CN102502635A - Method for preparing surface-modified infusible metallic carbide ultrafine powder - Google Patents
Method for preparing surface-modified infusible metallic carbide ultrafine powder Download PDFInfo
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- CN102502635A CN102502635A CN2011103437647A CN201110343764A CN102502635A CN 102502635 A CN102502635 A CN 102502635A CN 2011103437647 A CN2011103437647 A CN 2011103437647A CN 201110343764 A CN201110343764 A CN 201110343764A CN 102502635 A CN102502635 A CN 102502635A
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Abstract
The invention provides a method for preparing surface-modified infusible metallic carbide ultrafine powder. The infusible metallic carbide ultrafine powder is synthesized by using high-temperature thermal plasma, surface modification is performed on the powder in a synthesizing process simultaneously, and the product, i.e., infusible metallic carbide ultrafine powder is directly dispersed into a solvent to obtain uniform and stable slurry. The characteristics of ultra-fineness and high activity of plasma synthesized powder are brought into full play, and an activating process before modification is avoided by performing an instant modification process. The product, i.e., infusible metallic carbide ultrafine powder is mainly applied in the fields of high-temperature ceramics and composite materials.
Description
Technical field
The present invention relates to a kind of method for preparing the refractory carbide and the slurry of surface-treated.In more detail, this invention proposes the synthetic refractory carbide superfine powder of a kind of employing high-frequency thermal plasma, and in building-up process, realizes surface-treated, it can directly be scattered in obtain method even, stable slurry in the solvent.
Technical background
Refractory carbide materials chemistry good stability; Have good high temperature resistant, corrosion-resistant, wear resisting property; Be good high-temperature structured material, superhard tool material and surface protecting material; It also has good thermal conductivity simultaneously, has the potential using value in directions such as cutter material, armour material, build-up wear-resistant welding rods, is the research focus of non-oxide ceramic material in recent years.In addition, carbide makes an addition to the resistance to elevated temperatures and the intensity that can effectively improve material in the matrix material.The sintering character of superfine powder is superior to general powder, and the employing superfine powder is a raw material, in the sintering temperature that reduces pyroceramic, can improve the toughness and the intensity of stupalith.Superfine powder also helps to improve and adds dispersiveness and the homogeneity of carbide in matrix material, and effect is very obvious.
Gel casting forming technology (gel-casting) is the Omatete of U.S.'s Oak Ridge National Laboratory and a kind of new ceramics forming technique that the Jenny professor at first invented in early 1990s.It with the flexible method of organic polymer monomer polymerization be incorporated in the forming process of ceramics; Suspended nitride through preparation LV, high solids content; Under catalyzer and initiator effect,, form firm polymer with intersection chain structure through the organic monomer in-situ polymerization; The ceramic component that plastic different shape is complicated, thereby but the base substrate of acquisition intensity height, good uniformity and mechanical workout.Generally, the stability of suspended nitride reduces with the viscosity of slurry and variation, how under the LV condition, to obtain the suspended nitride of high solids content, is the successful key of gel casting forming.Wherein reduce particle size and modification is a valid approach to solid particles surface.
Summary of the invention
The present invention provides a kind of refractory carbide superfine powder of surface-treated and method of slurry of preparing, and adopts the synthetic refractory carbide superfine powder of high-frequency thermal plasma, and it directly is scattered in obtains even, stable slurry in the solvent.High-frequency thermal plasma synthetic superfine powder has guaranteed the homodisperse requirement of slurry, has satisfied stability requirement to powder-modified.The synthetic superfine powder that obtains of plasma body has higher activity, has the investigator to utilize the plasma arcs pyroprocessing to be used for powder-modified preceding activation specially.The instant modification in the powder production process that the present invention proposes has not only been shortened technical process, and has directly been saved the high-temperature process before the traditional technology surface-treated, and can obtain better effect.The selection of powder surface modifier and activation temperature is carried out according to the type of slurry solvent.
