CN107311685B - Preparation method for in-situ synthesis of refractory metal carbide nanowires by electrophoresis and thermal evaporation technology - Google Patents

Preparation method for in-situ synthesis of refractory metal carbide nanowires by electrophoresis and thermal evaporation technology Download PDF

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CN107311685B
CN107311685B CN201710484348.6A CN201710484348A CN107311685B CN 107311685 B CN107311685 B CN 107311685B CN 201710484348 A CN201710484348 A CN 201710484348A CN 107311685 B CN107311685 B CN 107311685B
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electrophoresis
carbon
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refractory metal
metal carbide
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史小红
闫宁宁
李戌一
李贺军
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Northwestern Polytechnical University
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
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Abstract

The invention relates to a preparation method for in-situ synthesis of a refractory metal carbide nanowire by electrophoresis and thermal evaporation technologies, and belongs to application of the refractory metal carbide nanowire prepared by the thermal evaporation and electrophoresis technologies in the technical field of composite materials. Firstly, depositing carbon nano tubes on carbon cloth by using an electrophoresis method; then obtaining the refractory metal carbide nano-wire on the surface of the carbon cloth containing the carbon nano-tube by an electrophoresis technology. The preparation method is simple, pollution-free, safe and stable, solves the problems of difficult preparation, small length-diameter ratio and uneven distribution of the refractory metal carbide nanowires to a great extent, and can effectively improve the mechanical property, fracture toughness, oxidation resistance, ablation resistance and creep resistance of the composite material. Meanwhile, the composite material can be widely applied to carbon/carbon, carbon/ceramic, magnesium-based and aluminum-based composite materials and hard alloys, and has good economic and social benefits.

