CN107740266B - Continuous SiC fiber surface in situ C-SiO2Preparation method of composite coating - Google Patents
Continuous SiC fiber surface in situ C-SiO2Preparation method of composite coating Download PDFInfo
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
Abstract
Continuous SiC fiber surface in situ C-SiO2Preparation method of composite coating is related to continuous SiC fiber.SiC fiber is placed in Muffle furnace, is heated up under air atmosphere, then in air atmosphere with being furnace-cooled to room temperature, the SiC fiber samples A after obtaining degumming；SiC fiber samples A after degumming is placed in porous graphite boat, is placed in heating tube furnace, inert atmosphere of ventilating at room temperature drains the air in tube furnace；After SiC fiber samples A after obtained degumming is heated up under inert atmosphere protection, N is turned off2Air valve opens Cl2Air valve, adjustment chlorine flowrate heat preservation, by modulation process, i.e., in SiC fiber surface in-situ preparation C-SiO2Composite coating closes Cl after heat preservation2Gas cools to room temperature with the furnace under inert atmosphere protection to get continuous SiC fiber surface in situ C-SiO2Composite coating.
Description
Technical field
The present invention relates to continuous SiC fibers, more particularly, to a kind of continuous SiC fiber surface that can be used for electro-magnetic wave absorption
C-SiO in situ2Preparation method of composite coating.
Background technique
The development of electronic information technology is also right so that the demand of civilian anti-radiation technology and military stealth technology increasingly increases
Absorbing material proposes urgent need (D.D.L.Chung.Electromagnetic interference shielding
effectiveness of carbon materials[J].Carbon.2001,39:279-285).Absorbing material is by molding work
Skill can be divided into coating-type and structural type.Coating-type material has the shortcomings that weight greatly and is easy to fall off, and structural absorbing mater ials
Advantage (preparation of Mu Wu high temperature resistant microwave absorbing coating and its Changsha performance study [D]: national defence section for inhaling wave and carrying can be had both
Skill university, 2004).Wherein, continuous fiber reinforced composite materials are a kind of high performance structures absorbing materials developed in recent years.First
The continuous SiC fiber for driving body conversion preparation has outstanding advantages (the Yajima S, Hayashi such as high intensity, high temperature resistant, low-density
J,Omori M,etal.Development of a silicon carbide fibre with high tensile
Strength [J] .Nature.1976,261:683-685), pass through high-temperature process (Brennan JJ.Fiber reinforced
Glass and glass-ceramics composites [J] .J Mater Sci Lett, 1996,30:240), doping it is heterogeneous
Element (Chen X.J.IronNanoparticle-Containing Silicon Carbide fibers prepared by
pyroolysis of Fe(CO)5-Doped polycarbosilane fibers[J].J.Am.Ceram.Soc.2010,93
(1): 89-95) or surface applies metallisation (Yang H J, Yuan J, Li Y, et al.Silicon
carbidepowders:Temperature-dependent dielectric properties and enhanced
microwave absorption at gigahertz range[J].Solid State Communications.2013,
The methods of 163:1-6), the adjusting to SiC fiber dielectric properties or magnetic property may be implemented, it is made to generate radar-wave absorbing effect.
But high-temperature process can significantly reduce the mechanical property of fiber；And for heterogeneous element doping, receive fiber preparation process
Limitation, element doping amount is limited (generally below 3%), thus very limited to the effect of electromagnetic performance.It is benefit that surface, which applies metallisation,
With physical deposition or the method for chemical plating, the magnetic metal coating such as iron, cobalt, nickel is applied in fiber surface, makes fiber that there is magnetic loss
Consume energy power.But metal coating has that density is big, Yi Cong SiC fiber surface falls off etc. and is difficult to overcome, and limits this side
The application of method.
Chemical vapor deposition (CVD) technology is also the effective ways for preparing SiC fiber surface coating, common sedimentation products
It is (SinghRN, BrunMK.Effect of boron nitride coating the on fiber- such as pyrolytic carbon, boron nitride
matrix interactions[J].Ceram.Eng Sci Proc.1987,8(7-8):636-643)、(Saeki A,
Takeda M,Yokoyama A, Yoshida T.Properties of CVD BN-coated Hi-Nicalon fiber
Reinforced SiC/SiC composite [J] .Ceram Eng Sci Proc.2000,21:363-370), these coatings
Main function be boundary layer as SiC fiber and ceramic matric composite, play the role of transmitting load and deflect crackle.
