CN108751197B - Method for preparing 3D carbide nanowire array in situ by precursor impregnation cracking and magnetic pulling method - Google Patents
Method for preparing 3D carbide nanowire array in situ by precursor impregnation cracking and magnetic pulling method Download PDFInfo
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Abstract
The invention relates to a method for preparing a 3D carbide nanowire array in situ by a precursor impregnation cracking and magnetic pulling method, which combines the precursor impregnation cracking and the magnetic pulling method and synthesizes a three-dimensional carbide nanowire array on the surface of a graphite sheet in situ. Preparing nanoscale iron oxide on the surface of the high-purity graphite flake by a coprecipitation method, and preparing Fe nanoparticles by hydrogen reduction; and then, putting the graphite flake containing Fe particles into a ZrC precursor for dipping, and then carrying out heat treatment under a magnetic field environment to obtain the ZrC nanowire array. The preparation method is simple, the nano wire can be designed, is pollution-free, safe and stable, the field emission performance and the electromagnetic wave absorption performance of the carbide nano material are improved, the field emission starting voltage of the material is reduced, and the combination of the matrix and the coating is enhanced. The material is widely applied to ceramic matrix composite materials, resin matrix composite materials, field emission pole shoe materials and hard alloys, and has good economic and social benefits.
Description
Technical Field
The invention belongs to an application technology of a three-dimensional carbide nanowire array in the technical field of composite materials, functional materials and alloys by precursor impregnation cracking and magnetic pulling in-situ preparation, and relates to a method for preparing a 3D carbide nanowire array in situ by precursor impregnation cracking and magnetic pulling.
Background
The carbide nano material has the characteristics of high melting point, high-temperature specific strength and specific modulus, good wave-absorbing performance, excellent heat-conducting performance, strong chemical stability and the like, and is widely applied to the fields of aerospace, military, medicine and building. Carbides are binary compounds of carbon with elements (other than hydrogen) having a smaller or similar electronegativity than carbon,the properties of elements are classified into metal carbides and non-metal carbides. The metallic carbide is a binary compound formed by d transition elements, especially VIB and VIIB and iron series elements and carbon. The structure is characterized in that carbon atoms are filled in tetrahedral holes of a close-packed metal lattice, and the conductivity of the metal is not influenced. For atomic radii greater than
The carbon atoms do not deform the metal lattice, but rather make the lattice more compact and solid. Carbides of these metals have extremely high melting points and hardness, such as tantalum carbide and tungsten carbide. Non-metallic carbides include silicon carbide and boron carbide. In these carbides, carbon atoms are covalently bonded to silicon and boron atoms, and belong to an atomic crystal. They are characterized by high hardness, high melting point and stable chemical properties.
One-dimensional nanomaterials have special properties that are distinct from the bulk. When the diameter of the material is equal to the de broglie wavelength, the conduction band and the valence band are further enlarged, the energy gap is increased along with the reduction of the diameter of the nano material, and the nonlinear optical and quantum effects are more and more obvious. The one-dimensional nano materials such as silicon carbide, zirconium carbide, boron carbide, titanium carbide, aluminum carbide and the like have stronger quantum size effect and better optical and field emission performance, and have good application prospect in the field of micro-nano manufacturing. Therefore, the research on the one-dimensional carbide nano material is one of the research hotspots in the field of condensed physical and micro-nano materials at present.
However, the biggest disadvantage of the one-dimensional nano material is that the growth direction is not controllable, which severely limits the designability of the one-dimensional carbide nano material. In the field of field emission, the carbon nano tube and the silicon carbide nano array are directionally designed, so that the current density of field emission can be greatly improved, and the threshold of starting voltage can be reduced; in the wave absorbing field, the absorption of electromagnetic waves can be realized by designing the arrangement mode of the carbide nano array; in the optical field, the characteristics of wide band gap, high critical breakdown voltage and high carrier saturation drift velocity of one-dimensional carbide are utilized, and the reasonably designed nano array can be applied to a photoluminescence device; in the field of composite materials, the multi-scale mechanical design of the composite material and the anti-oxidation and anti-ablation design of a composite material coating are realized by directionally designing the growth direction of the refractory metal carbide nanowires.
