CN108751197A - The method that 3D carbide nanometer linear arrays are prepared in situ with magnetic pulling method in polymer infiltration and pyrolysis - Google Patents
The method that 3D carbide nanometer linear arrays are prepared in situ with magnetic pulling method in polymer infiltration and pyrolysis Download PDFInfo
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- CN108751197A CN108751197A CN201810853080.3A CN201810853080A CN108751197A CN 108751197 A CN108751197 A CN 108751197A CN 201810853080 A CN201810853080 A CN 201810853080A CN 108751197 A CN108751197 A CN 108751197A
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Abstract
The present invention relates to a kind of methods that 3D carbide nanometer linear arrays are prepared in situ in polymer infiltration and pyrolysis and magnetic pulling method, are combined with magnetic pulling method using polymer infiltration and pyrolysis, in the method that graphite flake surface in situ synthesizes three-dimensional carbide nano-wire array.Nanoscale iron oxide is prepared on high purity graphite piece surface by coprecipitation, then nanometer Fe particle is prepared by hydrogen reducing；The graphite flake containing Fe particles is placed in ZrC presomas again and is impregnated, can be prepared by ZrC nano-wire arrays by heat treatment under magnetic field environment.Preparation method of the present invention is simple, nano wire can design, pollution-free and safety and stability, improve the field emission performance and electromagnetic wave absorption performance of carbide nanometer material, reduce the Flied emission cut-in voltage of material, the combination of enhancing matrix and coating.It is widely used in ceramic matric composite, polymer matrix composites, Flied emission pole shoe material and hard alloy, there is economic and social benefit well.
Description
Technical field
The invention belongs to polymer infiltration and pyrolysis and magnetic pulling method, and three-dimensional carbide nano-wire array is prepared in situ in composite wood
The application technology of material, functional material and technical field of alloy is related to a kind of polymer infiltration and pyrolysis and 3D is prepared in situ with magnetic pulling method
The method of carbide nanometer linear array is combined using polymer infiltration and pyrolysis with magnetic pulling method, is synthesized in graphite flake surface in situ
The method of three-dimensional carbide nano-wire array.
Background technology
Carbide nanometer material is high with fusing point, high temperature specific strength and specific modulus are big, absorbing property is good, heat conductivility is excellent
Different, the features such as chemical stability is strong, it is widely used in aerospace, military affairs, medicine and building field.Carbide is carbon and electricity
The binary compound that negativity is less than that or similar element is generated (outside dehydrogenation), metal carbon is divided into from attribute of an element
Compound and non-metallic carbide.Metal mold carbide is d transition elements, and especially VI B, VII B races and iron series element and carbon are formed
Binary compound.It is structurally characterized in that carbon atom is filled in the tetrahedron hole of closs packing metal lattice, does not influence metal
Electric conductivity.Atomic radius is more thanMetal, carbon atom will not be such that metal lattice deforms, only make lattice closer
It is solid.The carbide of these metals has high fusing point and hardness, such as ramet and tungsten carbide.Non-metallic carbide includes
Silicon carbide and boron carbide.In these carbide, carbon atom, with Covalent bonding together, belongs to atomic crystal with silicon, boron atom.They have
Have the characteristics that high rigidity, high-melting-point and chemical property are stablized.
Monodimension nanometer material has the special nature completely different with block.When the diameter and its de Broglie wavelength of material
When suitable, conduction band further expands with valence band, and energy gap is as the diameter of nano material reduces and increases, nonlinear optics and quantum
Effect performance is more and more obvious.The monodimension nanometer materials such as silicon carbide, zirconium carbide, boron carbide, titanium carbide and aluminium carbide have relatively strong
Quantum size effect and preferable optics, field emission performance, field of micro-Na manufacture have good application prospect.Therefore,
Study one of the research hotspot that one-dimensional carbide nanometer material is current Condensed Matter Physics and micro-nano material field.
However, the disadvantage of monodimension nanometer material is exactly that the direction of growth is uncontrollable, seriously limits one-dimensional carbide and receive
The design of rice material.In Flied emission field, the design carbon nanotube and nanometer silicon carbide array of orientation are greatly improved field
The current density and reduction turn on voltage threshold of transmitting；Wave field is being inhaled, by the arrangement side for designing carbide nanometer array
Formula can realize the absorption to electromagnetic wave；In optical field, the broad-band gap of one-dimensional carbide, high disruptive critical voltage, high load are utilized
The characteristics of flowing sub- saturation drift velocity rationally designs nano-array and can be applied to photo luminescent devices；In field of compound material, lead to
The direction of growth for crossing rational design refractory carbide nano wire is realized to the design of composite material multiple dimensioned mechanics and is realized
Anti-oxidation and anti-yaw damper design to composite coating.
