CN101318653B - Method for preparing TaC nano-powder material - Google Patents
Method for preparing TaC nano-powder material Download PDFInfo
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- CN101318653B CN101318653B CN200710011565XA CN200710011565A CN101318653B CN 101318653 B CN101318653 B CN 101318653B CN 200710011565X A CN200710011565X A CN 200710011565XA CN 200710011565 A CN200710011565 A CN 200710011565A CN 101318653 B CN101318653 B CN 101318653B
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Abstract
The invention provides a method for preparing TaC nanometer powder material, and the shell of the nanometer powder is carbon. The method is characterized in that argon gas and ethanol are used as the working gases and the preparation technology that arc discharge produces plasma is adopted; the component for anode consumption is Ta, the component for cathode consumption is graphite; the preparation of the TaC nanometer powder is carried out under the atmosphere of the mixture of the argon gas and C2H5OH, the pressure of the argon gas is 0.5kPa-0.5MPa, the dosage of C2H5OH is proportional to the volume of the working cavity and is 0.05-5ml/litre; the distance between the anode consumption and cathode is 0.1mm-5cm, the current of the arc discharge is 8-600A and the voltage of the arc discharge is 5-50V. Due to making use of ethanol to carry out the decomposition, carbon source in a gaseous state is provided, which improves the yield of the TaC nanometer powder and reduces the free carbon.
Description
Technical field
The present invention relates to a kind of technology for preparing the nano-powder material of metal, provide a kind of especially at argon gas and C
2H
5The method for preparing the TaC nano-powder material in the OH mixed atmosphere.
Background technology
The TaC nano-powder material has important use in coatings industry.TaC hardness is big, fusing point is that 3985 ℃, high-temperature behavior are good.The TaC nano-powder material as jet engine turbine blade and rocket nozzle coating, can improve its work-ing life significantly.In the electron emission pipe is produced, make the middle layer compound coating with the TaC nanometer powder.With a series of metal synthetic superalloys such as TaC and tungsten, aluminium, nickel, cobalt, vanadium, be the satisfactory texture material of superjet, rocket and guided missile etc.In mechanical industry, the cutter with Wimet such as TaC nano powder are made can stand nearly 3000 ℃ high temperature, and its hardness can be with the hardest in the world material---diamond compares favourably.TaC still is the type material, can prepare the nonideal second class hard superconductor.
Patent CN2003101103365, the preparation method of nanophase TaC-transition metal base composite powder discloses the method for preparing the TaC nano-powder material with chemical process.Use C
2H
5The method that OH prepares the TaC nano-powder material is not reported.
Summary of the invention
The purpose of this invention is to provide the nano-powder material technology for preparing metal.
Particularly, the invention provides a kind of preparation method of TaC compound nano powdered material, it is characterized in that: the preparation method of described TaC compound nano powdered material, adopt arc-over to produce the technology of preparing of plasma body.
The shell of described TaC nano-powder material is a carbon, and preferably, the carbon thickness of the shell is 2-5nm, sloughs unnecessary carbon with pure nitric acid heating.
Preparation TaC nanometer powder is at argon gas and C
2H
5Carry out in the OH mixed atmosphere; Ar pressure is 0.5kPa-0.5MPa; C
2H
5OH institute consumption is directly proportional with the working chamber volume, is the 0.05-5ml/ liter.
Among the preparation method of metallic carbide nano-powder material of the present invention, the composition of used consumable anode is Ta, and preferably, anode places on the water-cooled anode;
The composition of used consumption negative electrode is a graphite, and anode and cathode distance are 0.1mm-5cm; The electric current of arc-over is 8-600A, and voltage is 5-50V.
Among the preparation method of TaC nano-powder material of the present invention, after having prepared, can be with the argon gas passivation that contains the 0-70% air, passivation time is 0-100 hour, carries out the collection of nanometer powder again.
Among the preparation method of metallic carbide nano-powder material of the present invention, between described water-cooled anode and the consumable anode copper crucible is arranged, the thickness of copper crucible bottom is 3-30mm.
Adopt arc-over to produce the technology of preparing of plasma body among the present invention, concrete principle is:
The arc plasma Ta that has been ionization mainly in the preparation, C, Ar, the gas of H, it is made up of electronics, ion and neutral particle.Wherein electronics and ionic sum are equal substantially, thereby are electroneutral as a whole, if in a single day charge separation appears in plasma body, will produce huge electric field immediately.
In arc discharge process, the energy w=electric weight * voltage that electronics obtains in electric field, the quantity of electric charge of electronics is e=1.6 * 10
-19Coulomb, when voltage V=2 volt, thereby can obtain 2eV=2 * 1.6 * 10
-19Coulomb * volt=3.2 * 10
-19Joule.According to the microcosmic definition of temperature, E=W=3/2kT=2eV=3.2 * 10
-19Joule, just can obtain electronic temp T to the Boltzmann constant substitution:
T＝23200K
This only is to consider independent electronic behavior.The very big temperature of electron energy is very high, but quantity seldom.When plasma state becomes normal state, temperature decrease, this for fusing point up to 3985 ℃ and also the formation of the TaC of stable in properties condition is provided.