For the angle of electromagnetic absorption, BN is transparent to electromagnetic wave, therefore the BN coating of surface of SiC can make electromagnetic wave penetrate coating, into
Enter fiber.In the process, BN coating can play the role of impedance matching, potentially contribute to the absorption of electromagnetic wave (assuming that ceramics
Based composites matrix is wave transparent) (Fang Ye, et al.The improvement of wave-absorbing
ability of silicon carbide fibers by depositing boron nitride coating[J]
.Applied Surface Science.2013,20:611-616).But the absorbing property of material still depends primarily on painting at this time
SiC fiber inside layer；And for CVD pyrolytic carbon, due to carbon-coating compact structure, conductivity is higher, therefore, continuously
CVD carbon layer mainly plays reflex to electromagnetic wave.However, the carbon structure of dispersion but can have excellent absorbing property, than
Such as carbon black, chopped carbon fiber carbon material are mixed with electromagnetic wave transparent materials such as resins according to certain volume, carbon particle or chopped strand
Between the dipole that is discontinuously formed, wave-absorbing effect (Cao M S, Song W L, Hou Z is generated by way of " polarization loss "
L,et al.The effects of temperature and frequency on the dielectric
properties,electromagnetic interference shielding and microwave-absorption of
short carbon fiber/silica composites[J].Carbon. 2010,48(3):788-796)；H.M.Kou,
Y.Zhu,M.X.Chen,et al.Micro-wave absorbing performance of silica matrix
composites reinforced by carbon nanotubes and carbon fiber[J].Int.J.Appl.
Ceram.Technol.2012,10(2):245-250).In addition, controlling its pore-size by the way that carbon is prepared as porous structure
And shape, can also regulate and control carbon material electric conductivity (Guang Li, Tianshi Xie, Shenglin Yang et,
al.Microwave Absorption Enhancement of Porous Carbon Fibers Compared with
Carbon Nanofibers [J] .J.Phys. Chem.C 2012,116:9196-9201), and then it may be made to have electromagnetism
Ability is lost in wave.Therefore, if carbon structure that can be controllable in SiC fiber surface formation structure or component, may be such that SiC fiber has
Absorbing property.
Carbide-derived carbon (carbide-derived-carbon, CDC) technology is a kind of to be converted in situ into carbide
The advanced method of porous carbon structure.(Gogotsi YG,Jeon I-D,McNallan MJ.Carbon coatings on
silicon carbide by reaction with chlorine-containing gases.J Mater Chem 1997,
7 (9): 1841-1848) in gas storage (Mauricio RB, Jun SB, et al.Heat treatment-induced
structural changes in SiC-derived carbon and their impact on gas storage
Potential [J] .Phys.Chem.C 2010,114:16562-16575), supercapacitor (Yair Korenblit,
Marcus Rose,Emanuel Kockrick,et al.High-rate electrochemical capacitors based
on ordered mesoporous silicon carbide-derived carbon[J].American Chemical
Society.2010,4 (3): 1337-1344), friction coatings (Carroll B, Gogotsi Y, Kovalchenko A, et
al.Effect of humidity on the tribological properties of carbidr-derived-
Carbon (CDC) films on silicon carbide [J] .Tribology Letters.2003,15 (1): 51-55) etc.
Various fields extensive application prospect.CDC mainly includes halogen etching method (Gogotsi YG, Yoshimura
M.Formation of carbon filmsoncarbides under hydrothermal conditions.Nature.
1994；367:628-685.) thermal decomposition method (Lijima S, Graphitization of silicon carbide due to
Electron beam irradiation [J] .Solid State Chemistry.1982,42 (1): 101-105) and hydro-thermal
Method (Gogotsi Y G, Welz S. Formation of carbon coatings on SiC fibers by
selective etching in halogens and supercritical water[J].Ceramic Engineering
And Science Proceedings, 1998,19 (3): 87-94) etc..In contrast, halogen etching method has condition relatively warm
With react easy to control, uniform coating thickness, by-product is the features such as gas is easily drained, reactant is with high purity.Wherein, chlorination
Method is to prepare the most simple and practical method of CDC.Other than it can form porous carbon structure, CDC method also has carbon-coating institutional framework
The feature of multiplicity, it is nearly all by the available fullerene of factors, carbon nanotube, the ball-type graphite such as control process conditions etc.
Know carbon structure (Dash R, Yushin G, Gogotsi Y.Synthesis, Structure and Porosity Analysis
of Microporous and Mesoporous Carbon Derived from Zirconium Carbide[J].