Description

Preparation method for in-situ synthesis of refractory metal carbide nanowires by electrophoresis and thermal evaporation technology
Technical Field
The invention belongs to the technical field of composite materials, and relates to a preparation method for in-situ synthesis of a refractory metal carbide nanowire by electrophoresis and thermal evaporation technologies.
Background
Refractory metal carbide (XC) nanowires are the most potential structural materials in the high and new technical field at present. Due to the characteristics of ultrahigh melting point, hardness and modulus, excellent high-temperature specific strength, better abrasion resistance, extremely corrosion resistance and the like, the high-temperature wear-resistant steel is widely applied to the fields of aerospace, military, medicine, building and the like. However, due to the problems of high melting point, high hardness, strong chemical inertness and the like of the carbide nanowires, the further application of the carbide nanowires in engineering components is severely limited. Although the synthesis method is more, the further practical application of the carbide nano-wires is severely limited due to the defects of uneven distribution of the synthesized nano-wires and the like. With the continuous development of the high-tech field, the carbide nanowires are required to have better fracture toughness, creep resistance, higher modulus, more excellent corrosion resistance, high temperature resistance, particle erosion resistance and other performance characteristics as a second phase reinforced composite material component, so that the research on the carbide nanowires has important significance for improving the creep resistance, ablation resistance, oxidation resistance, toughening and reinforcing performances of the composite material.
The thermal evaporation technology is a technology which is crucial to the engineering application of the modified composite material, and comprises the modification of a coating, the modification of a matrix, the modification of the internal structure of a fiber and the like. The thermal evaporation technology is a process in which a substrate or a workpiece is placed in a certain container, and a reaction raw material is heated to be evaporated and gasified to deposit on the surface of a substrate or the workpiece and form a film or a coating or a nanowire. The Electrophoresis (EP) technique is a technique in which charged particles, nanowires, or the like move toward an electrode of an opposite electric polarity to the charged particles or nanowires under the action of an electric field. The main purpose is to utilize the different moving speed of charged particles in the electric field to achieve the separation technology. The nanometer material of the refractory metal carbide is prepared on the carbon fiber preform by the thermal evaporation and electrophoresis technology, and has important effects on improving the fracture toughness, creep resistance, oxidation resistance and ablation resistance of the composite material.
Zhundong university zhaoguolong et al carbothermic reduction of Ta2O5Mixing with carbon powder, using Ni as catalyst and NaCl as sintering aid to synthesize TaC whisker, in which the synthesized TaC is whisker rather than nanowire, and the whisker is seriously uneven and uncontrollable in shape, and xuliang et al also adopt carbothermic reduction method to make ZrO from ZrO2And mixing with carbon powder to form ZrC crystal whisker. Also the morphology is not controllable and the distribution is not uniform. If thermal evaporation and electrophoresis technology are adopted, the problem of limiting the carbide nanowires to be used as engineering components in practical application can be well solved, the size of the whiskers can be reduced to the nanowires through the thermal evaporation technology, and refractory metal carbides can be uniformly distributed in the fiber preform through the electrophoresis technology. By combining the electrophoresis method with the thermal evaporation technology, the high-melting-point refractory metal carbide nanowires can be prepared in situ in the composite material, and the purposes of improving the isotropy, the fracture toughness, the creep resistance, the ultrahigh-temperature oxidation resistance, the ablation resistance and the bonding strength of the matrix and the reinforcement are achieved.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a preparation method for in-situ synthesis of refractory metal carbide nanowires by using electrophoresis and thermal evaporation technologies, which is simple, pollution-free, safe and stable, and can effectively improve the mechanical property, the fracture toughness, the oxidation resistance, the ablation resistance and the creep resistance of a composite material. Meanwhile, the composite material can be widely applied to carbon/carbon, carbon/ceramic, magnesium-based and aluminum-based composite materials and hard alloys, and has good economic and social benefits.
Technical scheme
A preparation method for in-situ synthesis of refractory metal carbide nanowires by electrophoresis and thermal evaporation technology is characterized by comprising the following steps:
step 1, depositing pyrolytic carbon on carbon cloth:
placing the carbon cloth into a graphite mold clamp, filling the graphite mold clamp into a CVI furnace, vacuumizing the furnace chamber, and opening an argon valve for flushing; raising the temperature to 800-1100 ℃, raising the temperature at the rate of 4-5 ℃/min for 2-4h, and introducing argon at the flow rate of 1500ml/min for protection; when the temperature reaches 800-;
closing the natural gas valve and the flowmeter, adjusting the flow of the argon gas to 1500ml/min, closing a power supply, and naturally cooling to room temperature; closing the argon gas valve to finish depositing pyrolytic carbon on the carbon cloth;
and 2, electrophoresis of CNT on the carbon cloth by an electrophoresis method: fixing the carbon cloth deposited with pyrolytic carbon in the step 1 on a negative electrode plate of an electrophoresis apparatus, and placing the carbon cloth in slurry; correctly connecting the electric field polar plates to an electrophoresis apparatus, wherein the distance between the positive polar plate and the negative polar plate is 1 cm; the electrophoresis time is 1-10min, and the power supply parameters are set to 10-300V, 0.01-10A and 1-300W;
step 3, growing refractory metal carbide nanowires on the surface of the preform in situ by a thermal evaporation method:
suspending the material treated in the step 2 at the top end of the interior of a graphite mold containing chloride metal, then loading the graphite mold into a high-temperature sintering furnace, vacuumizing the furnace chamber, and opening an argon valve for washing; raising the temperature to 1500-; argon is introduced at the flow rate of 70-100ml/min for protection in the process of the thermal evaporation method.
The chloride metal is TaCl5Or ZrCl4。
Advantageous effects
The invention provides a preparation method for in-situ synthesis of refractory metal carbide nanowires by electrophoresis and thermal evaporation technologies, which comprises the steps of firstly depositing a layer of carbon on carbon cloth by an Isothermal Chemical Vapor Infiltration (ICVI) method to fill up the surface defects of carbon fiber preforms in the carbon cloth; secondly, fixing the carbon cloth on a cathode plate, and then placing the carbon cloth in isopropanol slurry containing the carbon nano tubes for electrophoresis for 1-10min (voltage is 10-300, current is 0.01-10A, and power is 1-300W); then the carbon cloth containing the carbon nano tube is hung on a container filled with chloride (TaCl)5、ZrCl4) And then carrying out heat treatment at 1500-2100 ℃ to obtain the refractory metal carbide nanowire. The carbide nanowires are uniformly distributed on the carbon cloth, and the phenomenon of thermal stress concentration caused by local agglomeration does not exist. Meanwhile, the electrophoresis and thermal evaporation processes hardly damage the carbon fibers, which plays a vital role in improving the mechanical property of the composite material. The carbide nanowires increase the interface with the matrix, so that the fracture toughness of the composite material is improved. The carbide nanowires have high melting points at high temperature, absorb more energy in the high-temperature oxidation process, and can effectively resist the washing of atmospheric flow particles. Therefore, the oxidation resistance and ablation resistance of the carbon/carbon composite material can be improved. In the magnesium-based and aluminum-based composite material, the carbide nanowires can refine grains and prevent the grains from growing. Therefore, the strength, toughness and creep resistance of the magnesium-based and aluminum-based composite material can be greatly improved.