The present invention provides a kind of refractory carbide superfine powder of surface-treated and method of slurry thereof of preparing, and comprises that the refractory carbide superfine powder of surface-treated is synthetic and powder is scattered in preparing slurry in the solvent.Wherein the refractory carbide superfine powder of high-frequency thermal plasma synthetic surface modification is the core of invention, comprises following step:
(1) raw material of synthetic refractory carbide is imported plasma arcs continuously;
(2) raw material that gets into plasma arcs reacts in the high-temperature zone;
(3) reactant leaves formation of deposits superfine powder behind the high-temperature zone;
(4) product gets into the powder gathering system under gas drives, and in this process, adds tensio-active agent;
(5) tensio-active agent and powder granule effect are carried out hydrophilic or hydrophobically modified to powder;
(6) in the powder gathering system, collect product.
In the step (1), the raw material of synthetic refractory carbide refers to contain the compound or the simple substance of refractory metal and carbon, and the form that gets into plasma arcs can be solid-state, liquid or gaseous state.
In the step (2), the high-temperature zone comprises plasma arcs interior region and the outside high-temperature area that is used to accomplish building-up reactions of plasma arcs.
In the step (3), the powder deposition comprises all processes such as generation, reunion and growth of powder nucleus.
In the step (4), tensio-active agent adds opportunity after powder forms, and adds the implantation site and is leading in the approach of scoop or in the scoop at powder collector or powder, and the adding mode is that gas evaporation adds.
In the step (5), fully act on, can add fashionable temperature for the control surface promoting agent, also can heat and be incubated this section reactor drum for guaranteeing tensio-active agent and powder granule.
The high-frequency thermal plasma method is with the obvious advantage aspect preparing at the high temperature superfine powder, and it is short that this improves technical process, and can realize producing in batches, is suitable for the production of refractory carbide superfine powder and slurry.
Description of drawings:
Fig. 1 is the structural representation of high frequency plasma equipment
Fig. 2 is the XRD spectra of product powder
Fig. 3 is the stereoscan photograph of product powder
Label among the figure: 1 airing system; 2 power supply systems; 3 feeder systems; 4 high-temperature areas; 5 powders form the zone; 6 powder collecting zones; 7 exhaust emissions treatment zones.
Embodiment
Adopting zirconium chloride and methane is raw material synthesizing superfine zirconium carbide powder.With hydrogen and methane gas is carrier gas, through screw feeder the zirconium chloride solid material is added in the high-frequency thermal plasma arc and reacts.The ratio that wherein adds zirconium chloride and methane amount of substance is 1/1, and the ratio of hydrogen and zirconium chloride amount of substance is 4/1.In the process of synthetic powder, add modified material; Modified material adopts silane coupling agent KH560; Add-on maintains and generates 5% of zirconium carbide quality, and silane coupling agent KH560 adopts the mode of gas evaporation to add the plasma body synthesis system, 300 ℃ of vaporization temperatures; Add the implantation site and enter the mouth at bagroom, temperature keeps 300 ℃ in the dust-precipitator.Below the product particle size 100nm, be scattered in even, the stable slurry of formation in the Dodecyl Mercaptan.
Zirconium carbide powder to the high frequency plasma prepared carries out thing phase, sreen analysis, and the result shows that product purity is higher, even particle size distribution, and particle size can be regulated and control in the 10-500nm scope.The structural representation of high frequency plasma equipment is seen accompanying drawing 1, adopts the XRD spectra of the zirconium carbide powder of high frequency plasma prepared to see accompanying drawing 2, adopts the stereoscan photograph of the zirconium carbide powder of high frequency plasma prepared to see accompanying drawing 3.
Adopting zirconium chloride and methane is raw material synthesizing superfine zirconium carbide powder.The zirconium chloride raw material evaporates outside plasma body, adds in the high-frequency thermal plasma arc with gas phase state then.Other experiment conditions are identical with embodiment 1.Below the product particle size 100nm, be scattered in even, the stable slurry of formation in the Dodecyl Mercaptan.
