CN107311685A - The preparation method of electrophoresis and thermal evaporation techniques fabricated in situ refractory carbide nano wire - Google Patents
The preparation method of electrophoresis and thermal evaporation techniques fabricated in situ refractory carbide nano wire Download PDFInfo
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- CN107311685A CN107311685A CN201710484348.6A CN201710484348A CN107311685A CN 107311685 A CN107311685 A CN 107311685A CN 201710484348 A CN201710484348 A CN 201710484348A CN 107311685 A CN107311685 A CN 107311685A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
- C04B2235/9684—Oxidation resistance
Abstract
The present invention relates to the preparation method of a kind of electrophoresis and thermal evaporation techniques fabricated in situ refractory carbide nano wire, belong to thermal evaporation+electrophoretic techniques and prepare application of the refractory carbide nano wire in technical field of composite materials.First with electrophoresis on carbon cloth deposition of carbon nanotubes;Refractory carbide nano wire is obtained in the carbon cloth surfaces containing CNT by electrophoretic techniques again.Preparation method of the present invention is simple, pollution-free and safety and stability, and the problem of refractory carbide nano wire prepares difficult, small draw ratio and skewness is largely solved, composite materials property, fracture toughness, anti-oxidation and anti-yaw damper ability and creep-resistant property can be effectively improved.It can be widely applied to simultaneously in carbon/carbon, carbon/pottery, magnesium-based, aluminum matrix composite and hard alloy, with good economic and social benefit.
Description
Technical field
The invention belongs to technical field of composite materials, it is related to a kind of electrophoresis and thermal evaporation techniques fabricated in situ refractory metal carbon
The preparation method of compound nano wire.
Background technology
Refractory carbide (XC) nano wire is the structural material of current high-technology field most application potential.By
In its superelevation fusing point, hardness and modulus, high temperature specific strength is excellent, and wear resistance preferably, the features such as extremely corrosion-resistant, is navigated in aviation
My god, military, medicine, building etc.-field is widely applied.But because carbide nanometer line fusing point is high, hardness is big, and chemistry is lazy
The problems such as property is strong, seriously limits carbide nanometer line further applying in engineering component.Although the method for synthesis is more,
But the defects such as the nano wire skewness due to synthesis seriously limit the further practical of such carbide nanometer line.With
Continuing to develop for high-tech area, it is desirable to which mutually enhancing composite element must be with preferable as second for carbide nanometer line
The performance such as fracture toughness, creep-resistant property, higher modulus, more excellent anticorrosive, high temperature resistant, anti-particle erosion it is special
Levy, therefore, research carbide nanometer line has to improving the performance such as composite creep resistant, anti-yaw damper, anti-oxidation, toughness reinforcing enhancing
Significance.
Thermal evaporation techniques are modified composite material vital technologies in engineer applied, including coating modified,
Modification of matrix modification and fibrous inner structure etc..Thermal evaporation techniques are that substrate or workpiece are placed in certain container, are passed through
Make its evaporation gasification to reaction raw materials heating and deposit and matrix or workpiece surface and the work for forming film or coating or nano wire
Skill process.Electrophoretic techniques (EP) be charged particle or nano wire etc. under electric field action, towards with its electrically opposite electrode move
Dynamic technology.Main purpose is that translational speed is different and reach the technology of separation in the electric field using charged particle.Pass through heat steaming
Hair+electrophoretic techniques prepares the nano material of refractory carbide in carbon fiber precast body, tough to improving fracture of composite materials
Property, creep-resistant property, oxidation proof propertiess and Burning corrosion resistance can play an important roll.
Shandong University zhaoguolong et al. uses carbothermic method by Ta2O5Mixed with carbon dust, and using Ni as catalyst,
NaCl is that sintering aid synthesizes TaC whiskers, and the TaC of synthesis is whisker rather than nano wire, and the serious uneven pattern of whisker can not
Control, xuliang et al. also uses carbothermic method by ZrO2ZrC whiskers are mixed to form with carbon dust.Same pattern is uncontrollable and divides
Cloth is uneven.If using thermal evaporation and electrophoretic techniques, can be very good to solve limitation carbide nanometer line as engineering component
Whisker size can be down to nano wire by actual applications the problem of, thermal evaporation techniques, and electrophoretic techniques can be by refractory metal
Carbide is evenly distributed in fiber preform.It is combined using electrophoresis with thermal evaporation techniques, it is possible to achieve in composite
Situ prepares high-melting-point refractory carbide nano wire, reaches raising composite isotropism, fracture toughness, creep resistant
The purpose of anti-oxidation and anti-yaw damper ability and matrix and reinforcement the bond strength of performance, superhigh temperature.
