CN1445164A - Technique for preparing ceramic powder of titanium carbide by using plasma chemical gas phase synthesis method - Google Patents
Technique for preparing ceramic powder of titanium carbide by using plasma chemical gas phase synthesis method Download PDFInfo
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- CN1445164A CN1445164A CN 02153391 CN02153391A CN1445164A CN 1445164 A CN1445164 A CN 1445164A CN 02153391 CN02153391 CN 02153391 CN 02153391 A CN02153391 A CN 02153391A CN 1445164 A CN1445164 A CN 1445164A
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Abstract
A process for preparing SiC ceramic powder by plasma chemical gas-phase synthesis method includes such steps as quickly heating the gas to high temp by plasma of DC arc, thermally evaporating CH3SiCl3, reaction to generate SiC, crystallizing, growing, fast cooling, and gas-solid separation by cloth-bag collector. Its advantages are high purity, fine granularity (0.08-0.5 microns), low cost and no environmental pollution.
Description
Technical Field
The invention relates to a process for industrially preparing nano silicon carbide ceramic powder by using a plasma chemical vapor phase method.
Technical Field
The silicon carbide has a series of advantages of high temperature resistance, corrosion resistance, thermal shock resistance, low density, high hardness and the like, and is an important novel ceramic material. Can be used for manufacturing high-performance ceramic engine parts, high-temperature nozzles, high-temperature fluid conveying devices, high-temperature sealing element valves, high-temperature ceramic bearings, ceramic cutting tools, high-hardness abrasives, grinding tools and the like; it can also be used for reinforcing alumina material and toughening zirconia material.
Most of the currently common silicon carbide powder preparation methods generally adopt a silicon dioxide or silicon powder carbothermic reduction method, and the silicon carbide powder prepared by the method can only be finally obtained into micron-sized silicon carbide powder through a plurality of processes such as crushing, grinding, acid washing, drying, sieving and the like. The process for producing the silicon carbide powder has high production cost and lower silicon carbide purity.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a compound CH with low production cost and high finished product purity3SiCl3The process for industrially producing the high-purity superfine silicon carbide powder by utilizing a plasma chemical vapor phase method.
The technical scheme of the invention is as follows: firstly, introducing plasma working gas N into a plasma generator2-H2-Ar, in N29-13m3/h；H227-32m3H; the flow rate of (2) and injecting 30 liters/minute of Ar, starting a plasma power supply, generating a plasma arc in a plasma generator, and closing Ar gas after the arc is normally started. The gas passing through the electric arc is heated to the high temperature of 4800-5200 ℃ and then enters a reactor, and then the CH heated and evaporated by the evaporator is evaporated3SiCl3Is fed into a reactor where decomposition, CH, takesplace rapidly3SiCl3The feeding rate is 16-25kg/h, the continuous injection is carried out, and the reaction temperature in the plasma reactor is kept at 1500-1800 ℃. Rapidly decomposing in a plasma reactor and generating solid SiC micropowder by utilizing free settling and quenching conditions.
And crystallizing and growing the generated SiC, cooling, and then carrying out gas-solid separation by a cloth bag powder collector to obtain SiC powder. And carrying out vacuum heat treatment on the obtained powder for 6-8 hours to obtain the silicon carbide powder.
The invention has the following positive effects: the process of the invention utilizes direct current arc plasma as a heat source, gas flowing through the arc is rapidly heated to high temperature and enters a reactor, and meanwhile, the gas is heated and steamed by an evaporatorSending CH3SiCl3Enters a reactor to carry out rapid decomposition and synthesis reaction of silicon carbide. The generated SiC is crystallized and grown up in a very short time (millisecond level), then is rapidly cooled down after being conveyed to a cold environment by airflow, and then is subjected to gas-solid separation by a cloth bag powder collector to obtain the nano-scale silicon carbide powder. The silicon carbide produced by the process has high purity, uniform particle size distribution, superfine particle size which can be adjusted between 0.08 and 0.5 mu m, low cost, high yield, suitability for large-scale production, no three-waste discharge and accordance with the requirement of environmental protection.
Drawings
The attached drawing is a structural schematic diagram of the production device of the invention.
Detailed Description
As shown in the figure, the whole production device in the process mainly comprises a power supply and a microcomputer data acquisition system; a gas-liquid feedstock supply system; a water-cooling circulation system; a powder synthesis and collection system; a post-processing system; exhaust gas treatment systems, and the like.
(1) A power supply and a microcomputer data acquisition system; and the power supply is provided for the plasma generator, data acquisition is carried out, and the power of the plasma generator and the temperature of the reactor are controlled.
(2) Gas-liquid raw material supply system: the working gas entering the plasma generator and the raw material gas entering the reactor are quantitatively controlled, so that the chemical composition and yield of reactants are controlled.
(3) A water cooling circulation system; cooling water is provided for the plasma generator and the material conveying pipeline, and the safe operation of the equipment is ensured.
