CN105198500A - Preparation method of sheet-shaped C/C-MoSi2 composite - Google Patents
Preparation method of sheet-shaped C/C-MoSi2 composite Download PDFInfo
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- CN105198500A CN105198500A CN201510537229.3A CN201510537229A CN105198500A CN 105198500 A CN105198500 A CN 105198500A CN 201510537229 A CN201510537229 A CN 201510537229A CN 105198500 A CN105198500 A CN 105198500A
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Abstract
The invention provides a preparation method of a sheet-shaped C/C-MoSi2 composite. The method includes the steps of conducting ultrasonic oscillation and stirring to obtain suspension liquid after molybdenum disilicide powder is dispersed in isopropanol, increasing the density of carbon fiber three-dimensional fabric through a hydrothermal glucose osmosis, placing the carbon fiber three-dimensional fabric in a glass sand core pumping filtration device, pouring the suspension liquid in a pumping filtration flat-bottom funnel so that all the suspension liquid can completely penetrate through a C/C composite, placing a sample in a glucose solution to be subjected to a homogeneous phase hydrothermal reaction so that the density of the composite can be further increased, taking out the sample after the reaction to be dried, and finally conducting thermal treatment. The prepared C/C-MoSi2 composite is moderate in density and compact in structure, and the interfaces of C/C and MoSi2 are well bonded. The C/C-MoSi2 composite good in performance can be obtained at a low temperature; experiment raw materials are easy to obtain, the preparation process is simple, operation is easy and convenient, cost is low, and the preparation method is friendly to the environment and free of pollution.
Description
Technical field
The invention belongs to C/C technical field of composite materials, relate to a kind of preparation method of laminar C/C-MoSi2 matrix material.
Background technology
Carbon/carbon (C/C) matrix material is the current high temperature composite that uniquely can be applied to 2800 DEG C, owing to having very excellent performance, it is had broad application prospects at aerospace field, the excellent properties such as such as thermal expansivity is low, density is low, high temperature resistant, resistance to ablation, high strength, high-modulus, particularly within 2200 DEG C of inert atmosphere, under condition, its strength and modulus raises and the excellent properties of increase with temperature.But C/C matrix material will be oxidized at the aerobic environment more than 370 DEG C, oxidation quality loss causes its strength degradation, limits its range of application, the use especially under high temperature or wet environment.Therefore, the high-temperature oxidation resistance improving C/C matrix material is very crucial for its application.
A kind of effective solution route in C/C matrix material, introduces superhigh temperature ceramics, such as SiC, ZrC, HfC etc.Utilize ceramic phase to play a protective role to C/C matrix material, also can not reduce the properties of C/C matrix material simultaneously, stability in high temperature environments can be improved on the contrary, broadened application scope.More carbon/carbon-refractory ceramics the matrix material of current research mainly contains C/C-SiC matrix material [LeiLiu, HejunLi.Effectofsurfcebltionproductsonthebltionresistnce ofC/C – SiCcompositesunderoxycetylenetorch.CorrosionScience, 2013, 67:60-66, S.Singh, V.K.Srivstv.EffectofoxidtiononelsticmodulusofC/C – SiCcomposites.MterilsSciencendEngineering, 2008, 468:534-539.], C/C-ZrC matrix material [Xue-ToShen, Ke-ZhiLi.Theeffectofzirconiumcrbideonbltionofcrbon/crbon compositesundernoxycetyleneflme.CorrosionScience, 2011, 53:105-112, ShenXueto, LiKezhi.Microstructurendbltionpropertiesofzirconiumcrbid edopedcrbon/crboncomposites.Crbon, 2010, 48:344-351, Chun-xunLiu, Jin-xunChen.PyrolysismechnismofZrCprecursorndfbrictionof C/C – ZrCcompositesbyprecursorinfiltrtionndpyrolysis.Trns.Nonf errousMet.Soc.Chin, 2014, 24:1779-1784.], C/C-SiC-ZrC matrix material [ZhoqinLi, HejunLi.Microstructurendbltionbehviorsofintegerfeltreinf orcedC/C-SiC-ZrCcompositesprepredbytwo-stepmethod.Cermic sInterntionl, 2012, 38:3419 – 3425, LeiZhung, Qin-gngFu.Effectofpre-oxidtiontretmentonthebondingstreng thndthermlshockresistnceofSiCcotingforC/C – ZrC – SiCcomposites.2015.], C/C-HfC matrix material [LingXue, Zhe-nSu.MicrostructurendbltionbehviorofC/C – HfCcompositesprepredbyprecursorinfiltrtionndpyrolysis.Co rrosionScience.2015] etc.
Except above-mentioned high temperature ceramic material, molybdenum disilicide also can be introduced in C/C matrix material as high temperature material, improves C/C anti-oxidant and mechanical property at high temperature.MoSi
2as a kind of intermetallic compound, there is very excellent performance equally, be the most potential current high-temperature structural material, can be applicable to more than 1200 DEG C.MoSi
2medium density, has high-melting-point high-modulus, has fabulous high-temperature stability and high-temperature oxidation resistance, the more important thing is that molybdenum disilicide has rust inhibition under high temperature aerobic environment, generates SiO with oxygen reaction
2protective layer, SiO
2there is mobility, can the defect such as crackle of packing C/C matrix material stop oxygen to react with inner C/C matrix material further, thus provide protection is served to C/C matrix material, can at high temperature use for a long time.The combination of molybdenum disilicide and carbon fiber can be made tight by homogeneous phase water-heat process sedimentary organism carbon, interface is good.
