CN105198500B - A kind of laminar C/C MoSi2The preparation method of composite - Google Patents
A kind of laminar C/C MoSi2The preparation method of composite Download PDFInfo
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Abstract
A kind of laminar C/C MoSi2The preparation method of composite, ultrasonic vibration after molybdenum disilicide powder is scattered in isopropanol, stirs to obtain suspension；Carbon fiber stereo fabric is lifted into density by the way of hydro-thermal infiltration glucose, is then placed into glass core Suction filtration device, suspension is poured into suction filtration Buchner filter so that suspension is all through C/C composites.Sample is placed in glucose solution carries out homogeneous hydro-thermal reaction further to improve composite density, and the style that will be taken out after reaction is finally heat-treated in drying.C/C MoSi prepared by the present invention2Composite density is moderate, compact structure, C/C and MoSi2Interface cohesion is good；The present invention is at low temperature the good C/C MoSi of availability2Composite；And experimental raw is readily available, preparation process is simple is easy to operate, low cost, environment-friendly pollution-free.
Description
Technical field
The invention belongs to C/C technical field of composite materials, it is related to a kind of preparation side of laminar C/C-MoSi2 composites
Method.
Background technology
Carbon/carbon (C/C) composite is the currently the only high-temperature composite material that can apply to 2800 DEG C, due to non-
The performance of Chang Youyi causes that it has broad application prospects in aerospace field, such as thermal coefficient of expansion is low, density is low, resistance to
The excellent properties such as high temperature, resistance to ablation, high intensity, high-modulus, particularly within 2200 DEG C of inert atmosphere under the conditions of its intensity
Raised and increased excellent properties with temperature with modulus.However, C/C composites will be by the aerobic environment more than 370 DEG C
Oxidation, oxidation quality loss causes its intensity to decline, and its range of application is limited, especially under high temperature or wet environment
Use.Therefore, the high-temperature oxidation resistance for improving C/C composites is very crucial for its application.
A kind of effective solution route is to introducing superhigh temperature ceramics, such as SiC, ZrC, HfC etc. in C/C composites.
C/C composites are played a protective role using ceramic phase, while the properties of C/C composites will not be also reduced, on the contrary
Stability in high temperature environments can be improved, expands range of application.More carbon/carbon-refractory ceramics composite wood is studied at present
Material mainly has C/C-SiC composites [Lei Liu, Hejun Li.Effect of surfce bltion products on
the bltion resistnce of C/C–SiC composites under oxycetylene torch.Corrosion
Science,2013,67:60-66、S.Singh,V.K.Srivstv.Effect of oxidtion on elstic
modulus of C/C–SiC composites.Mterils Science nd Engineering,2008,468:534-
539.], C/C-ZrC composites [Xue-To Shen, Ke-Zhi Li.The effect of zirconium crbide on
bltion of crbon/crbon composites under n oxycetylene flme.Corrosion Science,
2011,53:105-112、Shen Xueto,Li Kezhi.Microstructure nd bltion properties of
Zirconium crbide doped crbon/crbon composites.Crbon, 2010,48：344-351、Chun-xun
Liu,Jin-xun Chen.Pyrolysis mechnism of ZrC precursor nd fbriction of C/C–ZrC
composites by precursor infiltrtion nd pyrolysis.Trns.Nonferrous
Met.Soc.Chin,2014,24:1779-1784.], C/C-SiC-ZrC composites [Zhoqin Li, Hejun
Li.Microstructure nd bltion behviors of integer felt reinforced C/C-SiC-ZrC
composites prepred by two-step method.Cermics Interntionl,2012,38:3419–3425、
Lei Zhung,Qin-gng Fu.Effect of pre-oxidtion tretment on the bonding strength
nd therml shock resistnce of SiC coting for C/C–ZrC–SiC composites.2015.]、C/
C-HfC composites [Ling Xue, Zhe-n Su.Microstructure nd bltion behvior of C/C-HfC
composites prepred by precursor infiltrtion nd pyrolysis.Corrosion
Science.2015] etc..