(4) Powder synthesis and powder collection system: the system comprises a plasma reactor, a settler, a conveying pipeline and a powder collector, ensures that raw material gas can fully react in the reactor, and effectively collects reaction products.
(5) A post-processing system: and carrying out heat treatment on the collected powder material, effectively removing chloride ions in the powder, and metering and packaging.
(6) An exhaust gas treatment system: the system comprises a leaching tower and a treatment tank. The method is mainly used for treating gas generated in the reaction and protecting the environment.
The process firstly introduces plasma working gas N into a plasma generator2-H2Ar, then starting a plasma power supply, generating a plasma arc in a plasma generator, the gas passing through the arc being heated to a high temperature of about 5000 ℃ and entering the reactor while being evaporatedHeating evaporated CH by device3SiCl3The gas is also sent into a reactor, the gas is rapidly decomposed into SiC synthesis reaction under the action of plasma, the generated SiC is crystallized and grown in a very short time (millisecond level), fine particles with different particle sizes are formed by utilizing a controllable cooling speed, the particles are rapidly cooled down after being sent into a cold environment by air flow, and then gas-solid separation is realized by a cloth bag powder collector to obtain SiC ultrafine powder.
The waste gas passing through the cloth bag is leached by water in the leaching tower to remove HCl and then is exhausted. And collecting the HCl-containing wastewater for sale.
The SiC powder obtained from the powder collector contains chlorine (Cl)-) The amount is high, the silicon carbide powder is processed in a vacuum heat treatment furnace for 3 to 8 hours, and then the silicon carbide powder is measured and packaged to obtain a finished product of silicon carbide powder.
The invention will now be discussed in detail with reference to the following examples:
example 1: firstly, introducing plasma working gas N into a plasma generator2-H2-Ar, in N29-m3/h；H227-m3H; the flow rate of (2) and injecting 30 liters/minute of Ar, starting a plasma power supply, generating a plasma arc in a plasma generator, and closing Ar gas after the arc is normally started. Heating the gas passingthrough the electric arc to 5000 ℃ and then entering a reactor, and heating the evaporated CH by an evaporator3SiCl3Decomposition, CH, takes place rapidly in the reactor3SiCl3The adding speed is 16kg/h, the continuous injection is carried out, and the reaction temperature in the plasma reactor is keptAt 1650 ℃. Rapidly decomposing in a plasma reactor and generating solid SiC micropowder by utilizing free settling and quenching conditions. The generated SiC is crystallized and grown up in a very short time (millisecond grade), cooled and then is subjected to gas-solid separation by a cloth bag powder collector to obtain SiC powder. The obtained powder is subjected to vacuum heat treatment for 6 hours to obtain the silicon carbide powder with superfine particle size and uniform particle size distribution. The yield is more than 4.5 kg/h. The detection result of the performance index of the powder is as follows:
(1) purity:
| detecting items | SiC(％) | Sif(％) | Cf(％) | Cl-(％) | ∑0(％) |
| The result of the detection | 97.2 | 0.18 | 0.85 | 0.18 | 1.45 |
(2) Crystal form β -SiC
(3) Average particle size: d50 ═ 0.085 μm
(4) Specific surface area: 38.5m2Example 2,/g: firstly, introducing plasma working gas N into a plasma generator2-H2-Ar, in N213m3/h；H2-32m3H; is continuously injected, and 30 liters/min of Ar is injected, startedAnd a plasma power supply for generating a plasma arc in the plasma generator (and turning off the Ar gas after normal arcing). The gas after the electric arc is heated to 5200 deg.C and enters into a reactor, and the evaporated CH is heated by an evaporator3SiCl3Decomposition, CH, takes place rapidly in the reactor3SiCl3The addition rate was 25kg/h, the injection was continued and the reaction temperature in the plasma reactor was maintained at 1500 ℃. Rapidly decomposing in a plasma reactor and generating solid SiC micropowder by utilizing free settling and quenching conditions. The generated SiC is crystallized and grown up in a very short time (millisecond grade), cooled and then is subjected to gas-solid separation by a cloth bag powder collector to obtain SiC powder. The obtained powder is subjected to vacuum heat treatment for 7 hours to obtain the silicon carbide powder with superfine particle size and uniform particle size distribution. The yield is more than 4.5 kg/h. The detection result of the performance index of the powder is as follows:
(1) purity:
| detecting items | SiC(％) | Sif(％) | Cf(％) | Cl-(％) | ∑0(％) |
| The result of the detection | 97.5 | 0.15 | 0.7 | 0.21 | 1.3 |
(2) Crystal form β -SiC
(3) Average particle size: d50 ═ 0.24 μm