Mcroporous and Mesoporous Materials.2005,86:50-57)。Yury.Gogotsi(Y.G.Gogotsi,
S.Welz,J. Daghfal,et,al.Formation of carbon coatings on SiC fibers by
selective etching in halogens and supercritical water[J].American Ceramic
Society.1998,19 (3): 97-94) near stoichiometric proportion that first prepares CDC technical application in polymer pyrolysis contains
On the SiC fiber (Tyranno SA) of Al, research is pointed out, which forms the structure of pure carbon, carbon-coating after surface chlorination
It is suitable as ceramic matric composite boundary layer.Marcus Rose(Rose M,Kockrick E,et,al.High surface
area carbide-derived carbon fibers produced by electrospinning of
Polycarbosilane precursors [J] .Carbon.2010,48:403-407) etc. have studied Polycarbosilane through Static Spinning
Silk obtains the CDC research of SiC nanofiber, mainly discusses preparation condition and the control of CDC porosity and specific surface area is made
With.
Above-mentioned SiC fiber is near-stoichiometric type SiC fiber, and prepared CDC coating is substantially pure carbon
Coating, application target are as porous adsorbing material or composite material interface.So far, there is not yet being directed to hyperoxia type
C-SiO is prepared in situ in SiC fiber2The research report of composite coating, also have no discuss coated conductive, dielectric properties regulation and its
Inhaling a possibility that wave direction is applied.
Summary of the invention
The object of the present invention is to provide simple processes, the company of preparation temperature continuous production that is low, at low cost, being suitble to fiber
Continuous SiC fiber surface original position C-SiO2Preparation method of composite coating.
The present invention the following steps are included:
1) SiC fiber is placed in Muffle furnace, heated up under air atmosphere, then obtained in air atmosphere with room temperature is furnace-cooled to
SiC fiber samples A after obtaining degumming；
In step 1), the heating can be warming up to 450~550 DEG C with the heating rate of 1~3 DEG C/min, then keep the temperature 10
~30min；The rich oxygen type continuous SiC fiber using PCS through oxidation cross-linked preparation can be used in the SiC fiber, or using utilization
Other are modified the rich oxygen type SiC fiber of polycarbosilane precusor preparation, and fiber oxygen content is higher than 7wt.%, average diameter 10~
15 μm, resistivity is higher than 104Ω·cm。
2) the SiC fiber samples A after degumming that step 1) obtains is placed in porous graphite boat, is placed on heating tubular type
In furnace, inert atmosphere of ventilating at room temperature drains the air in tube furnace；
In step 2), the time of the inert atmosphere of ventilating at room temperature can be 30min or more, and the inert atmosphere can be
Argon gas or nitrogen.
3) after the SiC fiber samples A after the degumming for obtaining step 1) heats up under inert atmosphere protection, N is turned off2
Air valve opens Cl2Air valve, adjustment chlorine flowrate heat preservation, by modulation process, i.e., in SiC fiber surface in-situ preparation
C-SiO2Composite coating closes Cl after heat preservation2Gas cools to room temperature with the furnace under inert atmosphere protection to get continuous SiC fiber
Surface in situ C-SiO2Composite coating.
In step 3), the condition of the heating can be warming up to 500~800 DEG C with the heating rate of 3~5 DEG C/min；Institute
Stating adjustment chlorine flowrate can be 50~100ml/min, and the time of heat preservation can be 5~60min, and in the process, SiC fiber will be sent out
Raw following chemical reaction:
SiC(s)+2Cl2(g)=C (s)+SiCl4(g) (1)
SiCxOy(s)+2Cl2(g)=(x-y) C (s)+SiCl4(g)+yCO(g) (2)
Wherein, SiCxOyRefer mainly to various metastable phases containing Si (including the SiC in hyperoxia type continuous SiC fiber3O、SiC2O2、
SiCO3), due to Cl2There are etch selectivities to above-mentioned respectively phase containing Si, and not with the SiO in SiC fiber2Structural response.
The invention proposes the continuous SiC fiber surface in situ C-SiO for electro-magnetic wave absorption2Composite coating preparation side
Method, the continuous SiC fiber using PCS through oxidation cross-linked preparation carries out high-temperature chlorination as raw material in chlorine, in SiC fiber
Surface in situ generates C-SiO2Composite coating.The basic special province of continuous SiC fiber high-strength light with the composite coating, and have
There is the ability of good absorbing radar wave, is expected to become novel carrying/suction wave integrated composite reinforcement.This method
Has the characteristics that simple process, preparation temperature continuous production that is low, at low cost, being suitble to fiber.So far, both at home and abroad not yet
See the relevant report that wave-absorption fibre is prepared using the method.