In addition to above-mentioned high temperature ceramic material, molybdenum disilicide can also introduce C/C and be combined as exotic material
In material, C/C anti-oxidant and mechanical properties at high temperature are improved.MoSi2Equally have as a kind of intermetallic compound
Very excellent performance, is current most potential high-temperature structural material, can be applied to more than 1200 DEG C.MoSi2Density
It is moderate, with high-melting-point high-modulus, with fabulous high-temperature stability and high-temperature oxidation resistance, it is often more important that molybdenum disilicide exists
There is rust inhibition under high temperature aerobic environment, SiO is generated with oxygen reaction2Protective layer, SiO2With mobility, can be compound with packing C/C
The defects such as the crackle of material prevent oxygen from further being reacted with internal C/C composites, so as to serve guarantor to C/C composites
Shield is acted on, and can be used at high temperature for a long time.Can cause that molybdenum disilicide is fine with carbon by homogeneous water-heat process sedimentary organism carbon
That ties up is tightly combined, and interface is good.
Preparation method to current blocking/carbon-refractory ceramics composite is varied, mainly there is following several：First
Body dipping pyrolysismethod is driven, chemical vapor infiltration melts siliconising method, reacts melt impregnation, chemical vapour deposition technique etc..Forerunner
Body infiltration pyrolysis fado time impregnation technology cycle is long, is also easy to produce contraction crack, high cost [B.Yn, Z.F.Chen, J.X.Zhu,
J.Z.Zhng,Y.Jing,Effects of bltion t different regions in three-dimensionl
orthogonl C/SiC composites blted by oxycetylene t 1800℃,J.Mter.Process
Tech.209 (2009) 3438-3443.], the matrices of composite material densification rate prepared using chemical vapor infiltration is low, raw
The product cycle is long, composite stability low [J.Yin, H.B.Zhng, X.Xiong, J.Zuo, H.J.To, bltion
properties of C/C–SiC composites tested on n rc heter,Solid Stte Sci.13(2011)
2055-2059.], the composite for being prepared using melting siliconising method easily declines fibre reinforcement intensity, and cost is also too high
[Se Young Kim,etl.Wer-mechnicl properties of filler-dded liquid silicon
Infiltrtion C/C-SiC composites Mterils nd Design [J], 44 (2013) 107-113.], and use
Composite prepared by reaction melt impregnation is very big to Carbon Fiber Damage, causes composite materials property relatively low, is broken tough
Poor [Z.Q.Li, H.J.Li, S.Y.Zhng, J.Wng, W.Li, F.J.Sun, Effect of the rection melt of property
infiltrtion temperture on the bltion properties of 2D C/C–SiC–ZrC composites,
Corros.Sci.58(2012)12–19.].And it is multiple using vacuum filtration-homogeneous hydrothermal method prepares carbon/carbon-refractory ceramics
The method of condensation material has not been reported.
The content of the invention
To overcome the problems of the prior art, it is an object of the invention to provide a kind of laminar C/C-MoSi2 composite woods
The preparation method of material,
To reach above-mentioned purpose, present invention employs following technical scheme：
A kind of laminar C/C-MoSi2The preparation method of composite, comprises the following steps：
1) molybdenum disilicide powder is scattered in isopropanol to obtain mixture, in mixture molybdenum disilicide powder concentration be 35~
45g/L, stirs the mixture for uniformly, obtaining suspension；
2) carbon fiber stereo fabric is cut into disk；
3) disk is placed in glucose solution carries out homogeneous 6~8h of hydro-thermal process at 180~220 DEG C, in carbon fiber
Upper deposited carbon layer, obtains C/C samples；
4) by step 3) prepare C/C samples lie against in glass core Suction filtration device, suspension is then poured into vacuum
In the funnel of suction filtration level land, suction filtration is carried out；
5) by the sample after suction filtration in glucose solution in carrying out homogeneous 8~12h of hydro-thermal process at 180~220 DEG C, and
Homogeneous hydro-thermal process is repeated until it is 1.2~1.5g/cm to obtain density3Composite, then dry；
6) dried sample is carried out into 1~2h of heat treatment under argon gas protection in 1400~1600 DEG C, obtains flake
C/C-MoSi2Composite.
The step 1) in before stirring by 30~50min of mixture ultrasonic vibration；The time of stirring is 2~4h.
The average grain diameter of the molybdenum disilicide powder is controlled at 1~3 μm.
The density of the carbon fiber stereo fabric is 0.2~0.4g/cm3。
A diameter of 2~6cm of the disk, thickness is 0.5~3cm.
The step 3) and step 5) in the concentration of glucose solution be 0.5~1mol/L.