The content of the invention
The technical problem to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of electrophoresis and thermal evaporation techniques fabricated in situ infusibility
The preparation method of metal carbides nano wire, the invention preparation method is simple, pollution-free and safety and stability, can effectively improve multiple
Condensation material mechanical property, fracture toughness, anti-oxidation and anti-yaw damper ability and creep-resistant property.Simultaneously can be widely applied to carbon/carbon,
In carbon/pottery, magnesium-based, aluminum matrix composite and hard alloy, with good economic and social benefit.
Technical scheme
A kind of preparation method of electrophoresis and thermal evaporation techniques fabricated in situ refractory carbide nano wire, it is characterised in that
Step is as follows:
Step 1, pyrolytic carbon is deposited on carbon cloth:
Carbon cloth is put into graphite jig folder and is loaded in CVI stoves, argon gas valve is opened after being vacuumized to furnace chamber and is entered
Row is rinsed;Temperature is raised to 800-1100 DEG C, 4-5 DEG C of heating rate/min, the heating-up time is 2-4h, with 1500ml/min flows
It is passed through argon gas protection;When temperature reaches 800-1100 DEG C, natural air valve is opened, gas discharge 20-80L/h is set to, together
When Ar throughputs are set to 800-1600ml/min, deposit 0.5-5h;
Natural gas air valve and flowmeter are closed, argon flow amount is adjusted to 1500ml/min, power supply is closed, naturally cools to room
Temperature;Argon gas air valve is closed, completion deposits pyrolytic carbon on carbon cloth;
Step 2, electrophoresis the electrophoresis CNT on carbon cloth:The carbon cloth that step 1 is deposited into pyrolytic carbon is fixed on the negative pole of electrophoresis apparatus
On pole plate, it is placed in slurry;Electrode is correctly connected on electrophoresis apparatus, positive/negative plate is apart from 1cm;Electrophoresis time is
1-10min, power parameter is set to 10-300V, 0.01-10A, 1-300W;
Step 3, thermal evaporation are in precast body surface growth in situ refractory carbide nano wire:
Material after step 2 is handled hang on containing chloride metal graphite jig inner tip, then by stone
Black mould is fitted into high temperature sintering furnace, and argon gas valve is opened after being vacuumized to furnace chamber and is rinsed;Temperature is raised to 1500-
2100 DEG C, 4-7 DEG C of heating rate/min is incubated after 0.5-2h and is down to room temperature naturally, completes fabricated in situ refractory carbide
Nano wire;Argon gas protection is passed through with 70-100ml/min flows during thermal evaporation.
The chloride metal is TaCl5Or ZrCl4。
Beneficial effect
The preparation side of a kind of electrophoresis proposed by the present invention and thermal evaporation techniques fabricated in situ refractory carbide nano wire
Method, deposits one layer of carbon with isothermal chemical vapor infiltration (ICVI) method first on carbon cloth, fills up prefabricated carbon fiber body surface in carbon cloth
Planar defect;Secondly, carbon cloth is fixed on cathode plate, after be placed in electrophoresis 1- in the isopropanol slurry containing CNT
10min (voltage 10-300, electric current 0.01-10A, power 1-300W);The carbon cloth for containing CNT is hung on again and is equipped with
Chloride (TaCl5、ZrCl4) graphite jig inner tip position, afterwards by 1500-2100 DEG C heat treatment, you can be made hardly possible
Molten metal carbides nano wire.Such carbide nanometer line is evenly distributed on carbon cloth, in the absence of because locally reunite and caused by
Thermal stress concentration phenomenon.Meanwhile, electrophoresis and thermal evaporation process almost do not have to Carbon Fiber Damage, and this is for improving composite
Mechanical property has vital effect.Because carbide nanometer line adds the interface with matrix so that composite breaks
Split toughness raising.Carbide nanometer line has high-melting-point under high temperature, and high-temperature oxidation process absorbs more energy, and can have
Resist washing away for big air-flow particle in effect ground.Therefore the anti-oxidant of carbon/carbon compound material can be improved can Burning corrosion resistance energy.In magnesium
In base, aluminum matrix composite, carbide nanometer line can prevent crystal grain from growing up with crystal grain thinning.Therefore magnesium-based, aluminium are greatly improved
Intensity, toughness and the creep resisting ability of based composites.