Debye (Debye) length lambda
0Describe the caused charge separation yardstick of particle random motion, it is directly proportional with the square root of electronic temp T, and with electronic number density n
eSquare root be inversely proportional to.
λ
0＝(ε
0kT/e
2n
e)
1/2
ε
0Be specific inductivity, k is a Boltzmann constant.The quantitative partial charge separation that plasma body causes for a certain reason, the degree that electric neutrality is damaged described of Debye length.Also can be λ
0Whether regard ionized gas as is a yardstick of plasma body.
Temperature is 10
4K, Debye length is about 700 nanometers in the plasma body that arc-over produces, and density is 10
14Cm
-3, when temperature is 5 * 10
3K is about 500 nanometers. and the electric neutrality Debye length that is damaged is that temperature decrease is below fusing point in hundreds of nanometers approximately.The metallic compound steam is easy to forming core and grows up, and because of density is low, forms the particle of the TaC of nanometer.The particle of TaC further forms congeries.
Because the particle diameter of nano metal particles is little, specific surface is big, very easily oxidation in air, thereby be difficult to use.When forming golden carbide, its oxidation-resistance improves, and especially when carbon wraps up, becomes and is the stabilized nano powdered material.
The preparation method of TaC nano-powder material is as follows:
Device loam cake shown in Figure 1 (shown in Figure 1 1) is opened, with the Ta metal sheet as target (shown in Figure 1 4), be placed on the copper anode that leads to water coolant (shown in Figure 1 7), make negative electrode (shown in Figure 1 2) with graphite, between copper anode that leads to water coolant and target is fine copper crucible (shown in Figure 1 10), the lid mounted device loam cake, logical water coolant (shown in Figure 1 8), whole working spaces vacuumizes and is higher than 10
-3Behind the Pa, feed argon gas, pressure is 20kPa; Inject 0.8ml ethanol for every liter by working spaces's volume; Connect the dc pulse power supply, voltage is 10-50V, between target and electrode arc discharge takes place.The electric current that produces arc-over is 10-600A.Adjusting working current and voltage keep relative stability in the arc discharge process.Ethanol decomposes in the arc discharge process, fusing of Ta metal sheet and evaporation and ionization, Ta and C chemical combination form the nano particle of TaC, are deposited on anode, sidewall and on cover.After finishing required arc discharge process, cut off the electricity supply, arc light extinguishes.Extract working spaces's gas out, inject the nano particle of air and argon gas passivation TaC, after passivation finishes, open the nano powder of the TaC in the loam cake collection work chamber.
The nano powder of TaC adds pure nitric acid (concentration about 65%) and places flask, ebuillition of heated (about 110 ℃) 3-5 hour, and the dilute with water centrifugation obtains sloughing the nano particle of the TaC of carbon shell.Fig. 2-Fig. 9 is the analytical test result, and Figure 10 is its structure iron, and these have proved it is the nano powder of TaC.
Advantage of the present invention: can stably obtain nano-scale TaC powder with this method.Owing to use ethanol, utilize it to decompose, provide the source of carbon in the gaseous state mode, increase the productive rate of the nano powder of TaC, and reduced uncombined carbon.
Description of drawings
The present invention is further detailed explanation below in conjunction with drawings and the embodiments:
Fig. 1 is for preparing the device synoptic diagram of TaC nano-powder material with arc plasma; 1 is the device loam cake among the figure, is used for opening unit; The 2nd, Graphite Electrodes; The 3rd, the interface that is used to vacuumize; The 4th, to be composition count Ta more than 99% by atom for consumable anode, used consumable anode; The 5th, viewing window; The 6th, the metal baffle that is used for collecting the TaC nano particle; The 7th, the water-cooled anode; The 8th, the import and export of water coolant; The 9th, adjustable water-cooled cathode chuck; The 10th, fine copper crucible, the thickness of copper crucible bottom are 3-50mm; The 11st, direct supply, during work, the electric current that produces arc-over is 10-600A, voltage is 8-50V; The 12nd, the argon gas inlet, ar pressure is 2kPa-0.5MPa, can also be used to importing the argon gas that contains the 0-70% air; The 13rd, the ethanol input aperture.TaC rice particle deposition or on the baffle plate, or on loam cake and the sidewall, and can be isolated TaC with physics or chemical process on the copper crucible as required.
