly, the step of grinding zirconium hydroxide powder comprises the following steps:
adding zirconium hydroxide powder into a ball mill for coarse crushing, and then carrying out ultrafine crushing by using a disc jet mill.
Secondly, the steps of preparing the nano zirconium dioxide powder by a plasma arc flame combustion method are as follows:
firstly, plasma arc flame combustion method reaction
Referring to fig. 1, first, a plasma power source 4 is turned on, a generator 3 at the top of a plasma arc reaction chamber 2 starts to operate to form a plasma arc flame flow, and the power of the plasma power source 4 is adjusted to make the temperature of the flame flow at the top of the plasma arc reaction chamber 2 reach 2500 ℃. Then, the ground zirconium hydroxide powder is conveyed to the top end inside the plasma arc reaction chamber 2 through the feeder 1, and the zirconium hydroxide powder is subjected to rapid reaction (the reaction time is less than 1s) by plasma arc flame flow to obtain zirconium dioxide powder and falls to the bottom of the plasma arc reaction chamber 2.
② multistage separation and collection of zirconium dioxide powder
Under the action of the airflow, the zirconium dioxide powder at the bottom of the plasma reaction chamber 2 enters a multistage separator 5, and is stored by a collector 6 after multistage separation.
Thirdly, air current circulation
The air pump 7 is arranged between the collector 6 and the purifier 8, air flow enters the multistage separator 5, the collector 6, the air pump 7 and the purifier 8 from the plasma arc reaction chamber 2 in sequence, and the gas after purification treatment is stored and pressurized by the compressor 9 and then is introduced into the top of the plasma arc reaction chamber 2 again to form air flow circulation; a valve 10 is arranged on an airflow pipeline between the purifier 8 and the compressor 9 and is used for inputting fresh air, high-purity oxygen and exhaust gas.
FIG. 2 is the XRD spectrum of the nano zirconium dioxide powder prepared in example 1, and the analysis shows that the reaction product is zirconium dioxide. FIG. 3 is an overall SEM image of the nano zirconium dioxide powder prepared in example 1 (a and b represent high and low magnifications, respectively), which shows that the particle size distribution of the powder particles is relatively uniform, the average particle size is about 20nm, no large particles exist, and the product has no aggregation. Through detection, the purity of the prepared nano zirconium dioxide powder reaches over 99.9 percent.
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 (5)
1. A method for preparing nano zirconium dioxide powder by using plasma arc is characterized in that zirconium hydroxide powder is ground firstly, and then the nano zirconium dioxide powder is prepared by a plasma arc flame combustion method.
2. The method of claim 1, wherein the step of subjecting the zirconium hydroxide powder to a milling process comprises:
adding zirconium hydroxide powder into a ball mill for coarse crushing, and then carrying out ultrafine crushing by using a disc jet mill.
3. The method of claim 1 or 2, wherein the preparation of the nano zirconium dioxide powder by plasma arc flame combustion comprises the following steps:
firstly, plasma arc flame combustion method reaction
Firstly, starting a plasma power supply, and starting a generator at the top of a plasma arc reaction chamber to work to form plasma arc flame flow; then delivering the ground zirconium hydroxide powder to the top end inside the plasma arc reaction chamber through a feeder, and allowing the zirconium hydroxide powder to rapidly react through plasma arc flame flow to obtain zirconium dioxide powder and fall to the bottom of the plasma arc reaction chamber;
② multistage separation and collection of zirconium dioxide powder
Under the action of airflow, zirconium dioxide powder at the bottom of the plasma arc reaction chamber enters a multistage separator, and is stored by a collector after multistage separation;
thirdly, air current circulation
The air pump is arranged between the collector and the purifier, air flow enters the multistage separator, the collector, the air pump and the purifier from the plasma arc reaction chamber in sequence, and the gas after purification treatment is stored and pressurized by the compressor and then is introduced into the top of the plasma arc reaction chamber again to form air flow circulation; and a valve is arranged on an airflow pipeline between the purifier and the compressor and is used for inputting fresh air, high-purity oxygen and exhaust gas.
4. The method of claim 3, wherein the flame flow temperature at the top of the plasma arc reaction chamber is adjustable from 1500 ℃ to 2500 ℃ and the reaction time is less than 1 s.
5. The method of claim 3, wherein the power of the plasma power supply is adjustable between 30 and 70 kW.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011435214.3A CN112408473A (en) | 2020-12-10 | 2020-12-10 | Method for preparing nano zirconium dioxide powder by using plasma arc |
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| CN202011435214.3A CN112408473A (en) | 2020-12-10 | 2020-12-10 | Method for preparing nano zirconium dioxide powder by using plasma arc |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113913723A (en) * | 2021-12-14 | 2022-01-11 | 矿冶科技集团有限公司 | Micron-sized porous-structure thermal barrier coating powder and preparation method thereof |
Citations (4)
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|---|---|---|---|---|
| CN1740372A (en) * | 2005-09-21 | 2006-03-01 | 武汉理工大学 | Liquid phase plasma spraying process of preparing nanometer zirconia thermal-barrier coating |
| CN103864143A (en) * | 2014-01-25 | 2014-06-18 | 东莞市地大纳米材料有限公司 | Method for preparing nanometer zirconium oxide granulated powder |
| CN108213451A (en) * | 2016-12-14 | 2018-06-29 | 彭徽 | A kind of method and apparatus of metal powder nodularization |
| CN111872406A (en) * | 2020-07-21 | 2020-11-03 | 河南能微新材料科技股份有限公司 | Inductively coupled plasma powder production equipment and production process |
-
2020
- 2020-12-10 CN CN202011435214.3A patent/CN112408473A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740372A (en) * | 2005-09-21 | 2006-03-01 | 武汉理工大学 | Liquid phase plasma spraying process of preparing nanometer zirconia thermal-barrier coating |
| CN103864143A (en) * | 2014-01-25 | 2014-06-18 | 东莞市地大纳米材料有限公司 | Method for preparing nanometer zirconium oxide granulated powder |
| CN108213451A (en) * | 2016-12-14 | 2018-06-29 | 彭徽 | A kind of method and apparatus of metal powder nodularization |
| CN111872406A (en) * | 2020-07-21 | 2020-11-03 | 河南能微新材料科技股份有限公司 | Inductively coupled plasma powder production equipment and production process |
Non-Patent Citations (1)
| Title |
|---|
| C. ELISSALDE ET AL.,: "Single-step sintering of zirconia ceramics using hydroxide precursors and Spark Plasma Sintering below 400 °C", 《SCRIPTA MATERIALIA》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113913723A (en) * | 2021-12-14 | 2022-01-11 | 矿冶科技集团有限公司 | Micron-sized porous-structure thermal barrier coating powder and preparation method thereof |
| CN113913723B (en) * | 2021-12-14 | 2022-02-22 | 矿冶科技集团有限公司 | Micron-sized porous-structure thermal barrier coating powder and preparation method thereof |
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