CN107740266A - 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 PDF

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CN107740266A
CN107740266A CN201711034050.1A CN201711034050A CN107740266A CN 107740266 A CN107740266 A CN 107740266A CN 201711034050 A CN201711034050 A CN 201711034050A CN 107740266 A CN107740266 A CN 107740266A
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sic
sic fiber
situ
sio
composite coating
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CN107740266B (en
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李思维
徐浩南
陈立富
汤明
苏智明
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Xiamen University
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    • D—TEXTILES; PAPER
    • 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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • 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
    • D—TEXTILES; PAPER
    • 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

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  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
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Abstract

Continuous SiC fiber surface in situ C SiO2Preparation method of composite coating, it is related to continuous SiC fiber.SiC fibers are placed in Muffle furnace, heated up under air atmosphere, then obtain the SiC fiber samples A after degumming with room temperature is furnace-cooled in air atmosphere；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, the air in tube furnace is drained；After SiC fiber samples A after obtained degumming is heated up under inert atmosphere protection, N is turned off2Air valve, open Cl2Air valve, adjustment chlorine flowrate insulation, by modulation process, i.e., in SiC fiber surface in-situ preparation C SiO2Composite coating, Cl is closed after insulation2Gas, room temperature is cooled to the furnace under inert atmosphere protection, produce continuous SiC fiber surface in situ C SiO2Composite coating.