The hyperoxia type continuous SiC fiber that the present invention prepares Polycarbosilane through oxidation cross-linked technique and chlorine progress high temperature are anti-
It answers, reaction temperature is 500~800 DEG C, utilizes the selection with chlorine for a variety of structures containing Si in the hyperoxia type continuous SiC fiber
Property corrosion principle, in situ generated C-SiO in SiC fiber surface2Composite coating.The composite coating have thickness uniform, controllable,
With fiber bonding strength is moderate, resistivity can in a wide range of the comprehensive advantages such as regulation.Continuous SiC with the composite coating is fine
The ability with good absorbing radar wave is tieed up, is expected to become novel carrying/suction wave integrated composite reinforcement.
In the present invention, the continuous SiC fiber using PCS through oxidation cross-linked preparation is existed as raw material with the method that chlorine etches
In the certain thickness C-SiO of fiber surface in-situ preparation under high temperature2Layer, so that SiC fabric resistor rate is 105~10-1Ω·cm
It is interior adjustable, when resistivity is in 10-1~103Between when, fiber have good absorbing property.
The beneficial effects of the present invention are:
(1) chlorination reaction is utilized, is prepared for C-SiO in the continuous surface of SiC of Polycarbosilane conversion preparation2Composite coating,
This has the characteristics that the low reaction temperature, period, simple process, at low cost；
(2) C-SiO obtained by2Composite coating thickness uniform, controllable, it is moderate with SiC fibrous binding force, and the system of coating
It is standby not drop low-fiber mechanical property, it can be used as ceramic matric composite boundary layer application；
(3) C-SiO obtained by2Composite coating structure is controllable, and resistivity can be 105Ω·cm-10-1It is adjusted in Ω cm
Section, therefore dielectric properties are adjustable, are that great design structure inhales wave integrated material.
(4) C-SiO prepared by2Composite coating is microcellular structure, has adjustable specific surface area, potential for chemistry
The fields such as catalysis and absorption.
Detailed description of the invention
Fig. 1 is with C-SiO2The stereoscan photograph of the SiC fiber of composite coating.In Fig. 1, (a) fiber cross-sectional shape
Looks；(b) fiber surface morphology.
Fig. 2 is the depth analysis of SiC fiber Auger electron spectroscopy radially after reaction.
Fig. 3 is sample permittivity figure.
Fig. 4 is the reflectivity that sample is calculated in X-band.
Specific embodiment
Below with reference to embodiment and attached drawing, invention is further described in detail.
(1) be 12wt% by oxygen content, average diameter is 13 μm, every beam 500 SiC fibre bundles are cut into the small of 10cm long
Section.It places it in Muffle furnace, under air atmosphere, is warming up to 500 DEG C with the heating rate of 5 DEG C/min, keeps the temperature 30min.Then exist
With being furnace-cooled to room temperature under air atmosphere, the SiC fiber samples A after obtaining degumming.
(2) the SiC fiber samples A dispersion after degumming is placed in 15cm × 2cm × 2cm porous graphite boat and by graphite
Boat is put into quartz tube furnace flat-temperature zone, is sealed with rubber tube and rubber stopper, confined space is formed, at room temperature with the stream of 80ml/min
The logical N of speed2Gas, duration of ventilation 60min, to ensure that inner air tube drains.
(3) the SiC fiber samples A after degumming is continued in flowing N2Under gas shielded, it is warming up to 5 DEG C/min heating rate
600 DEG C, close N2Air valve.Open Cl2Air valve, Cl2Flow is 60ml/min, keeps the temperature 10min.Then stop logical Cl2Gas,
N2With room temperature is furnace-cooled under gas atmosphere, continuous SiC fiber surface in situ C-SiO is obtained2Composite coating.
With C-SiO2The stereoscan photograph of the SiC fiber of composite coating is referring to Fig. 1, and as shown in Figure 1, fiber surface is raw
At uniform composite coating, with a thickness of 1.28um, coating is tightly combined with fiber, does not find to remove.
The depth analysis of SiC fiber Auger electron spectroscopy radially referring to fig. 2, reflects each element by Fig. 2 and contains after reaction
The distribution situation of amount radially, it can be seen that a large amount of Si atoms on surface, which are etched away, generates carbon, and a part of Si and O are remained
Get off, forms C-SiO2Composite coating.
Test shows with the C-SiO2The SiC fiber specific resistance rate of coating is 7.8 Ω .cm.Fig. 3 and 4 is the fiber
Dielectric properties and the reflection of electromagnetic wave rate for calculating acquisition.As can be seen that sample average real part of permittivity is about 5, it is average to be situated between
Electric constant imaginary part is about 10, and average loss tangent value is about 2.When thickness of sample reaches 3mm, reflection loss is better than -5.5dB.System
After standby composite coating, the strength retention of the SiC fiber is 90%, shows that there is the SiC fiber satisfactory texture to inhale wave integration
Performance.
