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 PDF

Info

Publication number
CN105198500B
CN105198500B CN201510537229.3A CN201510537229A CN105198500B CN 105198500 B CN105198500 B CN 105198500B CN 201510537229 A CN201510537229 A CN 201510537229A CN 105198500 B CN105198500 B CN 105198500B
Authority
CN
China
Prior art keywords
composite
mosi
suction filtration
density
laminar
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201510537229.3A
Other languages
Chinese (zh)
Other versions
CN105198500A (en
Inventor
曹丽云
白喆
欧阳海波
黄剑锋
李翠艳
孔新刚
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Boxing Ruifeng New Material Co ltd
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201510537229.3A priority Critical patent/CN105198500B/en
Publication of CN105198500A publication Critical patent/CN105198500A/en
Application granted granted Critical
Publication of CN105198500B publication Critical patent/CN105198500B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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

A kind of laminar C/C-MoSi2The preparation method of composite
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.
CN201510537229.3A 2015-08-28 2015-08-28 A kind of laminar C/C MoSi2The preparation method of composite Active CN105198500B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510537229.3A CN105198500B (en) 2015-08-28 2015-08-28 A kind of laminar C/C MoSi2The preparation method of composite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510537229.3A CN105198500B (en) 2015-08-28 2015-08-28 A kind of laminar C/C MoSi2The preparation method of composite

Publications (2)

Publication Number Publication Date
CN105198500A CN105198500A (en) 2015-12-30
CN105198500B true CN105198500B (en) 2017-06-13

Family

ID=54946527

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510537229.3A Active CN105198500B (en) 2015-08-28 2015-08-28 A kind of laminar C/C MoSi2The preparation method of composite

Country Status (1)

Country Link
CN (1) CN105198500B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105732123B (en) * 2016-01-28 2018-08-24 陕西科技大学 A kind of C/C-MoSi2The preparation method of composite material
CN105669232B (en) * 2016-01-28 2018-06-26 陕西科技大学 A kind of SiC is modified C/C-MoSi2The preparation method of composite material
CN106083120A (en) * 2016-06-03 2016-11-09 陕西科技大学 One prepares gradient-structure C/C MoSi2the method of SiC ceramic matrix composite material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101386551A (en) * 2008-10-29 2009-03-18 陕西科技大学 Method for preparing carbon/carbon compound material nano silicon carbide-silicon molybdenum composite coating
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
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101386551A (en) * 2008-10-29 2009-03-18 陕西科技大学 Method for preparing carbon/carbon compound material nano silicon carbide-silicon molybdenum composite coating
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
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

Also Published As

Publication number Publication date
CN105198500A (en) 2015-12-30

Similar Documents

Publication Publication Date Title
CN105237025B (en) A kind of C/C SiC MoSi2The preparation method of ceramic matric composite
CN105130485B (en) A kind of laminar C/C SiC MoSi2The preparation method of ceramic matric composite
CN107032816A (en) A kind of silicon carbide nanometer line enhancing C/C SiC ZrB2The preparation method of ceramic matric composite
CN104230367B (en) A kind of SiC-ZrC-ZrB 2nano heterogeneous ceramic modification C/C matrix material and preparation method thereof
CN106045550B (en) The preparation method of SiC-ZrC gradient modifying carbon/carbon composite materials
CN105198500B (en) A kind of laminar C/C MoSi2The preparation method of composite
CN106083120A (en) One prepares gradient-structure C/C MoSi2the method of SiC ceramic matrix composite material
CN105541416A (en) Preparation method for HfC-SiC coating on C/C composite material surface
CN102674903B (en) Preparation method of SiC/C-AlPO4-mullite antioxidation coating for C/C composite material
CN105272328A (en) Preparation method of SiC whisker reinforced mullite anti-oxidation coating
CN105350294B (en) A kind of chopped carbon fiber of applying silicon carbide layer and preparation method thereof
CN114524674A (en) Heat-proof, heat-insulation and load-bearing integrated light carbon-ceramic composite material and preparation method thereof
CN109246977A (en) A kind of preparation method of high thermal conductivity graphite composite material
CN105669231B (en) A kind of fibre reinforced MoSi2The preparation method of SiC ceramic based composites
CN102674901B (en) Preparation method of carbon/carbon material C-AlPO4-mullite-MoSi2 composite outer coating layer
CN106631161A (en) Method for preparing high-temperature oxidation resistant composite coating on surface of carbon-based material
CN105777207A (en) Preparation method for carbon/carbon composite Yb2Si2O7 whisker toughened Yb2SiO5 composite coating
CN116120080B (en) ZrB (ZrB) 2 ZrC-SiC modified carbon/carbon composite material and preparation method and application thereof
CN115894085B (en) Composite ceramic coating material and preparation method and application thereof
CN106083209B (en) A kind of preparation method of micro-structured configuration interlayer interface Mullite/ yttrium silicate composite coatings
CN106478120B (en) A kind of preparation method of the modified C/C composite material of binary ceramic
CN105967755B (en) A kind of crystal whisker toughened mullite antioxidant coating of carbon/carbon composite mullite and preparation method thereof
CN102936145B (en) Preparation method of Y2SiO5 whisker toughened mullite composite coating
CN106064950B (en) A kind of quick preparation C/C-MoSi2The method of composite material
CN105669232B (en) A kind of SiC is modified C/C-MoSi2The preparation method of composite material

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20201208

Address after: 233000 Xianghe Home Floor No.9, Xinhuai Road, Dongsheng Street, Longzihu District, Bengbu City, Anhui Province

Patentee after: Bengbu Qibang Science and Technology Information Consulting Co.,Ltd.

Address before: 233000 Room 1402, Ziyang Building, Pearl Plaza, Huaishang District, Bengbu City, Anhui Province

Patentee before: Anhui Hanbang Technology Consulting Co.,Ltd.

Effective date of registration: 20201208

Address after: 233000 Room 1402, Ziyang Building, Pearl Plaza, Huaishang District, Bengbu City, Anhui Province

Patentee after: Anhui Hanbang Technology Consulting Co.,Ltd.

Address before: 710021 Shaanxi province Xi'an Weiyang University Park No. 1

Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY

TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20211228

Address after: 257237 Building 1, No. 23, Gangcheng Road, dongyinggang Economic Development Zone, Dongying City, Shandong Province

Patentee after: Dongying Shengdong Petrochemical Technology Co.,Ltd.

Address before: 233000 No.9, 1st floor, Xianghe Jiayuan, Xinhuai Road, Dongsheng Street, Longzihu District, Bengbu City, Anhui Province

Patentee before: Bengbu Qibang Science and Technology Information Consulting Co.,Ltd.

TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20221223

Address after: No. 419, Central Road, Xizha Village, Jinqiu Sub district Office, Boxing Economic Development Zone, Boxing County, Binzhou City, Shandong Province, 256500

Patentee after: Boxing Ruifeng New Material Co.,Ltd.

Address before: 257237 Building 1, No. 23, Gangcheng Road, dongyinggang Economic Development Zone, Dongying City, Shandong Province

Patentee before: Dongying Shengdong Petrochemical Technology Co.,Ltd.