Currently, including mainly alumina formwork method, catalyst assisting growth for the preparation method of one-dimensional nano line array
Method, electrochemical deposition method.Alumina formwork method be first by carbide presoma injection template in, after burnt by certain condition
Knot, then template is corroded, prepare nanowire/pipe array.Catalyst assisting growth method is first by catalyst by evaporating, splashing
The mode penetrate, being co-precipitated is prepared on substrate, then by way of collosol and gel, chemical vapor deposition, polymer infiltration and pyrolysis
Prepare nano-wire array.Strike is that fine and close oxidation film is initially formed in anode, broken since redox reaction occurs
The poor oxidation film of bad electric property reaches random Dissolve oxidation film by changing surrounding electric field intensity.When deposition is reached with dissolving
Stablizing for nano-wire array can be realized to balance to grow.
Invention content
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes that a kind of polymer infiltration and pyrolysis is made in situ with magnetic pulling method
The method of standby 3D carbide nanometer linear arrays, provides a kind of polymer infiltration and pyrolysis+magnetic pull technology fabricated in situ carbide nanometer
Array.This method prepares simple, pollution-free and safety and stability, is greatly improved the field emission performance and electricity of carbide nanometer material
Electro-magnetic wave absorption performance reduces the Flied emission cut-in voltage of material, enhances the combination of matrix and coating.It can be widely applied to ceramic base
Composite material (carbon/carbon, carbon/pottery, magnesium-based, aluminum matrix composite), polymer matrix composites, Flied emission pole shoe material and hard
In alloy, there is economic and social benefit well.
Technical solution
A kind of method that 3D carbide nanometer linear arrays are prepared in situ with magnetic pulling method in polymer infiltration and pyrolysis, it is characterised in that
Steps are as follows：
Step 1, coprecipitation prepare nanometer Fe particle on graphite flake：By urea and Fe(NO3)39H2O and deionized water
Be dissolved in beaker, magnetic agitation 30-60min, after by solution move into equipped with graphite flake polytetrafluoroethylliner liner in, packing dress
Kettle；
Reaction kettle is placed in baking oven, in 120-180 DEG C of constant temperature 1-3h；
The graphite flake drying in reaction kettle is taken out, is placed in horizontal type heat-treatment furnace, the temperature that hydrogen reducing is arranged is
500-700 DEG C, recovery time 1-3h, hydrogen is passed through simultaneously with argon gas, and the flow proportional of two kinds of gas is 2:1；
Temperature is down to room temperature taking-up, obtains a large amount of nanometer Fe particle and is attached on graphite flake surface；
The graphite flake, which is placed in alcohol, is cleaned by ultrasonic 30-60min；The molar ratio of the urea and Fe(NO3)39H2O is
3:2；
Step 2 prepares ZrC granular precursors on graphite flake：
Graphite flake containing nanometer Fe particle is placed in ZrC precursor solutions and is impregnated 1-3 days, drying is taken out and impregnates again,
3 times repeatedly, i.e., ZrC presoma solid granulates are made on graphite flake surface；
The ZrC precursor solutions are：1-5g ZrC presoma solid particles are dissolved in acetone soln, magnetic agitation 2-
ZrC precursor solutions are made in 5h；
Step 3, magnetic draw standby ZrC nano-wire arrays：
The graphite flake that the surface that step 2 obtains is adhered to ZrC presoma solid granulates is loaded on the pipe of corundum polycrystalline ceramics
In road, furnace chamber is vacuumized, argon gas valve is opened later, is rinsed；3 times repeatedly；
Whole process is passed through argon gas protection again, and argon flow amount 50-200SCCM is added magnetic field on graphite flake top, generates magnetic field
DC voltage is 10-200V, electric current 1-3A, magnetic pull 5-1000N, and magnetic field whole process is opened；
Temperature is raised to 1300-1500 DEG C by start-up temperature time control program, and 6-7 DEG C of heating rate/min keeps the temperature 0.5-
3h, program cooling, temperature fall time 3-5h；
Naturally it is down to room temperature, completes to prepare 3D carbide nanometer linear arrays.