Adopting hafnium chloride and methane is raw material synthesizing superfine hafnium carbide powder.With hydrogen and methane gas is carrier gas, through screw feeder the hafnium chloride solid material is added in the high-frequency thermal plasma arc and reacts.The ratio that wherein adds hafnium chloride and methane amount of substance is 1/1, and the ratio of hydrogen and hafnium chloride amount of substance is 4/1.In the process of synthetic powder, add modified material; Modified material adopts silane coupling agent KH560; Add-on maintains and generates 5% of hafnium carbide quality, and silane coupling agent KH560 adopts the mode of gas evaporation to add the plasma body synthesis system, 300 ℃ of vaporization temperatures; Add the implantation site and enter the mouth at bagroom, temperature keeps 300 ℃ in the dust-precipitator.Below the product particle size 100nm, be scattered in even, the stable slurry of formation in the Dodecyl Mercaptan.
Adopting tantalum chloride and methane is raw material synthesizing superfine tantalum carbide powder.With hydrogen and methane gas is carrier gas, through screw feeder the tantalum chloride solid material is added in the high-frequency thermal plasma arc and reacts.The ratio that wherein adds tantalum chloride and methane amount of substance is 1/1, and the ratio of hydrogen and tantalum chloride amount of substance is 4/1.Add modified material in the powder collector ingress; Modified material adopts silane coupling agent KH560; Add-on maintains and generates 5% of tantalum carbide quality, and silane coupling agent KH560 adopts the mode of gas evaporation to add the plasma body synthesis system, 300 ℃ of vaporization temperatures; Add the implantation site and enter the mouth at bagroom, temperature keeps 300 ℃ in the dust-precipitator.Below the product particle size 100nm, be scattered in even, the stable slurry of formation in the Dodecyl Mercaptan.
Adopting zirconium white and acetylene is raw material synthesizing superfine zirconium carbide powder.With hydrogen and acetylene gas is carrier gas, through screw feeder the zirconia solid raw material is added in the high-frequency thermal plasma arc and reacts.The ratio that wherein adds zirconium white and acetylene amount of substance is 2/1, and the ratio of hydrogen and zirconium white amount of substance is 4/1.Add modified material in the powder collector ingress; Modified material adopts silane coupling agent KH560; Add-on maintains and generates 5% of zirconium carbide quality, and silane coupling agent KH560 adopts the mode of gas evaporation to add the plasma body synthesis system, 300 ℃ of vaporization temperatures; Add the implantation site and enter the mouth at bagroom, temperature keeps 300 ℃ in the dust-precipitator.Below the product particle size 100nm, be scattered in even, the stable slurry of formation in the Dodecyl Mercaptan.
Adopting metal tantalum and acetylene is raw material synthesizing superfine tantalum carbide powder.With the acetylene gas is carrier gas, through screw feeder the ta powder solid material is added in the high-frequency thermal plasma arc and reacts.The ratio that wherein adds tantalum and acetylene amount of substance is 2/1.Add modified material in the powder collector ingress; Modified material adopts silane coupling agent KH560; Add-on maintains and generates 5% of tantalum carbide quality, and silane coupling agent KH560 adopts the mode of gas evaporation to add the plasma body synthesis system, 300 ℃ of vaporization temperatures; Add the implantation site and enter the mouth at bagroom, temperature keeps 300 ℃ in the dust-precipitator.Below the product particle size 100nm, be scattered in even, the stable slurry of formation in the Dodecyl Mercaptan.
Adopting hydrogenation hafnium and carbon dust is raw material synthesizing superfine hafnium carbide powder.After hydrogenation hafnium and carbon dust mixing, through reacting in the screw feeder adding high-frequency thermal plasma arc.Wherein the ratio of the amount of hydrogenation hafnium and toner substance is 1/1.In powder collector, add modified material; Modified material adopts silane coupling agent KH550; Add-on maintains and generates 5% of hafnium carbide quality, and silane coupling agent KH550 adopts the mode of gas evaporation to add the plasma body synthesis system, 200 ℃ of vaporization temperatures; Add the implantation site and enter the mouth at bagroom, temperature keeps 200 ℃ in the dust-precipitator.Below the product particle size 100nm, be scattered in even, the stable slurry of formation in the Dodecyl Mercaptan.