At present, the preparation method of the one-dimensional nanowire array mainly comprises an alumina template method, a catalyst assisted growth method and an electrochemical deposition method. The alumina template method is to inject the precursor of carbide into the template, then sinter the precursor under certain conditions, and then corrode the template to prepare the nanowire/tube array. The catalyst assisted growth method is that the catalyst is prepared on the substrate in the modes of evaporation, sputtering and coprecipitation, and then the nanowire array is prepared in the modes of sol-gel, chemical vapor deposition and precursor impregnation cracking. The electrolytic deposition method is to form a compact oxide film at the anode, and to randomly dissolve the oxide film by changing the intensity of the surrounding electric field because the oxide film with poor electrical properties is damaged by the oxidation-reduction reaction. When the deposition and dissolution reach balance, the stable growth of the nanowire array can be realized.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing a 3D carbide nano-wire array in situ by a precursor impregnation cracking and magnetic pulling method, and provides a method for synthesizing a carbide nano-wire array in situ by a precursor impregnation cracking and magnetic pulling technology. The method is simple in preparation, pollution-free, safe and stable, and can greatly improve the field emission performance and the electromagnetic wave absorption performance of the carbide nano material, reduce the field emission starting voltage of the material and enhance the combination of the substrate and the coating. The composite material can be widely applied to ceramic matrix composite materials (carbon/carbon, carbon/ceramic, magnesium-based and aluminum-based composite materials), resin matrix composite materials, field emission pole shoe materials and hard alloys, and has good economic and social benefits.
Technical scheme
A method for preparing a 3D carbide nanowire array in situ by precursor impregnation cracking and magnetic pull is characterized by comprising the following steps:
step 1, preparing nano Fe particles on a graphite sheet by a coprecipitation method: dissolving urea, ferric nitrate nonahydrate and deionized water in a beaker, magnetically stirring for 30-60min, transferring the solution into a polytetrafluoroethylene inner container filled with graphite sheets, and sealing and filling the kettle;
placing the reaction kettle in an oven, and keeping the temperature at 180 ℃ for 1-3h at 120-;
taking out the graphite flakes in the reaction kettle, drying, then placing in a horizontal heat treatment furnace, setting the reduction temperature of hydrogen at 500-700 ℃, the reduction time at 1-3h, introducing hydrogen and argon simultaneously, and setting the flow ratio of the two gases to be 2: 1;
cooling to room temperature, taking out to obtain a large amount of nano Fe particles attached to the surface of the graphite flake;
putting the graphite flake into alcohol to ultrasonically clean for 30-60 min; the molar ratio of the urea to the ferric nitrate nonahydrate is 3: 2;
step 2, preparing ZrC precursor particles on a graphite sheet:
putting the graphite flake containing the nano Fe particles into a ZrC precursor solution for dipping for 1-3 days, taking out, drying and dipping again, repeating the steps for 3 times, and thus obtaining ZrC precursor solid particles on the surface of the graphite flake;
the ZrC precursor solution is as follows: dissolving 1-5g of ZrC precursor solid particles in an acetone solution, and magnetically stirring for 2-5h to prepare a ZrC precursor solution;
step 3, preparing the ZrC nanowire array by magnetic pulling:
filling the graphite flake with the ZrC precursor solid particles attached to the surface, which is obtained in the step 2, in a corundum polycrystalline ceramic pipeline, vacuumizing a furnace chamber, and then opening an argon valve for flushing; repeating the steps for 3 times;
introducing argon gas for protection in the whole process, wherein the argon gas flow is 50-200SCCM, adding a magnetic field at the top end of the graphite sheet, the direct current voltage for generating the magnetic field is 10-200V, the current is 1-3A, the magnetic attraction is 5-1000N, and the magnetic field is opened in the whole process;
starting a temperature and time control program, raising the temperature to 1300-1500 ℃, raising the temperature at the rate of 6-7 ℃/min, keeping the temperature for 0.5-3h, and carrying out program cooling for 3-5 h;
and naturally cooling to room temperature to finish the preparation of the 3D carbide nanowire array.