The invention combines the process advantages of different methods, solves the problems of difficult preparation, small length-diameter ratio and uneven distribution of the refractory metal carbide nanowires to a great extent, and has certain improvement significance for improving the oxidation resistance, ablation resistance, fracture toughness and creep resistance of the composite material and the bonding strength of the matrix and the reinforcement. Thermal evaporation techniques can reduce the whisker size to nanowires, and electrophoretic techniques can uniformly distribute refractory metal carbides in the fiber preform. By combining the electrophoresis method with the thermal evaporation technology, the high-melting-point refractory metal carbide nanowires can be prepared in situ in the composite material, and the purposes of improving the isotropy, the fracture toughness, the creep resistance, the ultrahigh-temperature oxidation resistance, the ablation resistance and the bonding strength of the matrix and the reinforcement are achieved.
The preparation method is simple, pollution-free, safe and stable, and can effectively improve the mechanical property, the fracture toughness, the oxidation resistance, the ablation resistance and the creep resistance of the composite material and the bonding strength of the matrix and the reinforcement. Meanwhile, the composite material can be widely applied to carbon/carbon, carbon/ceramic, magnesium-based and aluminum-based composite materials and hard alloys, and has good economic and social benefits.
Drawings
FIG. 1: technological process chart for preparing carbide nanowire modified composite material by thermal evaporation and electrophoresis technology
FIG. 2: scanning Electron Microscopy (SEM) images of refractory metal carbide nanowires obtained by combining electrophoresis and thermal evaporation techniques;
(a) SEM picture after carbon fiber surface electrophoresis; (b) SEM images after heat treatment;
FIG. 3: x-ray diffraction patterns (XRD) of the TaC nanowire and the ZrC nanowire;
(a) a TaC nanowire XRD pattern; (b) XRD pattern of ZrC nanowire.
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: carbon cloth (T300,40 x 60mm), slurry 50-5000ml (aluminum phosphate, CNT, isopropanol), TaCl5、ZrCl4. The invention uses equipment: the electrophoresis equipment comprises a set of electrophoresis equipment, an ICVI furnace and a high-temperature sintering furnace.
The specific operation steps are as follows:
(1) deposition of pyrolytic carbon on carbon cloth
① the carbon cloth was placed in a graphite mold holder and charged in a CVI furnace, the furnace chamber was evacuated, then the argon valve was opened and the rinse was performed, and so on for 3 times.
② starting temperature and time control program, raising the temperature to 800-1100 deg.C, raising the temperature rate at 4-5 deg.C/min for 2-4h, introducing argon gas for protection, and making the argon gas flow at 1500 ml/min.
③ constant temperature stage, when the temperature reaches 800-1100 ℃, open the natural gas valve, set the natural gas flow at 20-80L/h, and set the Ar gas flow at 800-1600ml/min, deposit for 0.5-5 h.
④ closing the natural gas valve and flowmeter, regulating the flow of argon to 1500ml/min, turning off the power supply, naturally cooling to room temperature, closing the natural gas valve and flowmeter, ending the experiment, and sampling.
(2) Electrophoresis method for electrophoresis of CNT on carbon cloth
① the slurry containing CNT is sonicated for 1-2h and is ready for use.
② connecting the electric field plates to the electrophoresis apparatus correctly, setting the power supply parameters to 10-300V, 0.01-10A, 1-300W, and setting the electrophoresis time to 1-10 min.
③ fixing the carbon cloth on the negative plate of the electrophoresis apparatus, placing in the slurry with the positive and negative plates at a distance of 1cm, running the program, ending, sampling, and oven drying.
(3) In-situ growth of refractory metal carbide nano-wire on the surface of prefabricated body by thermal evaporation method
The samples were run in a ZGS-350 type high temperature sintering furnace (3000 ℃ C.).
① the samples were suspended in TaCl-containing solutions5、ZrCl4Then the graphite mold is put into a high-temperature sintering furnace, the furnace chamber is vacuumized, and then an argon valve is opened for washing. This was repeated 3 times.
② starting temperature and time control program, increasing the temperature to 1500-.
③ the procedure was closed, cooled naturally to room temperature and sampled.
Example 1
The carbon cloth was placed in a graphite mold clamp and charged in a CVI furnace. And vacuumizing the furnace chamber, and then opening an argon valve for flushing. Repeating the steps for 3 times; starting a temperature time control program, raising the temperature to 1100 ℃, raising the temperature rate to 4-5 ℃/min, raising the temperature for 4h, introducing argon for protection, and leading the flow of the argon to be 1500 ml/min; and (5) a constant temperature stage. When the temperature reaches 1100 ℃, opening a natural gas valve, setting the flow of natural gas as 80L/h, setting the flow of Ar as 1600ml/min, and depositing for 0.5-5 h; closing the natural gas valve and the flowmeter, adjusting the flow of the argon gas to 1500ml/min, closing a power supply, and naturally cooling to room temperature; and (5) closing the argon gas valve and the flow meter, finishing the experiment and sampling.
Carrying out ultrasonic treatment on the slurry containing the CNT for 1-2h for later use; correctly connecting the electric field polar plate to the electrophoresis apparatus; setting power supply parameters to 40V, 0.02A, 1W; setting the electrophoresis time to be 3 min; fixing the carbon cloth deposited with pyrolytic carbon on a negative electrode plate of an electrophoresis apparatus, placing the carbon cloth in slurry, operating the program when the distance between the positive electrode plate and the negative electrode plate is 1cm, and sampling and drying the carbon cloth for later use.
Suspending the samples in TaCl-containing solutions5、ZrCl4Then the graphite mold is put into a high-temperature sintering furnace, the furnace chamber is vacuumized, and then an argon valve is opened for washing. This was repeated 3 times. Starting a temperature time control program, raising the temperature to 1500 ℃, keeping the temperature at the rate of 4-7 ℃/min for 0.5-2h, introducing argon for protection, and ensuring that the flow of the argon is 70-100 ml/min; the program is closed, the temperature is naturally reduced to the room temperature, and the sample is taken.
Example 2
The carbon cloth was placed in a graphite mold clamp and charged in a CVI furnace. And vacuumizing the furnace chamber, and then opening an argon valve for flushing. Repeating the steps for 3 times; starting a temperature time control program, raising the temperature to 1100 ℃, raising the temperature rate to 4-5 ℃/min, raising the temperature for 4h, introducing argon for protection, and leading the flow of the argon to be 1500 ml/min; and (5) a constant temperature stage. When the temperature reaches 1100 ℃, opening a natural gas valve, setting the flow of natural gas as 80L/h, setting the flow of Ar as 1600ml/min, and depositing for 0.5-5 h; closing the natural gas valve and the flowmeter, adjusting the flow of the argon gas to 1500ml/min, closing a power supply, and naturally cooling to room temperature; and (5) closing the argon gas valve and the flow meter, finishing the experiment and sampling.
Carrying out ultrasonic treatment on the slurry containing the CNT for 1-2h for later use; correctly connecting the electric field polar plate to the electrophoresis apparatus; setting power supply parameters to 40V, 0.02A, 1W; setting the electrophoresis time to be 3 min; fixing the carbon cloth deposited with pyrolytic carbon on a negative electrode plate of an electrophoresis apparatus, placing the carbon cloth in slurry, operating the program when the distance between the positive electrode plate and the negative electrode plate is 1cm, and sampling and drying the carbon cloth for later use.
Suspending the samples in TaCl-containing solutions5、ZrCl4Then the graphite mold is put into a high-temperature sintering furnace, the furnace chamber is vacuumized, and then an argon valve is opened for washing. This was repeated 3 times. Starting a temperature time control program, raising the temperature to 1600 ℃, keeping the temperature at the rate of 4-7 ℃/min for 0.5-2h, introducing argon for protection, and ensuring that the flow of the argon is 70-100 ml/min; the program is closed, the temperature is naturally reduced to the room temperature, and the sample is taken.