Present invention incorporates the process advantage of distinct methods, largely solve refractory carbide nano wire and prepare
The problem of difficult, small draw ratio and skewness, anti-aging capability, anti-yaw damper for improving composite are fracture toughness, anti-
The bond strength of creep ability and matrix and reinforcement has certain progress meaning.Thermal evaporation techniques can drop whisker size
To nano wire, refractory carbide can be evenly distributed in fiber preform by electrophoretic techniques.Steamed using electrophoresis with heat
Hair technology is combined, it is possible to achieve original position prepares high-melting-point refractory carbide nano wire in the composite, reaches raising
Composite isotropism, fracture toughness, creep-resistant property, superhigh temperature be anti-oxidation and anti-yaw damper ability and matrix and reinforcement
Bond strength purpose.
Preparation method of the present invention is simple, pollution-free and safety and stability, can effectively improve composite materials property, fracture
Toughness, anti-oxidation, anti-yaw damper ability, the bond strength of creep-resistant property and matrix and reinforcement.It can be widely applied to simultaneously
In carbon/carbon, carbon/pottery, magnesium-based, aluminum matrix composite and hard alloy, with good economic and social benefit.
Brief description of the drawings
Fig. 1:Thermal evaporation prepares carbide nanometer line modified composite material process chart with electrophoretic techniques
Fig. 2:Electrophoretic techniques shows with the scanning electron that thermal evaporation techniques are combined the refractory carbide nano wire of acquisition
Micro- (SEM) figure;
(a) the SEM figures after carbon fiber surface electrophoresis;(b) the SEM figures after being heat-treated;
Fig. 3:The X ray diffracting spectrum (XRD) of TaC nano wires and ZrC nano wires;
(a) TaC nano wires XRD;(b) XRD of ZrC nano wires.
Embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described:
The raw material that the present invention is used has:Carbon cloth (T300,40 × 60mm), (phosphoric acid aluminium, CNT is different by slurry 50-5000ml
Propyl alcohol), TaCl5、ZrCl4.The present invention uses equipment:Electrophoresis equipment is a set of, ICVI stoves, high temperature sintering furnace.
Concrete operation step is as follows:
(1) pyrolytic carbon is deposited on carbon cloth
1. carbon cloth is put into graphite jig folder and is loaded in CVI stoves.Furnace chamber is vacuumized, argon gas is opened afterwards
Valve, is rinsed.So 3 times repeatedly.
2. start-up temperature time control program, 800-1100 DEG C, 4-5 DEG C of heating rate/min, during heating are raised to by temperature
Between be 2-4h, be passed through argon gas protection, argon flow amount 1500ml/min.
3. constant temperature stage.When temperature reaches 800-1100 DEG C, natural air valve is opened, gas discharge is set to 20-
80L/h, while Ar throughputs are set into 800-1600ml/min, deposits 0.5-5h.
4. natural gas air valve and flowmeter are closed, argon flow amount is adjusted to 1500ml/min, power supply is closed, naturally cools to
Room temperature;Argon gas air valve and flowmeter are closed, experiment terminates, sampled.
(2) electrophoresis electrophoresis CNT on carbon cloth
1. it is standby by the slurry ultrasound 1-2h containing CNT.
2. Electrode is correctly connected on electrophoresis apparatus;Power parameter is set to 10-300V, 0.01-10A, 1-
300W;Electrophoresis time is set to 1-10min.