Advantageous effect
The side of 3D carbide nanometer linear arrays is prepared in situ with magnetic pulling method for a kind of polymer infiltration and pyrolysis proposed by the present invention
Method uses polymer infiltration and pyrolysis and magnetic pulling method combined technology, 3D zirconium carbides is prepared in graphite flake surface in situ for the first time
(ZrC) nano-wire array.The method first prepares nanoscale Fe particles using chemical coprecipitation technique on graphite flake surface, then will carry Fe
The graphite flake (G/Fe) of particle, which is placed in zirconium carbide presoma (PZrC) solution, impregnates certain time, and it is multiple to prepare G/Fe/PZrC
Fit based material；Again by the composite material prior to cold stage crosslinking curing, after be heat-treated in hot stage, but entire heat treatment
Stage need to load magnetic field and be passed through inert gas shielding；3D zirconium carbide nano-wire arrays can be prepared by being cooled to room temperature.The 3D
Zirconium carbide nano wire grows uniform, good crystallinity, the direction of growth controllably on graphite flake surface and nano wire is without any buckling phenomenon.
Due to its diameter compared with small, enhancement factor is big, direction be unanimously greatly improved carbide nanometer material field emission performance and greatly
Reduction Flied emission cut-in voltage, can be extensively using the pole shoe material for making in field emission scanning electron microscope, transmission electron microscope.Meanwhile by
Excellent in the radiation resistance of zirconium carbide, resistivity ratio silicon carbide is 250 times small, and conductivity is 23 times of silicon carbide, effectively uses
Temperature is 2 times of silicon carbide, can be widely applied to aerospace field is high-power, in high temperature radioresistance micro-nano device.In addition,
The combination that carbide nano-array is greatly improved matrix and coating is prepared in situ in composite material surface, effectively improves composite wood
The anti-oxidation and Burning corrosion resistance energy of material.
The present invention is controlled by applying external force (magnetic field), in matrix surface beam system for 3D refractory carbide nanometers
Line/pipe array, can be improved the field emission performance and electromagnetic wave absorption performance of carbide nanometer material, and the Flied emission for reducing material is opened
Voltage is opened, the combination of matrix and coating is enhanced.Preparation method of the present invention is simple, nano wire can design, pollution-free and safety surely
It is fixed, it is greatly improved the field emission performance and electromagnetic wave absorption performance of carbide nanometer material, the Flied emission for reducing material is opened
Voltage enhances the combination of matrix and coating.Can be widely applied to ceramic matric composite, (carbon/carbon, carbon/pottery, magnesium-based, aluminium base are multiple
Condensation material), polymer matrix composites, in Flied emission pole shoe material and hard alloy, there is economic well and society's effect
Benefit.
Description of the drawings
Fig. 1：Polymer infiltration and pyrolysis prepares carbide nanometer linear array process flow chart with magnetic pull technology
Fig. 2：Magnetic pulling method prepares the installation drawing of carbide nanometer line
Fig. 3：Magnetic pulling method grows the SEM figures of ZrC nano-wire arrays in graphite flake surface in situ
(a) low power pattern, (b) high power pattern
Specific implementation mode
In conjunction with embodiment, attached drawing, the invention will be further described：
The raw material that the present invention uses has：ZrC presomas, Fe(NO3)39H2O, urea, deionized water, absolute ethyl alcohol, third
Ketone, hydrogen, argon gas.
The present invention uses equipment：It is horizontal type heat-treatment furnace, calutron, baking oven, ultrasonic washing instrument, magnetic agitation instrument, anti-
Answer kettle.
Steps are as follows：
(1) coprecipitation prepares nanometer Fe particle on graphite flake
1. first graphite flake is placed in containing in spirituous beaker, after be put into ultrasonic washing instrument and clean 30-60min.
2. weighing several grams of urea and Fe(NO3)39H2O, be dissolved in beaker with deionized water, wherein urea and
The molar ratio of Fe(NO3)39H2O is 3:2, magnetic agitation 30-60min, after by solution move into equipped with graphite flake polytetrafluoroethylene (PTFE)
In liner, filling tank is sealed.
3. reaction kettle is placed in baking oven, baking oven maximum temperature is 120-180 DEG C, constant temperature 1-3h.
4. taking out the graphite flake in reaction kettle, it is baked to, is placed in horizontal type heat-treatment furnace, the temperature of hydrogen reducing is set
Degree is 500-700 DEG C, and recovery time 1-3h, hydrogen is passed through simultaneously with argon gas, and the flow proportional of two kinds of gas is 2:1.