The suction filtration is carried out using vavuum pump, and vavuum pump pumping is pressed onto -0.09~-0.1MP, and rate of air sucked in required is 8~
10L/min, power is 180W, and frequency 50Hz, voltage is 220V.
The drying is carried out in electric drying oven with forced convection；Heat treatment is carried out in a vacuum furnace.
The dry temperature is 60~100 DEG C, and the time is to dry 2~5h.
Compared with prior art, beneficial effects of the present invention are embodied in：
The characteristics of present invention is using vacuum filtration-homogeneous hydrothermal deposition method, first by this letter of vacuum filtration equipment
Single experimental provision causes MoSi2Particle penetrates into and deposits in low-density carbon/carbon compound material, it is to avoid polymer infiltration and pyrolysis
Damage of the preparation technology and high temperature more long etc. method to carbon fiber, simultaneously as can obtain that there is ladder the characteristics of suction filtration
The composite of structure is spent, gradient composites can improve adhesion strength, reduce residual stress and crackle between different materials
Driving force, and interface crosspoint is eliminated, greatly reduce technology difficulty and cost.Homogeneous hydro-thermal method is equally easy and effective, dense
The moderate glucose solution of degree under subcritical and supercritical water heat condition, carbonization pyrolysis reduction to improve composite density,
And improve the interface cohesion of ceramic matrix and carbon fiber.And environmentally friendly, with low cost with glucose as raw material, reaction is produced
Substance environment close friend is pollution-free, has the reaction time short using hydrothermal synthesis method, temperature is low, efficiency high, energy-conserving and environment-protective the features such as.
Later stage is short and effective to the heat treatment time of composite, can cause biological carbon carbonization, and due to carbon fiber
The biological carbon-coating of external sediment, thus will not have too many fire damage to carbon fiber, hot place can improve carbon fiber and carbon and two silication
The bond strength of molybdenum；And cause that hole of holding one's breath present in carbon felt is changed into open pore, be conducive to subsequent process further to improve compound
Density of material.C/C-MoSi prepared by the present invention2Composite density is moderate, compact structure, C/C and MoSi2Interface cohesion is good
It is good.The present invention can be obtained at low temperature has that intensity is high and friction and wear behavior is excellent, high-temperature oxidation resistance is good
C/C-MoSi2Composite.Raw material of the present invention is readily available, and preparation process is simple is easy to operate, low cost, environment-friendly nothing
Pollution.
Flake composite material size obtained by the present invention can as anti-yaw damper structural material, high temperature friction sheet material,
With certain application value.The present invention prepares C/C-MoSi that is fine and close, having compact structure2Composite, is expected to improve C/C
Composite mechanical property under the high temperature conditions, is expected to acquirement C/C composites high-temperature oxidation resistant, the new of Burning corrosion resistance energy and dashes forward
It is broken, it is significant in the application of high-temperature field to expanding C/C composites.
Brief description of the drawings
Fig. 1 is C/C-MoSi prepared by embodiment 12The XRD of composite；
Fig. 2 is C/C-MoSi prepared by embodiment 12Composite material surface SEM schemes；
Fig. 3 is C/C-MoSi prepared by embodiment 12Composite section SEM schemes.
Specific embodiment
The present invention is elaborated with reference to the accompanying drawings and examples.
Embodiment 1：
1) commercially available molybdenum disilicide powder (by dry ball milling 24h, average grain diameter is controlled at 1~3 μm) is selected, isopropanol is (pure
Degree >=99.8%), glucose (purity >=99%) is raw material；
2) appropriate molybdenum disilicide powder 6g is taken first to be scattered in 150mL isopropanols, is configured to the mixing that concentration is 40g/L
Thing, mixture ultrasonic vibration (ultrasonic power is 800W) 50min is then placed within stirring 2h on magnetic stirring apparatus, must suspend
Liquid；
3) it is 0.2g/cm by density3Carbon fiber stereo fabric (manufacturer：Jiangsu day bird new and high technology share is limited
Company) a diameter of 3cm is cut into, thickness is the disk of 0.5cm；
4) being placed in disk in the glucose solution of 0.5mol/L carries out 180 DEG C of homogeneous hydro-thermal process 6h, on carbon fiber
Deposited carbon layer, plays a protective role to fiber, and lifts certain density, obtains C/C samples；
5) by step 4) prepare C/C samples lie against in glass core Suction filtration device, suspension is then poured into vacuum
In suction filtration Buchner filter, suction filtration is carried out, vavuum pump pumping is pressed onto -0.1MP, and rate of air sucked in required is 8~10L/min, and power is 180W, frequency
Rate 50Hz, voltage is 220V；
6) sample after suction filtration is carried out into homogeneous hydro-thermal process in concentration is 0.5mol/L glucose solutions in 180 DEG C
10h, obtains composite, further improves composite density, repeats hydro-thermal process until the density of composite reaches
1.2g/cm3；
7) water heating kettle is opened, sample is taken out, then the style of taking-up is put into electric drying oven with forced convection and at 80 DEG C
Dry 3h；
8) dried sample is placed in vacuum drying oven, in 1h is heat-treated at 1500 DEG C under argon gas protection, obtains final product flake
C/C-MoSi2Composite.