3. by deposit pyrolytic carbon carbon cloth be fixed in the negative plates of electrophoresis apparatus, be placed in slurry, positive/negative plate away from
From 1cm, operation program terminates, and sampling drying is standby.
(3) thermal evaporation is in precast body surface growth in situ refractory carbide nano wire
Sample is carried out in ZGS-350 types high temperature sintering furnace (3000 DEG C).
1. sample is hung on and contains TaCl respectively5、ZrCl4Graphite jig inner tip position, then by graphite mo(u)ld
Tool is fitted into high temperature sintering furnace, and furnace chamber is vacuumized, and argon gas valve is opened afterwards, is rinsed.So 3 times repeatedly.
2. start-up temperature time control program, 1500-2100 DEG C, 4-7 DEG C of heating rate/min, insulation are raised to by temperature
0.5-2h, is passed through argon gas protection, argon flow amount 70-100ml/min.
3. bolt down procedure, is down to room temperature naturally, sampling.
Embodiment 1
Carbon cloth is put into graphite jig folder and is loaded in CVI stoves.Furnace chamber is vacuumized, argon gas is opened afterwards
Valve, is rinsed.So 3 times repeatedly;Start-up temperature time control program, 1100 DEG C are raised to by temperature, and 4-5 DEG C of heating rate/
Min, the heating-up time is 4h, is passed through argon gas protection, argon flow amount 1500ml/min;The constant temperature stage.When temperature reaches 1100 DEG C,
Natural air valve is opened, gas discharge is set to 80L/h, while Ar throughputs are set into 1600ml/min, 0.5-5h is deposited;Close
Natural gas air valve and flowmeter are closed, argon flow amount is adjusted to 1500ml/min, power supply is closed, naturally cools to room temperature;Close argon
Gas air valve and flowmeter, experiment terminate, sampling.
It is standby by the slurry ultrasound 1-2h containing CNT;Electrode is correctly connected on electrophoresis apparatus;Power supply is joined
Number is set to 40V, 0.02A, 1W;Electrophoresis time is set to 3min;The carbon cloth for depositing pyrolytic carbon is fixed on to the negative pole pole of electrophoresis apparatus
On plate, it is placed in slurry, positive/negative plate terminates apart from 1cm, operation program, and sampling drying is standby.
Sample is hung on and contains TaCl respectively5、ZrCl4Graphite jig inner tip position, then by graphite jig
It is fitted into high temperature sintering furnace, furnace chamber is vacuumized, argon gas valve is opened afterwards, is rinsed.So 3 times repeatedly.Start temperature
Time control program is spent, temperature 1500 DEG C is raised to, 4-7 DEG C of heating rate/min is incubated 0.5-2h, is passed through argon gas protection, argon
Throughput 70-100ml/min;Bolt down procedure, is down to room temperature naturally, sampling.
Embodiment 2
Carbon cloth is put into graphite jig folder and is loaded in CVI stoves.Furnace chamber is vacuumized, argon gas is opened afterwards
Valve, is rinsed.So 3 times repeatedly;Start-up temperature time control program, 1100 DEG C are raised to by temperature, and 4-5 DEG C of heating rate/
Min, the heating-up time is 4h, is passed through argon gas protection, argon flow amount 1500ml/min;The constant temperature stage.When temperature reaches 1100 DEG C,
Natural air valve is opened, gas discharge is set to 80L/h, while Ar throughputs are set into 1600ml/min, 0.5-5h is deposited;Close
Natural gas air valve and flowmeter are closed, argon flow amount is adjusted to 1500ml/min, power supply is closed, naturally cools to room temperature;Close argon
Gas air valve and flowmeter, experiment terminate, sampling.
It is standby by the slurry ultrasound 1-2h containing CNT;Electrode is correctly connected on electrophoresis apparatus;Power supply is joined
Number is set to 40V, 0.02A, 1W;Electrophoresis time is set to 3min;The carbon cloth for depositing pyrolytic carbon is fixed on to the negative pole pole of electrophoresis apparatus
On plate, it is placed in slurry, positive/negative plate terminates apart from 1cm, operation program, and sampling drying is standby.