Above said embodiment be to explanation of the present invention, be not to qualification of the present invention.Design, method and scope that the present invention requires to protect all are documented in claims of the present invention.
Claims (9)
1. a method for preparing the refractory carbide superfine powder of surface-treated comprises the steps: that the raw material of (1) synthetic refractory carbide is imported plasma arcs continuously; (2) raw material that gets into plasma arcs reacts in the high-temperature zone; (3) reactant leaves formation of deposits superfine powder behind the high-temperature zone; (4) product gets into the powder gathering system under gas drives, and in this process, adds tensio-active agent; (5) tensio-active agent and powder granule effect are carried out modification to powder; (6) in the powder gathering system, collect product.It is characterized in that: in the synthetic refractory carbide superfine powder process of high-frequency thermal plasma, introduce modified material, realization powder preparing and surface-treated are accomplished continuously.
2. method according to claim 1 is characterized in that: modified material powder in the plasma reaction system produces any position of back and powder collection and introduces.
3. method according to claim 1 and 2 is characterized in that: powder-modified process and powder synthetic process are carried out simultaneously, realize through in the high-frequency thermal plasma synthesis system, introducing the gaseous state modified material.
4. method according to claim 1 and 2 is characterized in that: modified material is silane coupling agent etc. has modifying function to refractory carbide a tensio-active agent.
5. method according to claim 1 and 2 is characterized in that: the position temperature that adds modified material is controlled at room temperature to 300 ℃ scope.
6. method according to claim 5 is characterized in that: the position temperature control that adds the gaseous state modified material realizes through waste heat or the outer mode that heats of utilizing plasma arcs.
7. method according to claim 1 is characterized in that: refractory carbide comprises zirconium carbide, hafnium carbide, tantalum carbide high temperature material.
8. according to claim 1 or 2 said methods, it is characterized in that: the raw material of synthetic refractory carbide, by carbon dust, methane or acetylene carbon source is provided, by refractory metal simple substance, muriate, oxide compound or hydrogenate source metal is provided.
9. method for preparing insoluble metal carbide slurry is characterized in that: prepare the insoluble metal carbide of surface-treated according to claim 1, the refractory carbide superfine powder is scattered in solvent, form the refractory carbide slurry.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019205546A1 (en) * | 2018-04-25 | 2019-10-31 | 华南理工大学 | Functionalized two-dimensional layered transition metal carbide material f-mxene and preparation method therefor and use thereof in rubber |
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| CN1520383A (en) * | 2001-04-24 | 2004-08-11 | ̩���ɵ�����ϵͳ��˾ | Plasma synthesis of titanium dioxide nanopowder and powder doping and surface modification process |
| CN101318653A (en) * | 2007-06-06 | 2008-12-10 | 中国科学院金属研究所 | Method for preparing TaC nano-powder material |
| CN101417789A (en) * | 2008-11-05 | 2009-04-29 | 东华大学 | Plasma modification processing method of metallic oxide nano powder at atmosphere pressure and normal temperature |
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Patent Citations (4)
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| US5578108A (en) * | 1993-09-29 | 1996-11-26 | Ykk Corporation | Ultrafine particles of amorphous metal and method for production thereof |
| CN1520383A (en) * | 2001-04-24 | 2004-08-11 | ̩���ɵ�����ϵͳ��˾ | Plasma synthesis of titanium dioxide nanopowder and powder doping and surface modification process |
| CN101318653A (en) * | 2007-06-06 | 2008-12-10 | 中国科学院金属研究所 | Method for preparing TaC nano-powder material |
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| 唐振方,刘彭义,叶勤,孙汪典,凌育远,钟红海: "热等离子体反应合成WC超细粉体", 《机械工程材料》, vol. 27, no. 5, 31 May 2003 (2003-05-31), pages 28 - 31 * |
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| WO2019205546A1 (en) * | 2018-04-25 | 2019-10-31 | 华南理工大学 | Functionalized two-dimensional layered transition metal carbide material f-mxene and preparation method therefor and use thereof in rubber |
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