Claims (1)

1. A preparation method for in-situ synthesis of refractory metal carbide nanowires by electrophoresis and thermal evaporation technology is characterized by comprising the following steps:
step 1, depositing pyrolytic carbon on carbon cloth:
placing the carbon cloth into a graphite mold clamp, filling the graphite mold clamp into a CVI furnace, vacuumizing the furnace chamber, and opening an argon valve for flushing; raising the temperature to 800-1100 ℃, raising the temperature at the rate of 4-5 ℃/min for 2-4h, and introducing argon at the flow rate of 1500ml/min for protection; when the temperature reaches 800-;
closing the natural gas valve and the flowmeter, adjusting the flow of the argon gas to 1500ml/min, closing a power supply, and naturally cooling to room temperature; closing the argon gas valve to finish depositing pyrolytic carbon on the carbon cloth;
and 2, electrophoresis of CNT on the carbon cloth by an electrophoresis method: fixing the carbon cloth deposited with pyrolytic carbon in the step 1 on a negative electrode plate of an electrophoresis apparatus, and placing the carbon cloth in slurry; correctly connecting the electric field polar plates to an electrophoresis apparatus, wherein the distance between the positive polar plate and the negative polar plate is 1 cm; the electrophoresis time is 1-10min, and the power supply parameters are set to 10-300V, 0.01-10A and 1-300W;
step 3, growing refractory metal carbide nanowires on the surface of the preform in situ by a thermal evaporation method:
suspending the material treated in the step 2 at the top end of the interior of a graphite mold containing chloride metal, then loading the graphite mold into a high-temperature sintering furnace, vacuumizing the furnace chamber, and opening an argon valve for washing; raising the temperature to 1500-; introducing argon at a flow rate of 70-100ml/min for protection in the process of the thermal evaporation method;
the chloride metal is TaCl5Or ZrCl4。
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CN103061112A (en) * 2012-12-05 2013-04-24 天津大学 Composite material of silicon carbide and carbon nanotube and preparation method thereof
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CN103061112A (en) * 2012-12-05 2013-04-24 天津大学 Composite material of silicon carbide and carbon nanotube and preparation method thereof
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