The C/C-MoSi that as seen from Figure 1 prepared by the present invention2The main component of composite is C and MoSi2, can be seen by Fig. 2
Go out the present invention and prepare C/C-MoSi2Composite material surface is comparatively dense, not multiple crackses and hole, it is uniform and smooth, by
Fig. 3 can be seen that C/C-MoSi of the present invention2Composite fiber is combined preferably with matrix.
Embodiment 2：
2) take appropriate molybdenum disilicide powder 5.25g first to be scattered in 150mL isopropanols, it is 35g/L's to be configured to concentration
Mixture, mixture ultrasonic vibration (ultrasonic power is 800W) 30min is then placed within stirring 2h on magnetic stirring apparatus, obtains
Suspension；
3) it is 0.3g/cm by density3Carbon fiber stereo fabric (manufacturer：Jiangsu day bird new and high technology share is limited
Company) a diameter of 4cm is cut into, thickness is the disk of 1cm；
4) being placed in disk in the glucose solution of 0.75mol/L carries out 200 DEG C of homogeneous hydro-thermal process 6h, on carbon fiber
Deposited carbon layer, plays a protective role to fiber, and lifts certain density, obtains C/C samples；
5) by step 4) prepare C/C samples lie against in glass core Suction filtration device, suspension is then poured into vacuum
In suction filtration Buchner filter, suction filtration is carried out, vavuum pump pumping is pressed onto -0.1MP, and rate of air sucked in required is 10L/min, and power is 180W, frequency
50Hz, voltage is 220V；
6) sample after suction filtration is carried out at homogeneous hydro-thermal in concentration is for the glucose solution of 0.75mol/L in 200 DEG C
Reason 12h, obtains composite, further improves composite density, repeats hydro-thermal process until the density of composite reaches
1.37g/cm3；
7) water heating kettle is opened, sample is taken out, then the style of taking-up is put into electric drying oven with forced convection and at 80 DEG C
Dry 3h.
8) dried sample is placed in vacuum drying oven, in 1h is heat-treated at 1500 DEG C under argon gas protection, obtains final product flake
C/C-MoSi2Composite.
Embodiment 3：
1) commercially available molybdenum disilicide powder (by dry ball milling 24h, average grain diameter is controlled at 1~3 μm) is selected, isopropanol is (pure
Degree >=99.8%), glucose (purity >=99%) is raw material；
2) take appropriate molybdenum disilicide powder 6.75g first to be scattered in 150mL isopropanols, it is 45g/L's to be configured to concentration
Mixture, suspension ultrasonic vibration (ultrasonic power is 800W) 50min is then placed within stirring 2h on magnetic stirring apparatus, obtains
Suspension；
3) it is 0.4g/cm by density3Carbon fiber stereo fabric cut into a diameter of 3cm, thickness is the disk of 2cm；
4) being placed in disk in the glucose solution of 0.5mol/L carries out 190 DEG C of homogeneous hydro-thermal process 8h, on carbon fiber
Deposited carbon layer, plays a protective role to fiber, and lifts certain density, obtains C/C samples；
5) by step 4) prepare C/C samples lie against in glass core Suction filtration device, suspension is then poured into vacuum
In suction filtration Buchner filter, suction filtration is carried out, vavuum pump pumping is pressed onto -0.1MP, and rate of air sucked in required is 10L/min, and power is 180W, frequency
50Hz, voltage is 220V；
6) sample after suction filtration is carried out at homogeneous hydro-thermal in concentration is for the glucose solution of 0.5mol/L in 220 DEG C
Reason 8h, obtains composite, further improves composite density, repeats hydro-thermal process until the density of composite reaches
1.2g/cm3；
7) water heating kettle is opened, sample is taken out, then the style of taking-up is put into electric drying oven with forced convection and at 80 DEG C
Dry 3h；
8) dried sample is placed in vacuum drying oven, in 1h is heat-treated at 1500 DEG C under argon gas protection, obtains final product flake
C/C-MoSi2Composite.