Advantageous effects
The invention provides a method for preparing a 3D carbide nanowire array in situ by a precursor immersion cracking and magnetic pulling method. Preparing nanoscale Fe particles on the surfaces of graphite sheets by adopting a coprecipitation technology, and then putting the graphite sheets (G/Fe) with the Fe particles into a zirconium carbide precursor (PZrC) solution for soaking for a certain time to prepare a G/Fe/PZrC complex system material; then, the composite material is crosslinked and cured at a low temperature stage, and then is subjected to heat treatment at a high temperature stage, but a magnetic field needs to be loaded and inert gas needs to be introduced for protection in the whole heat treatment stage; and cooling to room temperature to prepare the 3D zirconium carbide nanowire array. The 3D zirconium carbide nanowire grows uniformly on the surface of a graphite flake, has good crystallinity and controllable growth direction, and does not have any bending phenomenon. The carbide nano material has the advantages of small diameter, large enhancement factor and consistent direction, can greatly improve the field emission performance of the carbide nano material and greatly reduce the field emission starting voltage, and can be widely applied to pole shoe materials of field emission scanning electron microscopes and transmission electron microscopes. Meanwhile, the zirconium carbide has excellent radiation resistance, the resistivity is 250 times lower than that of silicon carbide, the conductivity is 23 times of that of the silicon carbide, and the effective use temperature is 2 times of that of the silicon carbide, so that the zirconium carbide can be widely applied to high-power and high-temperature radiation-resistant micro-nano devices in the aerospace field. In addition, the in-situ preparation of the carbide nano array on the surface of the composite material can greatly improve the combination of the matrix and the coating and effectively improve the oxidation resistance and the ablation resistance of the composite material.
The invention directionally prepares the 3D refractory metal carbide nanowire/tube array on the surface of the substrate by applying external force (magnetic field) control, can improve the field emission performance and the electromagnetic wave absorption performance of the carbide nano material, reduces the field emission starting voltage of the material, and enhances the combination of the substrate and the coating. The preparation method is simple, the nano wire can be designed, is pollution-free, safe and stable, the field emission performance and the electromagnetic wave absorption performance of the carbide nano material can be greatly improved, the field emission starting voltage of the material is reduced, and the combination of the matrix and the coating is enhanced. The composite material can be widely applied to ceramic matrix composite materials (carbon/carbon, carbon/ceramic, magnesium-based and aluminum-based composite materials), resin matrix composite materials, field emission pole shoe materials and hard alloys, and has good economic and social benefits.
Drawings
FIG. 1: process flow chart for preparing carbide nanowire array by precursor impregnation cracking and magnetic pulling technology
FIG. 2: device diagram for preparing carbide nano-wire by magnetic pulling method
FIG. 3: SEM image of ZrC nanowire array grown in situ on surface of graphite sheet by magnetic pulling method
(a) Low power morphology, (b) high power morphology
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the raw materials used in the invention are: ZrC precursor, ferric nitrate nonahydrate, urea, deionized water, absolute ethyl alcohol, acetone, hydrogen and argon.
The invention uses equipment: the device comprises a horizontal heat treatment furnace, an electromagnetic device, an oven, an ultrasonic cleaner, a magnetic stirring instrument and a reaction kettle.
The method comprises the following steps:
(1) preparation of nano Fe particles on graphite sheet by coprecipitation method
Firstly, putting graphite flakes into a beaker containing alcohol, and then putting the beaker into an ultrasonic cleaner for cleaning for 30-60 min.
Weighing a plurality of grams of urea and ferric nitrate nonahydrate, dissolving the urea and the ferric nitrate nonahydrate in a beaker by using deionized water, wherein the molar ratio of the urea to the ferric nitrate nonahydrate is 3:2, magnetically stirring for 30-60min, transferring the solution into a polytetrafluoroethylene inner container filled with graphite sheets, and sealing and filling the inner container into a kettle.
Thirdly, the reaction kettle is arranged in an oven, the highest temperature of the oven is 120 and 180 ℃, and the temperature is kept for 1-3 h.
Taking out the graphite flake in the reaction kettle, drying the graphite flake, placing the graphite flake in a horizontal heat treatment furnace, setting the reduction temperature of hydrogen at 500-.
And fifthly, cooling the temperature to room temperature and taking out the graphite flake to obtain a large amount of nano Fe particles attached to the surface of the graphite flake.