(4) Specific surface area: 27.8m2/g
Example 3: firstly, introducing plasma working gas N into a plasma generator2-H2-Ar, in N211m3/h；H230m3H; the flow rate of (2) and injecting 30 liters/minute of Ar, starting a plasma power supply, generating a plasma arc in a plasma generator, and closing Ar gas after the arc is normally started. Warp beamThe gas passing through the electric arc is heated to 4800 ℃ and enters a reactor, and then the CH evaporated by the heating of an evaporator is added3SiCl3Decomposition, CH, takes place rapidly in the reactor3SiCl3The addition rate was 20kg/h, the injection was continued and the reaction temperature in the plasma reactor was maintained at 1800 ℃. Rapidly decomposing in a plasma reactor and generating solid SiC micropowder by utilizing free settling and quenching conditions. The generated SiC is crystallized and grown up in a very short time (millisecond grade), cooled and then is subjected to gas-solid separation by a cloth bag powder collector to obtain SiC powder. The obtained powder is subjected to vacuum heat treatment for 8 hours to obtain the silicon carbide powder with superfine particle size and uniform particle size distribution. The yield is more than 4.5 kg/h. The detection result of the performance index of the powder is as follows:
(1) purity:
| detecting items | SiC(％) | Sif(％) | Cf(％) | Cl-(％) | ∑0(％) |
| The result of the detection | 97.7 | 0.12 | 0.58 | 0.24 | 1.2 |
(2) Crystal form β -SiC
(3) Average particle size: d50 ═ 0.38 mu m
(4) Specific surface area: 24.2m2/g。
Claims (1)
1. A process for preparing silicon carbide ceramic powder by plasma chemical vapor synthesis method is characterized in that firstly, a plasma working gas N is introduced into a plasma generator2-H2-Ar, in N29-13m3/h；H227-32m3H; the flow rate of (2) and injecting 30 liters/minute of Ar, starting a plasma power supply, generating a plasma arc in a plasma generator, and closing Ar gas after the arc is normally started. The gas passing through the electric arc is heated to the high temperature of 4800-5200 ℃ and then enters a reactor, and then the CH heated and evaporated by the evaporator is evaporated3SiCl3Decomposition, CH, takes place rapidly in the reactor3SiCl3The feeding rate is 16-25kg/h, the continuous injection is carried out, and the reaction temperature in the plasma reactor is kept at 1500-1800 ℃. Rapidly decomposing in a plasma reactor and generating solid SiC micropowder by utilizing free settling and quenching conditions. And crystallizing and growing the generated SiC, cooling, and then carrying out gas-solid separation by a cloth bag powder collector to obtain SiC powder. And carrying out vacuum heat treatment on the obtained powder for 6-8 hours to obtain the silicon carbide powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB021533911A CN1184142C (en) | 2002-11-29 | 2002-11-29 | Technique for preparing ceramic powder of titanium carbide by using plasma chemical gas phase synthesis method |
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| CNB021533911A CN1184142C (en) | 2002-11-29 | 2002-11-29 | Technique for preparing ceramic powder of titanium carbide by using plasma chemical gas phase synthesis method |
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| CN1184142C CN1184142C (en) | 2005-01-12 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101950721A (en) * | 2009-07-10 | 2011-01-19 | 东京毅力科创株式会社 | Surface treatment method |
| CN102583382A (en) * | 2012-01-13 | 2012-07-18 | 梁洪奎 | Method for synthesizing silicon-carbide nano-powder by quasi-gaseous phase method |
| CN105120999B (en) * | 2013-04-24 | 2017-11-28 | 赢创德固赛有限公司 | Method and apparatus for preparing multi-silane |
| CN111261861A (en) * | 2020-01-22 | 2020-06-09 | 金雪莉 | Method for continuously preparing high-purity carbon-silicon nano material |
-
2002
- 2002-11-29 CN CNB021533911A patent/CN1184142C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101950721A (en) * | 2009-07-10 | 2011-01-19 | 东京毅力科创株式会社 | Surface treatment method |
| US8318034B2 (en) | 2009-07-10 | 2012-11-27 | Tokyo Electron Limited | Surface processing method |
| CN101950721B (en) * | 2009-07-10 | 2012-12-05 | 东京毅力科创株式会社 | Surface treatment method |
| US8715782B2 (en) | 2009-07-10 | 2014-05-06 | Tokyo Electron Limited | Surface processing method |
| CN102583382A (en) * | 2012-01-13 | 2012-07-18 | 梁洪奎 | Method for synthesizing silicon-carbide nano-powder by quasi-gaseous phase method |
| CN102583382B (en) * | 2012-01-13 | 2013-06-05 | 梁洪奎 | Method for synthesizing silicon-carbide nano-powder by quasi-gaseous phase method |
| CN105120999B (en) * | 2013-04-24 | 2017-11-28 | 赢创德固赛有限公司 | Method and apparatus for preparing multi-silane |
| CN111261861A (en) * | 2020-01-22 | 2020-06-09 | 金雪莉 | Method for continuously preparing high-purity carbon-silicon nano material |
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| CN1184142C (en) | 2005-01-12 |
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