Embodiment 4：
1) commercially available molybdenum disilicide powder (by dry ball milling 24h, average grain diameter is controlled at 1~3 μm) is selected, isopropanol is (pure
Degree >=99.8%), glucose (purity >=99%) is raw material；
2) appropriate molybdenum disilicide powder 6g is taken first to be scattered in 150mL isopropanols, is configured to the mixing that concentration is 40g/L
Thing, mixture ultrasonic vibration (ultrasonic power is 800W) 40min is then placed within stirring 2h on magnetic stirring apparatus, must suspend
Liquid；
3) it is 0.2g/cm by density3Carbon fiber stereo fabric cut into a diameter of 4cm, thickness is the disk of 0.5cm；
4) being placed in disk in the glucose solution of 1mol/L carries out 180 DEG C of homogeneous hydro-thermal process 8h, is sunk on carbon fiber
Carbon, plays a protective role to fiber, and lifts certain density, obtains C/C samples；
5) by step 4) prepare C/C samples be put in glass core Suction filtration device, suspension is then poured into vacuum and is taken out
In filter level land funnel, suction filtration is carried out, vavuum pump pumping is pressed onto -0.1MP, and rate of air sucked in required is 9L/min, and power is 180W, frequency
50Hz, voltage is 220V；
6) sample after suction filtration is carried out into homogeneous hydro-thermal process in concentration is for the glucose solution of 1mol/L in 200 DEG C
10h, obtains composite, further improves composite density, repeats hydro-thermal process until the density of composite reaches
1.47g/cm3；
7) water heating kettle is opened, sample is taken out, then the style of taking-up is put into electric drying oven with forced convection and at 80 DEG C
Dry 3h；
8) dried sample is placed in vacuum drying oven, in 1h is heat-treated at 1500 DEG C under argon gas protection, obtains final product flake
C/C-MoSi2Composite.
Embodiment 5：
1) commercially available molybdenum disilicide powder (by dry ball milling 24h, average grain diameter is controlled at 1~3 μm) is selected, isopropanol is (pure
Degree >=99.8%), glucose (purity >=99%) is raw material；
2) take appropriate molybdenum disilicide powder 6.75g first to be scattered in 150mL isopropanols, it is 45g/L's to be configured to concentration
Mixture, mixture ultrasonic vibration (ultrasonic power is 800W) 30min is then placed within stirring 2.5h on magnetic stirring apparatus,
Obtain suspension；
3) it is 0.4g/cm by density3Carbon fiber stereo fabric cut into a diameter of 3cm, thickness is the disk of 0.5cm；
4) being placed in disk in the glucose solution of 0.75mol/L carries out 200 DEG C of homogeneous hydro-thermal process 7h, on carbon fiber
Deposited carbon layer, plays a protective role to fiber, and lifts certain density, obtains C/C samples；
5) by step 4) prepare C/C samples be put in glass core Suction filtration device, suspension is then poured into vacuum and is taken out
In filter level land funnel, suction filtration is carried out, vavuum pump pumping is pressed onto -0.1MP, and rate of air sucked in required is 10L/min, and power is 180W, frequency
50Hz, voltage is 220V；
6) sample after suction filtration is carried out at homogeneous hydro-thermal in concentration is for the glucose solution of 0.75mol/L in 180 DEG C
Reason 12h, obtains composite, further improves composite density, repeats hydro-thermal process until the density of composite reaches
1.38g/cm3；
7) water heating kettle is opened, sample is taken out, then the style of taking-up is put into electric drying oven with forced convection and at 60 DEG C
Dry 3h.
8) dried sample is placed in vacuum drying oven, in 1h is heat-treated at 1500 DEG C under argon gas protection, obtains final product flake
C/C-MoSi2Composite.