(2) Preparation of ZrC precursor particles on graphite sheet
Weighing 1-5g of ZrC precursor solid particles, dissolving in an acetone solution, and magnetically stirring for 2-5h to obtain the ZrC precursor solution.
And secondly, putting the graphite flake containing the nano Fe particles into a ZrC precursor solution for dipping for 1-3 days, taking out, drying and dipping again, and repeating the steps for 3 times to obtain ZrC precursor solid particles with a certain content on the surface of the graphite flake.
(3) ZrC nanowire array prepared by magnetic drawing
The samples were run in a horizontal high temperature tube furnace.
Filling a sample in a pipeline of corundum polycrystalline ceramic. And vacuumizing the furnace chamber, and then opening an argon valve for flushing. This was repeated 3 times.
Introducing argon for protection in the whole process, wherein the flow of the argon is 50-200SCCM, adding a magnetic field at the top end of the sample, and opening the magnetic field in the whole process.
Starting a temperature and time control program, raising the temperature to 1300 ℃ and 1500 ℃, keeping the temperature for 0.5-3h at the temperature raising rate of 6-7 ℃/min, and carrying out program cooling for 3-5 h.
Closing the program, naturally cooling to room temperature, and sampling.
Example 1
The high-purity graphite flake is cut into 20X 5mm flakes by a cutter, and the flakes are put into a beaker containing alcohol and then cleaned in an ultrasonic cleaner for 30 min. Weighing a plurality of grams of urea and ferric nitrate nonahydrate, dissolving the urea and the ferric nitrate nonahydrate in a beaker by using deionized water, wherein the molar ratio of the urea to the ferric nitrate nonahydrate is 3:2, magnetically stirring for 30min, transferring the solution into a polytetrafluoroethylene inner container filled with graphite sheets, and sealing and filling the kettle. And (3) placing the reaction kettle in an oven, wherein the highest temperature of the oven is 120 ℃, and keeping the temperature for 1 h. Taking out the graphite flake in the reaction kettle, drying the graphite flake, putting the graphite flake in a horizontal heat treatment furnace, setting the reduction temperature of hydrogen at 500 ℃ for 1h, and simultaneously introducing hydrogen and argon, wherein the flow ratio of the two gases is 2: 1. When the temperature is reduced to room temperature, the graphite flake is taken out, and a large amount of nano Fe particles attached to the surface of the graphite flake can be obtained.
Weighing 1g of ZrC precursor solid particles, dissolving in an acetone solution, and magnetically stirring for 2h to obtain the ZrC precursor solution. And (3) putting the graphite flake containing the nano Fe particles into a ZrC precursor solution, soaking for 1 day, taking out, drying, soaking again, and repeating the steps for 3 times to obtain ZrC precursor solid particles with a certain content on the surface of the graphite flake.
The samples were run in a horizontal high temperature tube furnace. The samples were loaded into tubes of corundum polycrystalline ceramic. And vacuumizing the furnace chamber, and then opening an argon valve for flushing. This was repeated 3 times. Argon is introduced for protection in the whole process, the argon flow is 50SCCM, a magnetic field is added at the top end of the sample, and the magnetic field is opened in the whole process. Starting a temperature and time control program, raising the temperature to 1400 ℃, raising the temperature rate to 6 ℃/min, keeping the temperature for 1h, and carrying out program cooling for 3 h; the program is closed, the temperature is naturally reduced to the room temperature, and the sample is taken.
Example 2
The high-purity graphite flake is cut into 20X 5mm flakes by a cutter, and the flakes are put into a beaker containing alcohol and then cleaned in an ultrasonic cleaner for 60 min. Weighing a plurality of grams of urea and ferric nitrate nonahydrate, dissolving the urea and the ferric nitrate nonahydrate in a beaker by using deionized water, wherein the molar ratio of the urea to the ferric nitrate nonahydrate is 3:2, magnetically stirring for 60min, transferring the solution into a polytetrafluoroethylene inner container filled with graphite sheets, and sealing and filling the kettle. And (3) placing the reaction kettle in an oven, wherein the highest temperature of the oven is 180 ℃, and keeping the temperature for 3 hours. Taking out the graphite flake in the reaction kettle, drying the graphite flake, putting the graphite flake in a horizontal heat treatment furnace, setting the reduction temperature of hydrogen at 700 ℃, the reduction time at 3h, and simultaneously introducing hydrogen and argon, wherein the flow ratio of the two gases is 2: 1. When the temperature is reduced to room temperature, the graphite sheet is taken out, and a large amount of nano Fe particles attached to the surface of the graphite sheet can be obtained.