Fig. 2 is the X-ray diffracting spectrum that covers the TaC metal compound nano powder material of carbon parcel on the deposition; Institute's scalar diffraction angle 34.8,40.4,58.54,69.4 and 73.62 is respectively the diffraction peak of TaC crystal face (111), (200), (220), (311) and (222) among the figure;
Fig. 3 is for covering the high-resolution electron microscopy photo of TaC nano-powder material for covering on the deposition of carbon parcel on the deposition; (a) the pattern picture of nano-powder material; (b) nano-powder material (111) face;
Fig. 4 is the TaC nano metal powder congeries that are deposited on carbon parcel on the target; (a), (b), (c), (d), (e) be the photo of 5mm to 2 μ m different scales;
Fig. 5 is null field cooling (ZFC) and band cooling (FC) curve of TaC thing nano-powder material; Superconducting transition temperature is 10K;
Fig. 6 is the magnetzation curve of TaC thing nano-powder material, illustrates that the TaC nanometer powder shows as nonideal type characteristic;
Fig. 7 is TaC nano-powder material 4f7/2 and 4f5/2 electron binding energy, and the electron binding energy of the 4f5/2 of TaC is 24.73 ev (eV), and the electron binding energy of 4f7/2 is 22.79 ev; The 4f5/2 electron binding energy of Ta is 23.5 ev, and the electron binding energy of 4f7/2 is 21.8 ev;
Fig. 8 is the electromicroscopic photograph of the TaC nanometer powder of decapsidate not on the battery lead plate;
Fig. 9 is for being heated to the TaC nanometer powder of 3 hours decapsidates of boiling with 65% nitric acid dousing;
Figure 10 is the structure iron of TaC, lattice parameter=4.465nm.
Embodiment
Embodiment 1
As target, ar pressure is 0.02MPa with the block of Ta, and the electric current that produces arc-over is 60-110A, and voltage is 15-25V, and ethanol is the 0.7ml/ liter by working spaces's volume.Behind the arc extinction, put into the air passivation of argon gas and the 0.02Mpa of 0.01Mpa, passivation time is 5 hours, the TaC nano-powder material of preparation.Fig. 2-Fig. 9 is the analytical test result.
As target, working gas is with argon gas and hydrogen with Ta, and pressure is 0.02MPa and 2kPa hydrogen, and the electric current that gas produces arc-over is 60-110A, and voltage is 15-25V, and ethanol is the 0.5ml/ liter by working spaces's volume.Behind the arc extinction, put into the air passivation of argon gas and the 0.02Mpa of 0.01Mpa, passivation time is 5 hours, prepares the TaC nano-powder material.Fig. 2-Fig. 9 is the analytical test result.
Claims (4)
1. method for preparing the TaC nano-powder material, the shell of nanometer powder is a carbon, it is characterized in that: as working gas, adopt arc-over to produce the technology of preparing of plasma body with argon gas and ethanol;
The composition of used consumable anode is Ta, and the composition of used consumption negative electrode is a graphite;
Preparation TaC nanometer powder is at argon gas and C
2H
5Carry out in the OH mixed atmosphere, ar pressure is 0.5kPa-0.5MPa, C
2H
5OH institute consumption is directly proportional with the working chamber volume, is the 0.05-5ml/ liter;
Used consumable anode and cathode distance are 0.1mm-5cm, and the electric current of arc-over is 8-600A, and voltage is 5-50V.
2. according to the described method for preparing the TaC nano-powder material of claim 1, it is characterized in that: described TaC nano-powder particles diameter is less than 50nm.
3. according to the described method for preparing the TaC nano-powder material of claim 1, it is characterized in that: the carbon thickness of the shell of described TaC nanometer powder is 2-5nm, sloughs unnecessary carbon with pure nitric acid heating.
4. according to the described method for preparing the TaC nano-powder material of claim 1, it is characterized in that: the anode Ta that is consumed, place the copper crucible on the water-cooled copper anode, the thickness of copper crucible bottom is 3-30mm.
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| CN101318653B true CN101318653B (en) | 2010-09-15 |
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| CN102447054B (en) * | 2010-10-13 | 2014-05-07 | 中国科学院金属研究所 | Mini-sized low-temperature ultralow-frequency signal element manufactured by carbon-coated TaC (Tantalum Carbide) nanometer capsules |
| CN102502635A (en) * | 2011-07-15 | 2012-06-20 | 中国科学院过程工程研究所 | Method for preparing surface-modified infusible metallic carbide ultrafine powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1548566A (en) * | 2003-05-07 | 2004-11-24 | 韩国机械研究院 | Process for manufacturing nano-phase TaC-transition metal based complex powder |
| CN1730435A (en) * | 2005-06-07 | 2006-02-08 | 中国科学院山西煤炭化学研究所 | The hot-forming method for preparing tantalum/charcoal carbide composite material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1548566A (en) * | 2003-05-07 | 2004-11-24 | 韩国机械研究院 | Process for manufacturing nano-phase TaC-transition metal based complex powder |
| CN1730435A (en) * | 2005-06-07 | 2006-02-08 | 中国科学院山西煤炭化学研究所 | The hot-forming method for preparing tantalum/charcoal carbide composite material |
Non-Patent Citations (2)
| Title |
|---|
| 闫志巧等.TaC粉末/涂层制备技术的研究进展.材料导报29 12.2005,29(12),80-83. |
| 闫志巧等.TaC粉末/涂层制备技术的研究进展.材料导报29 12.2005,29(12),80-83. * |
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