Embodiment 6
1) the molybdenum disilicide powder of 1~3 μm of particle diameter is scattered in isopropanol to obtain mixture, molybdenum silicide powder in mixture
Bulk concentration is 40g/L, and mixture ultrasonic vibration (ultrasonic power is 800W) 45min is then placed within being stirred on magnetic stirring apparatus
3h is mixed, suspension is obtained；
2) it is 0.2g/cm by density3Carbon fiber stereo fabric cut into a diameter of 5cm, thickness is the disk of 3cm；
3) be placed in disk carries out homogeneous hydro-thermal process 6h at 220 DEG C in the glucose solution of 0.5mol/L, fine in carbon
Deposited carbon layer in dimension, obtains C/C samples；
4) by step 3) prepare C/C samples lie against in glass core Suction filtration device, suspension is then poured into vacuum
In the funnel of suction filtration level land, suction filtration is carried out；Suction filtration is carried out using vavuum pump, and vavuum pump pumping is pressed onto -0.09MP, and rate of air sucked in required is 8L/
Min, power is 180W, and frequency 50Hz, voltage is 220V；
5) by the sample after suction filtration in the glucose solution of 0.5mol/L in carrying out homogeneous hydro-thermal process 9h at 210 DEG C,
And homogeneous hydro-thermal process is repeated until it is 1.5g/cm to obtain density3Composite, then in electric drying oven with forced convection and
2h is dried at 100 DEG C；
6) dried sample is put into vacuum drying oven, heat treatment 2h is carried out in 1400 DEG C under argon gas protection, obtain thin
Sheet C/C-MoSi2Composite.
Embodiment 7
1) the molybdenum disilicide powder of 1~3 μm of particle diameter is scattered in isopropanol to obtain mixture, molybdenum silicide powder in mixture
Bulk concentration is 45g/L, and mixture ultrasonic vibration (ultrasonic power is 800W) 35min is then placed within being stirred on magnetic stirring apparatus
4h is mixed, suspension is obtained；
2) it is 0.4g/cm by density3Carbon fiber stereo fabric cut into a diameter of 6cm, thickness is the disk of 1cm；
3) be placed in disk carries out homogeneous hydro-thermal process 7h at 210 DEG C in the glucose solution of 1mol/L, in carbon fiber
Upper deposited carbon layer, obtains C/C samples；
4) by step 3) prepare C/C samples lie against in glass core Suction filtration device, suspension is then poured into vacuum
In the funnel of suction filtration level land, suction filtration is carried out；Suction filtration is carried out using vavuum pump, and vavuum pump pumping is pressed onto -0.09MP, and rate of air sucked in required is 10L/
Min, power is 180W, and frequency 50Hz, voltage is 220V；
5) by the sample after suction filtration in the glucose solution of 1mol/L in carrying out homogeneous hydro-thermal process 10h at 190 DEG C,
And homogeneous hydro-thermal process is repeated until it is 1.4g/cm to obtain density3Composite, then in electric drying oven with forced convection and 60
1h is dried at DEG C；
6) dried sample is put into vacuum drying oven, heat treatment 1h is carried out in 1600 DEG C under argon gas protection, obtain thin
Sheet C/C-MoSi2Composite.
Carbon in the present invention on carbon fiber stereo fabric using hydro-thermal mode depositing dosed quantities, suitably reduces fabric pore
Aperture, the density range of the C/C samples for obtaining is 0.2~0.5g/cm3；Due to deposition carbon, the density of C/C samples is slightly larger than carbon
The density of fiber stereo fabric.
The characteristics of present invention is using vacuum filtration-homogeneous hydrothermal deposition method, first by this letter of vacuum filtration equipment
Single experimental provision causes MoSi2Particle penetrates into and deposits in low-density carbon/carbon compound material, it is to avoid polymer infiltration and pyrolysis
Damage of the preparation technology and high temperature more long etc. method to carbon fiber, simultaneously as can obtain that there is ladder the characteristics of suction filtration
The composite of structure is spent, gradient composites can improve adhesion strength, reduce residual stress and crackle between different materials
Driving force, and interface crosspoint is eliminated, greatly reduce technology difficulty and cost.Homogeneous hydro-thermal method is equally easy and effective, dense
The moderate glucose solution of degree under subcritical and supercritical water heat condition, carbonization pyrolysis reduction to improve composite density,
And improve the interface cohesion of ceramic matrix and carbon fiber.And environmentally friendly, with low cost with glucose as raw material, reaction is produced
Substance environment close friend is pollution-free, has the reaction time short using hydrothermal synthesis method, temperature is low, efficiency high, energy-conserving and environment-protective the features such as.