Weighing 3g of ZrC precursor solid particles, dissolving in an acetone solution, and magnetically stirring for 5h to obtain the ZrC precursor solution. And (3) putting the graphite flake containing the nano Fe particles into a ZrC precursor solution, dipping for 3 days, taking out, drying, dipping again, and repeating the steps for 3 times to obtain ZrC precursor solid particles with a certain content on the surface of the graphite flake.
The samples were loaded into tubes of corundum polycrystalline ceramic. And vacuumizing the furnace chamber, and then opening an argon valve for flushing. This was repeated 3 times. Argon is introduced for protection in the whole process, the argon flow is 200SCCM, a magnetic field is added at the top end of the sample, and the magnetic field is opened in the whole process. Starting a temperature and time control program, raising the temperature to 1500 ℃, raising the temperature rate to 7 ℃/min, preserving the heat for 3h, and carrying out program cooling for 5 h. The program is closed, the temperature is naturally reduced to the room temperature, and the sample is taken.
Graphite in all the examples>99.99 percent of urea>99.9％，Fe(NO3)2·9H2O>98% absolute ethanol and Acetone (AR), CH4>99.9％，Ar>99.999％，H2>99.999％。
Claims (1)
1. A method for preparing a 3D carbide nanowire array in situ by precursor impregnation cracking and magnetic pull is characterized by comprising the following steps:
step 1, preparing nano Fe particles on a graphite sheet by a coprecipitation method: putting the graphite flake into alcohol to ultrasonically clean for 30-60 min; dissolving urea, ferric nitrate nonahydrate and deionized water in a beaker, magnetically stirring for 30-60min, transferring the solution into a polytetrafluoroethylene inner container filled with graphite sheets, and sealing and filling the kettle;
placing the reaction kettle in an oven, and keeping the temperature at 180 ℃ for 1-3h at 120-;
taking out the graphite flakes in the reaction kettle, drying, then placing in a horizontal heat treatment furnace, setting the reduction temperature of hydrogen at 500-700 ℃, the reduction time at 1-3h, introducing hydrogen and argon simultaneously, and setting the flow ratio of the two gases to be 2: 1;
cooling to room temperature, taking out to obtain a large amount of nano Fe particles attached to the surface of the graphite flake;
the molar ratio of the urea to the ferric nitrate nonahydrate is 3: 2;
step 2, preparing ZrC precursor particles on a graphite sheet:
putting the graphite flake containing the nano Fe particles into a ZrC precursor solution for dipping for 1-3 days, taking out, drying and dipping again, repeating the steps for 3 times, and thus obtaining ZrC precursor solid particles on the surface of the graphite flake;
the ZrC precursor solution is as follows: dissolving 1-5g of ZrC precursor solid particles in an acetone solution, and magnetically stirring for 2-5h to prepare a ZrC precursor solution;
step 3, preparing the ZrC nanowire array by magnetic pulling:
filling the graphite flake with the ZrC precursor solid particles attached to the surface, which is obtained in the step 2, in a corundum polycrystalline ceramic pipeline, vacuumizing a furnace chamber, and then opening an argon valve for flushing; repeating the steps for 3 times;
introducing argon gas for protection in the whole process, wherein the argon gas flow is 50-200SCCM, adding a magnetic field at the top end of the graphite sheet, the direct current voltage for generating the magnetic field is 10-200V, the current is 1-3A, the magnetic attraction is 5-1000N, and the magnetic field is opened in the whole process;
starting a temperature and time control program, raising the temperature to 1300-1500 ℃, raising the temperature at the rate of 6-7 ℃/min, keeping the temperature for 0.5-3h, and carrying out program cooling for 3-5 h;
and naturally cooling to room temperature to finish the preparation of the 3D carbide nanowire array.
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