Description

Continuous SiC fiber surface in situ C-SiO2Preparation method of composite coating
Technical field
The present invention relates to continuous SiC fiber, more particularly, to a kind of continuous SiC fiber surface available for electro-magnetic wave absorption C-SiO in situ2Preparation method of composite coating.
Background technology
The development of electronic information technology causes the demand of civilian radioresistance technology and military stealth technology increasingly to increase, also right Absorbing material proposes active demand (D.D.L.Chung.Electromagnetic interference shielding effectiveness of carbon materials[J].Carbon.2001,39:279-285).Absorbing material is by shaping work Skill can be divided into coating-type and structural type.Coating-type material has weight greatly and easy the shortcomings that coming off, and structural absorbing mater ials Advantage (preparation of Mu Wu high temperature resistant microwave absorbing coatings and its performance study [D] the Changsha for inhaling ripple and carrying can be had concurrently:National defence section Skill university, 2004).Wherein, continuous fiber reinforced composite materials are a kind of high performance structures absorbing materials developed in recent years.First Driving continuous SiC fiber prepared by body conversion has the outstanding advantages such as high intensity, high temperature resistant, low-density (Yajima S, Hayashi J,Omori M,etal.Development of a silicon carbide fibre with high tensile strength[J].Nature.1976,261:683-685), high-temperature process (Brennan JJ.Fiber reinforced are passed through glass and glass-ceramics composites[J].J Mater Sci Lett,1996,30:240), adulterate 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.2013,163:1-6) the methods of, it is possible to achieve Regulation to SiC fibers dielectric properties or magnetic property, it is set to produce radar-wave absorbing effect.But high-temperature process can significantly reduce The mechanical property of fiber；And for heterogeneous element doping, receive the limitation of fiber preparation process, element doping amount limited (one As less than 3%), thus the effect to electromagnetic performance is very limited.It is the side using physical deposition or chemical plating that surface, which applies metallisation, Method, the magnetic metal coatings such as iron, cobalt, nickel are applied in fiber surface, make fiber that there is magnetic loss ability.But metal coating exists close Degree is big, is easily come off etc. from SiC fiber surfaces the problem of being difficult to overcome, and limits the application of this method.
Chemical vapor deposition (CVD) technology is also to prepare the effective ways of SiC fiber surface coatings, 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 fibers and ceramic matric composite, play a part of transmitting load and deflect crackle. For the angle of electromagnetic absorption, BN is transparent to electromagnetic wave, therefore the BN coatings of surface of SiC can make electromagnetic wave penetrate coating, enter Enter fiber.In the process, BN coatings can play impedance matching effect, 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 now the absorbing property of material still depends primarily on painting SiC fibers inside layer；And for CVD pyrolytic carbons, because carbon-coating compact structure, electrical conductivity are higher, therefore, continuously CVD carbon layer mainly plays reflex to electromagnetic wave.However, scattered carbon structure can but 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, the form for passing through " polarization loss " produces wave-absorbing effect (Cao M S, Song W L, Hou Z 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, by the way that carbon is prepared as into loose structure, control Its pore-size and shape are made, electric conductivity (Guang Li, the Tianshi Xie, Shenglin of carbon material can also be regulated and controled 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 may possess it Ability is lost in electromagnetic wave.Therefore, if SiC fibers can may be made in the controllable carbon structure of SiC fiber surfaces formation structure or component With absorbing property.
Carbide-derived carbon (carbide-derived-carbon, CDC) technology is that carbide is converted in situ into by one kind 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) (Mauricio RB, Jun SB, et al.Heat treatment-induced are stored in gas structural changes in SiC-derived carbon and their impact on gas storage potential[J].Phys.Chem.C 2010,114:16562-16575), ultracapacitor (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..Compare Under, halogen etching method have relatively mild condition, the easy to control, uniform coating thickness of reaction, accessory substance be gas be easily drained, The features such as reactant purity is high.Wherein, chloridising is to prepare the most simple and practical methods of CDC.Except porous carbon structure can be formed Outside, CDC methods also have carbon-coating institutional framework it is various the characteristics of, by control the factors such as process conditions can obtain fullerene, Carbon structure known to CNT, ball-type graphite etc. are nearly all (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) CDC technologies are applied first and prepared in polymer pyrolysis Near stoichiometric proportion the SiC fibers (Tyranno SA) containing Al on, research is pointed out, SiC fibers shape after surface chlorination Into the structure of pure carbon, carbon-coating 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. grind Study carefully the CDC researchs that Polycarbosilane obtains SiC nanofibers through electrostatic spinning, mainly discuss preparation condition for CDC holes The control action of rate and specific surface area.
Above-mentioned SiC fibers are near-stoichiometric type SiC fibers, and prepared CDC coatings are 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 SiC fibers are in situ to prepare C-SiO2The research report of composite coating, also have no discuss coated conductive, dielectric properties regulation and control and its Inhaling the possibility of ripple direction application.
The content of the invention
It is an object of the invention to provide technique is simple, preparation temperature is low, cost is low, the company of the continuous production of suitable fiber Continuous SiC fiber surfaces original position C-SiO2Preparation method of composite coating.
The present invention comprises the following steps：
1) SiC fibers are placed in Muffle furnace, heated up under air atmosphere, then obtained in air atmosphere with room temperature is furnace-cooled to Obtain the SiC fiber samples A after degumming；
In step 1), the heating can be warming up to 450~550 DEG C with 1~3 DEG C/min heating rate, then be incubated 10 ~30min；The SiC fibers can use the rich oxygen type continuous SiC fiber prepared using the oxidized crosslinkings of PCS, or use and utilize Other are modified rich oxygen type SiC fibers prepared by polycarbosilane precusor, 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 the degumming for obtaining step 1) is placed in porous graphite boat, is placed on heating tubular type In stove, inert atmosphere of ventilating at room temperature, the air in tube furnace is drained；
In step 2), the time for ventilating inert atmosphere at room temperature can be more than 30min, 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, open Cl2Air valve, adjustment chlorine flowrate insulation, by modulation process, i.e., in SiC fiber surface in-situ preparations C- SiO2Composite coating, Cl is closed after insulation2Gas, room temperature is cooled to the furnace under inert atmosphere protection, produce continuous SiC fiber table Face original position C-SiO2Composite coating.
In step 3), the condition of the heating can be warming up to 500~800 DEG C with 3~5 DEG C/min heating rate；Institute It can be 50~100ml/min to state adjustment chlorine flowrate, and the time of insulation can be 5~60min, and in the process, SiC fibers 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 fibers2Structural response.
The present invention proposes the continuous SiC fiber surface in situ C-SiO for electro-magnetic wave absorption2Composite coating preparation side Method, the continuous SiC fiber prepared using the oxidized crosslinkings of PCS carry out high-temperature chlorination, in SiC fibers as raw material in chlorine 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, be expected to the reinforcement as new carrying/suction ripple integrated composite.This method There is the continuous production that technique is simple, preparation temperature is low, cost is low, is adapted 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 present invention is anti-by hyperoxia type continuous SiC fiber prepared by the oxidized crosslinking process of Polycarbosilane and chlorine progress high temperature Should, reaction temperature is 500~800 DEG C, using with selection of the chlorine for a variety of structures containing Si in the hyperoxia type continuous SiC fiber Property corrosion principle, C-SiO is in situ generated in SiC fiber surfaces2Composite coating.The composite coating have thickness uniform, controllable, With fiber bonding strength is moderate, resistivity can in a wide range of the comprehensive advantage such as regulation and control.Continuous SiC with the composite coating is fine Ability of the dimension with good absorbing radar wave, is expected to the reinforcement as new carrying/suction ripple integrated composite.
In the present invention, as raw material, the method etched with chlorine exists the continuous SiC fiber prepared using the oxidized crosslinkings of PCS In the certain thickness C-SiO of fiber surface in-situ preparation under high temperature2Layer so that SiC fabric resistor rates are 105~10-1Ω·cm It is interior adjustable, when resistivity is in 10-1~103Between when, fiber has good absorbing property.
The beneficial effects of the invention are as follows：
(1) chlorination reaction is utilized, C-SiO is prepared in continuous surface of SiC prepared by Polycarbosilane conversion2Composite coating, There should be the characteristics of low reaction temperature, period, technique is simple, cost is low；
(2) C-SiO obtained by2Composite coating thickness uniform, controllable, it is moderate with SiC fibrous binding forces, and the system of coating It is standby not drop low-fiber mechanical property, ceramic matric composite boundary layer application can be used as；
(3) C-SiO obtained by2Composite coating structure is controllable, and resistivity can be 105Ω·cm-10-1Adjusted in Ω cm Section, therefore dielectric properties are adjustable, are that great design structure inhales ripple integrated material.
(4) C-SiO prepared by2Composite coating is microcellular structure, has adjustable specific surface area, potential to be used for chemistry The field such as catalysis and absorption.
Brief description of the drawings
Fig. 1 is with C-SiO2The stereoscan photograph of the SiC fibers of composite coating.In Fig. 1, (a) fiber cross-sectional shape Looks；(b) fiber surface morphology.
Fig. 2 is the depth analysis of SiC fibers Auger electron spectroscopy radially after reaction.
Fig. 3 is sample permittivity figure.
Fig. 4 is the reflectivity that sample calculates in X-band.
Embodiment
The present invention is described in further detail with reference to embodiment and accompanying drawing.
(1) it is 12wt% by oxygen content, average diameter is 13 μm, the SiC fibre bundles per beam 500 are cut into the small of 10cm length Section.It is placed on Muffle furnace, under air atmosphere, is warming up to 500 DEG C with 5 DEG C/min heating rate, is incubated 30min.Then exist With room temperature is furnace-cooled under air atmosphere, the SiC fiber samples A after degumming is obtained.
(2) it is placed in the SiC fiber samples A after degumming is scattered 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 80ml/min stream 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 rates 600 DEG C, close N2Air valve.Open Cl2Air valve, Cl2Flow is 60ml/min, is incubated 10min.Then logical Cl is stopped2Gas, N2 With 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 fibers of composite coating is referring to Fig. 1, as shown in Figure 1, fiber surface life Into uniform composite coating, thickness 1.28um, coating is tightly combined with fiber, does not find to peel off.
The depth analysis of SiC fibers Auger electron spectroscopy radially reflects each element by Fig. 2 and contained referring to Fig. 2 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 is remained Get off, form C-SiO2Composite coating.
Test shows, with the C-SiO2The SiC fiber ratio resistances 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 fibers is 90%, shows that there is the SiC fibers satisfactory texture to inhale ripple integration Performance.