Sample is hung on and contains TaCl respectively5、ZrCl4Graphite jig inner tip position, then by graphite jig
It is fitted into high temperature sintering furnace, furnace chamber is vacuumized, argon gas valve is opened afterwards, is rinsed.So 3 times repeatedly.Start temperature
Time control program is spent, temperature 1600 DEG C is raised to, 4-7 DEG C of heating rate/min is incubated 0.5-2h, is passed through argon gas protection, argon
Throughput 70-100ml/min;Bolt down procedure, is down to room temperature naturally, sampling.
Claims (2)
1. a kind of preparation method of electrophoresis and thermal evaporation techniques fabricated in situ refractory carbide nano wire, it is characterised in that step
It is rapid as follows:
Step 1, pyrolytic carbon is deposited on carbon cloth:
Carbon cloth is put into graphite jig folder and is loaded in CVI stoves, argon gas valve is opened after being vacuumized to furnace chamber and is rushed
Wash;Temperature is raised to 800-1100 DEG C, 4-5 DEG C of heating rate/min, the heating-up time is 2-4h, is passed through with 1500ml/min flows
Argon gas is protected;When temperature reaches 800-1100 DEG C, natural air valve is opened, gas discharge is set to 20-80L/h, simultaneously will
Ar throughputs are set to 800-1600ml/min, deposit 0.5-5h;
Natural gas air valve and flowmeter are closed, argon flow amount is adjusted to 1500ml/min, power supply is closed, naturally cools to room temperature;
Argon gas air valve is closed, completion deposits pyrolytic carbon on carbon cloth;
Step 2, electrophoresis the electrophoresis CNT on carbon cloth:The carbon cloth that step 1 is deposited into pyrolytic carbon is fixed on the negative plates of electrophoresis apparatus
On, it is placed in slurry;Electrode is correctly connected on electrophoresis apparatus, positive/negative plate is apart from 1cm;Electrophoresis time is 1-
10min, power parameter is set to 10-300V, 0.01-10A, 1-300W;
Step 3, thermal evaporation are in precast body surface growth in situ refractory carbide nano wire:
Material after step 2 is handled hang on containing chloride metal graphite jig inner tip, then by graphite mo(u)ld
Tool is fitted into high temperature sintering furnace, and argon gas valve is opened after being vacuumized to furnace chamber and is rinsed;Temperature is raised to 1500-2100
DEG C, 4-7 DEG C of heating rate/min is incubated after 0.5-2h and is down to room temperature naturally, completes fabricated in situ refractory carbide nanometer
Line;Argon gas protection is passed through with 70-100ml/min flows during thermal evaporation.
2. the preparation side of electrophoresis and thermal evaporation techniques fabricated in situ refractory carbide nano wire according to claim 1
Method, it is characterised in that:The chloride metal is TaCl5Or ZrCl4。
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Cited By (3)
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CN109133060A (en) * | 2018-10-25 | 2019-01-04 | 西北工业大学 | Refractory carbide nano wire/pipe device and method is prepared in situ in template and thermal evaporation techniques |
CN111455430A (en) * | 2020-04-21 | 2020-07-28 | 西北工业大学 | In-situ synthesis of radial Mg (OH) on surface of Mg-based composite material2Method of threading |
CN113072071A (en) * | 2021-04-14 | 2021-07-06 | 西北工业大学 | Preparation method of electrophoretic carbon nano tube and zero-catalysis in-situ synthesis HfC nano wire by thermal evaporation technology |
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CN109133060A (en) * | 2018-10-25 | 2019-01-04 | 西北工业大学 | Refractory carbide nano wire/pipe device and method is prepared in situ in template and thermal evaporation techniques |
CN111455430A (en) * | 2020-04-21 | 2020-07-28 | 西北工业大学 | In-situ synthesis of radial Mg (OH) on surface of Mg-based composite material2Method of threading |
CN111455430B (en) * | 2020-04-21 | 2022-05-13 | 西北工业大学 | In-situ synthesis of radial Mg (OH) on surface of Mg-based composite material2Method of threading |
CN113072071A (en) * | 2021-04-14 | 2021-07-06 | 西北工业大学 | Preparation method of electrophoretic carbon nano tube and zero-catalysis in-situ synthesis HfC nano wire by thermal evaporation technology |
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