Later stage is short and effective to the heat treatment time of composite, can cause biological carbon carbonization, and due to carbon fiber
The biological carbon-coating of external sediment, thus will not have too many fire damage to carbon fiber, hot place can improve carbon fiber and carbon and two silication
The bond strength of molybdenum；And cause that hole of holding one's breath present in carbon felt is changed into open pore, be conducive to subsequent process further to improve compound
Density of material.
Flake composite material size designed by the present invention can as anti-yaw damper structural material, high temperature friction sheet material,
With certain application value.
The present invention prepares C/C-MoSi that is fine and close, having compact structure2Composite, is expected to raising C/C composites and exists
Mechanical property under hot conditions, is expected to obtain C/C composites high-temperature oxidation resistant, the new breakthrough of Burning corrosion resistance energy, to expanding
C/C composites are significant in the application of high-temperature field.
Claims (4)
1. a kind of laminar C/C-MoSi2The preparation method of composite, it is characterised in that comprise the following steps：
1) molybdenum disilicide powder is scattered in isopropanol and obtains mixture, molybdenum disilicide powder concentration is 35~45g/ in mixture
L, stirs the mixture for uniformly, obtaining suspension；
2) carbon fiber stereo fabric is cut into disk；
3) disk is placed in glucose solution carries out homogeneous 6~8h of hydro-thermal process at 180~220 DEG C, is sunk on carbon fiber
Carbon, obtains C/C samples；
4) by step 3) prepare C/C samples lie against in glass core Suction filtration device, suspension is then poured into vacuum filtration
In the funnel of level land, suction filtration is carried out；
5) by the sample after suction filtration in glucose solution in carrying out homogeneous 8~12h of hydro-thermal process at 180~220 DEG C, and repeat
Homogeneous hydro-thermal process is until it is 1.2~1.5g/cm to obtain density3Composite, then dry；
6) dried sample is carried out into 1~2h of heat treatment under argon gas protection in 1400~1600 DEG C, obtains laminar C/C-
MoSi2Composite；
The density of the carbon fiber stereo fabric is 0.2~0.4g/cm3；
The suction filtration is carried out using vavuum pump, and vavuum pump pumping is pressed onto -0.09~-0.1MP, and rate of air sucked in required is 8~10L/
Min, power is 180W, and frequency 50Hz, voltage is 220V；
The average grain diameter of the molybdenum disilicide powder is controlled at 1~3 μm；
Characterized in that, a diameter of 2~6cm of the disk, thickness is 0.5~3cm；
The step 3) and step 5) in the concentration of glucose solution be 0.5~1mol/L；
The C/C-MoSi for preparing2Composite structure is fine and close, C/C and MoSi2Interface cohesion is good.
2. a kind of laminar C/C-MoSi according to claim 12The preparation method of composite, it is characterised in that described
Step 1) in before stirring by 30~50min of mixture ultrasonic vibration；The time of stirring is 2~4h.
3. a kind of laminar C/C-MoSi according to claim 12The preparation method of composite, it is characterised in that described
Drying is carried out in electric drying oven with forced convection；Heat treatment is carried out in a vacuum furnace.
4. a kind of laminar C/C-MoSi according to claim 1 or 32The preparation method of composite, it is characterised in that
The dry temperature is 60~100 DEG C, and the time is to dry 2~5h.
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| CN101407433A (en) * | 2008-11-06 | 2009-04-15 | 陕西科技大学 | Preparation of carbon/carbon composite material molybdenum disilicide outer coating |
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| CN104529500A (en) * | 2014-12-31 | 2015-04-22 | 陕西科技大学 | Cf/C-MC ultra-high-temperature ceramic matrix composite and preparation method thereof |
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| CN101407433A (en) * | 2008-11-06 | 2009-04-15 | 陕西科技大学 | Preparation of carbon/carbon composite material molybdenum disilicide outer coating |
| CN101863683A (en) * | 2009-04-15 | 2010-10-20 | 中国科学院上海硅酸盐研究所 | Anti-oxidation coating and preparation method thereof |
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