Claims (8)

1. continuous SiC fiber surface in situ C-SiO2Preparation method of composite coating, it is characterised in that comprise the following steps：
1) SiC fibers are 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 the degumming for obtaining step 1) is placed in porous graphite boat, is placed on heating tube furnace In, inert atmosphere of ventilating at room temperature, the air in tube furnace is drained；
3) after the SiC fiber samples A after the degumming for obtaining step 1) heats up under inert atmosphere protection, N is turned off2Air valve, Open Cl2Air valve, adjustment chlorine flowrate insulation, by modulation process, i.e., in SiC fiber surface in-situ preparations C-SiO2It is compound Coating, Cl is closed after insulation2Gas, room temperature is cooled to the furnace under inert atmosphere protection, produce continuous SiC fiber surface in situ C- SiO2Composite coating.
2. continuous SiC fiber surface in situ C-SiO as claimed in claim 12Preparation method of composite coating, it is characterised in that in step It is rapid 1) in, the heating with 1~3 DEG C/min heating rate is warming up to 450~550 DEG C, then is incubated 10~30min.
3. continuous SiC fiber surface in situ C-SiO as claimed in claim 12Preparation method of composite coating, it is characterised in that in step It is rapid 1) in, the SiC fibers use the rich oxygen type continuous SiC fiber prepared using the oxidized crosslinkings of PCS, or using utilizing other Rich oxygen type SiC fibers prepared by modified polycarbosilane precusor, fiber oxygen content are higher than 7wt.%, average diameter is at 10~15 μm, Resistivity is higher than 104Ω·cm。
4. continuous SiC fiber surface in situ C-SiO as claimed 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 more than 30min.
5. continuous SiC fiber surface in situ C-SiO as claimed in claim 12Preparation method of composite coating, it is characterised in that in step It is rapid 2) in, the inert atmosphere is argon gas or nitrogen.
6. continuous SiC fiber surface in situ C-SiO as claimed in claim 12Preparation method of composite coating, it is characterised in that in step It is rapid 3) in, the condition of the heating is warming up to 500~800 DEG C with 3~5 DEG C/min heating rate.
7. continuous SiC fiber surface in situ C-SiO as claimed in claim 12Preparation method of composite coating, it is characterised in that in step It is rapid 3) in, it is described adjustment chlorine flowrate be 50~100ml/min, the time of insulation is 5~60min.
8. continuous SiC fiber surface in situ C-SiO as claimed in claim 12Preparation method of composite coating, it is characterised in that in step It is rapid 3) in, following chemical reaction will occur for SiC fibers：
SiC(s)+2Cl2(g)=C (s)+SiCl4(g) (1)
SiCxOy(s)+2Cl2(g)=(x-y) C (s)+SiCl4(g)+yCO(g) (2)
Wherein, SiCxOyThe various metastable phases containing Si in hyperoxia type continuous SiC fiber are referred mainly to, the Si metastable phases include SiC3O、SiC2O2、SiCO3。
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CN109968757A (en) * 2019-04-22 2019-07-05 中国人民解放军国防科技大学 Ablation-resistant light heat-proof heat-insulation integrated composite material and preparation method thereof
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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
CN112499612A (en) * 2020-12-23 2021-03-16 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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