Claims (4)
1. continuous SiC fiber surface in situ C-SiO2Preparation method of composite coating, it is characterised in that the following steps are included:
1) SiC fiber is placed in Muffle furnace, heated up under air atmosphere, then taken off in air atmosphere with room temperature is furnace-cooled to
SiC fiber samples A after glue；
2) the SiC fiber samples A after degumming that step 1) obtains is placed in porous graphite boat, is placed on heating tube furnace
In, inert atmosphere of ventilating at room temperature drains the air in tube furnace；
3) after the SiC fiber samples A after the degumming for obtaining step 1) heats up under inert atmosphere protection, nitrogen air valve is turned off
Door opens chlorine air valve, adjustment chlorine flowrate heat preservation, by modulation process, i.e., in SiC fiber surface in-situ preparation C-SiO2
Composite coating closes chlorine after heat preservation, cools to room temperature with the furnace under inert atmosphere protection to get continuous SiC fiber surface original
Position C-SiO2Composite coating；
The condition of the heating is warming up to 500~800 DEG C with the heating rate of 3~5 DEG C/min；
The adjustment chlorine flowrate is 50~100ml/min, and the time of heat preservation is 5~60min；
Following chemical reaction will occur for SiC fiber:
SiC(s)+2Cl2(g)=C (s)+SiCl4(g)
SiCxOy(s)+2Cl2(g)=(x-y) C (s)+SiCl4(g)+yCO(g)
Wherein, SiCxOyRefer to that the various metastable phases containing Si in continuous SiC fiber, the Si metastable phase are selected from SiC3O、SiC2O2、
SiCO3One of.
2. continuous SiC fiber surface in situ C-SiO as described in claim 12Preparation method of composite coating, it is characterised in that in step
It is rapid 1) in, the heating with the heating rate of 1~3 DEG C/min is warming up to 450~550 DEG C, then keeps the temperature 10~30min.
3. continuous SiC fiber surface in situ C-SiO as described in claim 12Preparation method of composite coating, it is characterised in that in step
It is rapid 1) in, the SiC fiber use utilize rich oxygen type continuous SiC fiber of the PCS through oxidation cross-linked preparation, or using utilize other
The rich oxygen type SiC fiber of modified polycarbosilane precusor preparation, fiber oxygen content are higher than 7wt.%, and average diameter is in 10~15 μ
M, resistivity are higher than 104Ω·cm。
4. continuous SiC fiber surface in situ C-SiO as described in claim 12Preparation method of composite coating, it is characterised in that in step
It is rapid 2) in, it is described at room temperature ventilate inert atmosphere time be 30min or more.
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| CN111348941B (en) * | 2020-04-29 | 2022-05-10 | 中国人民解放军国防科技大学 | Carbide-derived carbon/rhenium/iridium coating on surface of C/C composite material and preparation method thereof |
| CN112499612B (en) * | 2020-12-23 | 2023-01-10 | 北京林业大学 | Silicon carbide ceramic derived carbon material with wood hierarchical pore structure and preparation method thereof |
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| CN105439563A (en) * | 2014-08-28 | 2016-03-30 | 中国科学院大连化学物理研究所 | Integral porous carbon-silicon carbide composite material, and preparation method and application thereof |
| CN106192078A (en) * | 2016-07-19 | 2016-12-07 | 中国人民解放军国防科学技术大学 | A kind of air curing is used to carry out method prepared by low oxygen content continuous SiC fiber |
| CN106757239A (en) * | 2017-01-25 | 2017-05-31 | 厦门大学 | A kind of method of silicon carbide fibre electroplating nickel on surface |
| CN107128926A (en) * | 2017-06-28 | 2017-09-05 | 湖南大学 | A kind of preparation method of self-supporting Carbide-derived carbons nano wire |
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| CN105439563A (en) * | 2014-08-28 | 2016-03-30 | 中国科学院大连化学物理研究所 | Integral porous carbon-silicon carbide composite material, and preparation method and application thereof |
| CN106192078A (en) * | 2016-07-19 | 2016-12-07 | 中国人民解放军国防科学技术大学 | A kind of air curing is used to carry out method prepared by low oxygen content continuous SiC fiber |
| CN106757239A (en) * | 2017-01-25 | 2017-05-31 | 厦门大学 | A kind of method of silicon carbide fibre electroplating nickel on surface |
| CN107128926A (en) * | 2017-06-28 | 2017-09-05 | 湖南大学 | A kind of preparation method of self-supporting Carbide-derived carbons nano wire |
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