5. temperature is down to room temperature taking-up, you can obtain a large amount of nanometer Fe particle and be attached on graphite flake surface.
(2) ZrC granular precursors are prepared on graphite flake
1. weighing 1-5g ZrC presoma solid particles to be dissolved in acetone soln, magnetic agitation 2-5h can be prepared by ZrC
Precursor solution.
It is impregnated 1-3 days 2. the graphite flake containing nanometer Fe particle is placed in ZrC precursor solutions, takes out drying and soak again
Stain, 3 times repeatedly, you can the ZrC presoma solid granulates of certain content are made on graphite flake surface.
(3) magnetic draws standby ZrC nano-wire arrays
Sample carries out in horizontal type high temperature process furnances.
1. sample is loaded in the pipeline of corundum polycrystalline ceramics.Furnace chamber is vacuumized, opens argon gas valve later, into
Row rinses.3 times repeatedly.
2. whole process is passed through argon gas protection, magnetic field is added on sample top in argon flow amount 50-200SCCM, and magnetic field whole process is opened
It opens.
3. temperature is raised to 1300-1500 DEG C by start-up temperature time control program, 6-7 DEG C of heating rate/min is kept the temperature
0.5-3h, program cooling, temperature fall time 3-5h.
4. bolt down procedure is down to room temperature naturally, sampling.
Embodiment 1
High purity graphite piece is cut into the thin slice of 20 × 20 × 5mm with cutting machine, graphite flake is placed in containing spirituous beaker
In, after be put into ultrasonic washing instrument and clean 30min.Weigh several grams of urea and Fe(NO3)39H2O, with deionized water by its
It is dissolved in beaker, wherein the molar ratio of urea and Fe(NO3)39H2O is 3:2, magnetic agitation 30min, after by solution move into fill
Have in the polytetrafluoroethylliner liner of graphite flake, seals filling tank.Reaction kettle is placed in baking oven, baking oven maximum temperature is 120 DEG C, permanent
Warm 1h.The graphite flake in reaction kettle is taken out, is baked to, is placed in horizontal type heat-treatment furnace, the temperature that hydrogen reducing is arranged is
500 DEG C, recovery time 1h, hydrogen is passed through simultaneously with argon gas, and the flow proportional of two kinds of gas is 2:1.When temperature is down to room temperature
It takes out, you can obtain a large amount of nanometer Fe particle and be attached on graphite flake surface.
It weighs 1g ZrC presoma solid particles to be dissolved in acetone soln, magnetic agitation 2h can be prepared by ZrC presomas
Solution.Graphite flake containing nanometer Fe particle is placed in ZrC precursor solutions and is impregnated 1 day, drying is taken out and impregnates again, it is so anti-
It is 3 times multiple, you can the ZrC presoma solid granulates of certain content are made on graphite flake surface.
Sample carries out in horizontal type high temperature process furnances.Sample is loaded in the pipeline of corundum polycrystalline ceramics.To furnace chamber into
Row vacuumizes, and opens argon gas valve later, is rinsed.3 times repeatedly.Whole process is passed through argon gas and protects, argon flow amount 50SCCM,
Magnetic field is added on sample top, magnetic field whole process is opened.Temperature is raised to 1400 DEG C, heating speed by start-up temperature time control program
6 DEG C/min of rate keeps the temperature 1h, program cooling, temperature fall time 3h；Bolt down procedure is down to room temperature naturally, sampling.
Embodiment 2
High purity graphite piece is cut into the thin slice of 20 × 20 × 5mm with cutting machine, graphite flake is placed in containing spirituous beaker
In, after be put into ultrasonic washing instrument and clean 60min.Weigh several grams of urea and Fe(NO3)39H2O, with deionized water by its
It is dissolved in beaker, wherein the molar ratio of urea and Fe(NO3)39H2O is 3:2, magnetic agitation 60min, after by solution move into fill
Have in the polytetrafluoroethylliner liner of graphite flake, seals filling tank.Reaction kettle is placed in baking oven, baking oven maximum temperature is 180 DEG C, permanent
Warm 3h.The graphite flake in reaction kettle is taken out, is baked to, is placed in horizontal type heat-treatment furnace, the temperature that hydrogen reducing is arranged is
700 DEG C, recovery time 3h, hydrogen is passed through simultaneously with argon gas, and the flow proportional of two kinds of gas is 2:1.When temperature is down to room temperature
It takes out, you can obtain a large amount of nanometer Fe particle and be attached to graphite flake surface.
It weighs 3g ZrC presoma solid particles to be dissolved in acetone soln, magnetic agitation 5h can be prepared by ZrC presomas
Solution.Graphite flake containing nanometer Fe particle is placed in ZrC precursor solutions and is impregnated 3 days, drying is taken out and impregnates again, it is so anti-
It is 3 times multiple, you can the ZrC presoma solid granulates of certain content are made on graphite flake surface.
Sample is loaded in the pipeline of corundum polycrystalline ceramics.Furnace chamber is vacuumized, opens argon gas valve later, is carried out
It rinses.3 times repeatedly.Whole process is passed through argon gas protection, and magnetic field is added on sample top in argon flow amount 200SCCM, and magnetic field is whole
It opens.Temperature is raised to 1500 DEG C, 7 DEG C/min of heating rate by start-up temperature time control program, keeps the temperature 3h, program cooling, drop
The warm time is 5h.Bolt down procedure is down to room temperature naturally, sampling.
Graphite in all implementation examples>99.99%, urea>99.9%, Fe (NO3)2·9H2O>98%, absolute ethyl alcohol and
Acetone (AR), CH4>99.9%, Ar>99.999%, H2>99.999%.
Claims (1)
1. a kind of method that 3D carbide nanometer linear arrays are prepared in situ with magnetic pulling method in polymer infiltration and pyrolysis, it is characterised in that step
It is rapid as follows：
Step 1, coprecipitation prepare nanometer Fe particle on graphite flake：By urea and Fe(NO3)39H2O and deionized water dissolving
In beaker, magnetic agitation 30-60min, after by solution move into equipped with graphite flake polytetrafluoroethylliner liner in, seal filling tank；
Reaction kettle is placed in baking oven, in 120-180 DEG C of constant temperature 1-3h；
The graphite flake drying in reaction kettle is taken out, is placed in horizontal type heat-treatment furnace, the temperature that hydrogen reducing is arranged is 500-700
DEG C, recovery time 1-3h, hydrogen is passed through simultaneously with argon gas, and the flow proportional of two kinds of gas is 2:1；
Temperature is down to room temperature taking-up, obtains a large amount of nanometer Fe particle and is attached on graphite flake surface；
The graphite flake, which is placed in alcohol, is cleaned by ultrasonic 30-60min；The molar ratio of the urea and Fe(NO3)39H2O is 3:2；
Step 2 prepares ZrC granular precursors on graphite flake：
Graphite flake containing nanometer Fe particle is placed in ZrC precursor solutions and is impregnated 1-3 days, drying is taken out and impregnates again, so
3 times repeatedly, i.e., ZrC presoma solid granulates are made on graphite flake surface；
The ZrC precursor solutions are：1-5g ZrC presoma solid particles are dissolved in acetone soln, magnetic agitation 2-5h systems
Obtain ZrC precursor solutions；
Step 3, magnetic draw standby ZrC nano-wire arrays：
The graphite flake that the surface that step 2 obtains is adhered to ZrC presoma solid granulates is loaded in the pipeline of corundum polycrystalline ceramics,
Furnace chamber is vacuumized, argon gas valve is opened later, is rinsed；3 times repeatedly；
Whole process is passed through argon gas protection again, and argon flow amount 50-200SCCM is added magnetic field on graphite flake top, generates the direct current in magnetic field
Voltage is 10-200V, electric current 1-3A, magnetic pull 5-1000N, and magnetic field whole process is opened；
Temperature is raised to 1300-1500 DEG C by start-up temperature time control program, and 6-7 DEG C of heating rate/min keeps the temperature 0.5-3h,
Program cools down, temperature fall time 3-5h；
Naturally it is down to room temperature, completes to prepare 3D carbide nanometer linear arrays.
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| CN201810853080.3A CN108751197B (en) | 2018-07-30 | 2018-07-30 | Method for preparing 3D carbide nanowire array in situ by precursor impregnation cracking and magnetic pulling method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111943678A (en) * | 2020-08-14 | 2020-11-17 | 西北工业大学 | HfxZr1-xC ceramic solid solution nanowire and preparation method thereof |
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| CN111943678A (en) * | 2020-08-14 | 2020-11-17 | 西北工业大学 | HfxZr1-xC ceramic solid solution nanowire and preparation method thereof |
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