The preparation method of blocking/carbon-refractory ceramics matrix material is varied up till now, mainly contains following several: precursor heat of immersion solution, chemical vapor infiltration, melting siliconising method, reaction melt impregnation, chemical Vapor deposition process etc.The polymer infiltration and pyrolysis fado time impregnation technology cycle is long, easy generation shrinkage crack, high [the B.Yn of cost, Z.F.Chen, J.X.Zhu, J.Z.Zhng, Y.Jing, Effectsofbltiontdifferentregionsinthree-dimensionlorthog onlC/SiCcompositesbltedbyoxycetylenet1800 DEG C, J.Mter.ProcessTech.209 (2009) 3438 – 3443.], the matrices of composite material densification rate adopting chemical vapor infiltration to prepare is low, production cycle is long, low [the J.Yin of matrix material stability, H.B.Zhng, X.Xiong, J.Zuo, H.J.To, bltionpropertiesofC/C – SiCcompositestestedonnrcheter, SolidStteSci.13 (2011) 2055 – 2059.], the standby matrix material of melting siliconising legal system is adopted easily to make fibre reinforcement strength degradation, cost is too high [SeYoungKim also, etl.Wer-mechniclpropertiesoffiller-ddedliquidsiliconinfi ltrtionC/C – SiCcompositesMterilsndDesign [J], 44 (2013) 107 – 113.], and the matrix material adopting reaction melt impregnation to prepare is very large to Carbon Fiber Damage, cause composite materials property on the low side, fracture toughness property difference [Z.Q.Li, H.J.Li, S.Y.Zhng, J.Wng, W.Li, F.J.Sun, Effectofrectionmeltinfiltrtiontempertureonthebltionprope rtiesof2DC/C – SiC – ZrCcomposites, Corros.Sci.58 (2012) 12 – 19.].And the method adopting vacuum filtration-homogeneous phase hydrothermal method to prepare carbon/carbon-refractory ceramics matrix material have not been reported.
Summary of the invention
For overcoming the problems of the prior art, the object of the present invention is to provide a kind of preparation method of laminar C/C-MoSi2 matrix material,
For achieving the above object, present invention employs following technical scheme:
A kind of laminar C/C-MoSi
2the preparation method of matrix material, comprises the following steps:
1) be scattered in by molybdenum disilicide powder in Virahol and obtain mixture, in mixture, molybdenum disilicide powder concentration is 35 ~ 45g/L, is stirred by mixture, obtains suspension;
2) carbon fiber stereo fabric is cut into disk;
3) disk is placed in glucose solution and at 180 ~ 220 DEG C, carries out homogeneous phase hydrothermal treatment consists 6 ~ 8h, deposited carbon layer on carbon fiber, obtain C/C sample;
4) by step 3) the C/C sample prepared lies against in glass core Suction filtration device, and then suspension is poured in the funnel of vacuum filtration level land, carry out suction filtration;
5) sample after suction filtration is carried out homogeneous phase hydrothermal treatment consists 8 ~ 12h in glucose solution at 180 ~ 220 DEG C, and repeat homogeneous phase hydrothermal treatment consists until obtaining density is 1.2 ~ 1.5g/cm
3matrix material, then dry;
6) dried sample is heat-treated 1 ~ 2h in 1400 ~ 1600 DEG C under argon shield, obtain laminar C/C-MoSi
2matrix material.
Described step 1) in stir before by mixture ultrasonic vibration 30 ~ 50min; The time of stirring is 2 ~ 4h.
The median size of described molybdenum disilicide powder controls at 1 ~ 3 μm.
The density of described carbon fiber stereo fabric is 0.2 ~ 0.4g/cm
3.
The diameter of described disk is 2 ~ 6cm, and thickness is 0.5 ~ 3cm.
Described step 3) and step 5) in the concentration of glucose solution be 0.5 ~ 1mol/L.
Described suction filtration adopts vacuum pump to carry out, and vacuum pump is bled and is pressed onto-0.09 ~-0.1MP, and rate of air sucked in required is 8 ~ 10L/min, and power is 180W, frequency 50Hz, and voltage is 220V.
Described drying is carried out in electric drying oven with forced convection; Thermal treatment is carried out in a vacuum furnace.
The temperature of described drying is 60 ~ 100 DEG C, and the time is dry 2 ~ 5h.
Compared with prior art, beneficial effect of the present invention is embodied in:
The present invention utilizes the feature of vacuum filtration-homogeneous phase hydrothermal deposition method, first makes MoSi by this simple experimental installation of vacuum filtration equipment
2particle infiltrates and deposits in low density carbon/carbon compound material, avoid the longer preparation technology of the methods such as polymer infiltration and pyrolysis and high temperature to the damage of carbon fiber, simultaneously, feature due to suction filtration can obtain the matrix material with gradient-structure, gradient composites can improve cohesive strength, reduce the unrelieved stress between differing materials and cracks deflection and bridge, and eliminate point of crossing, interface, greatly reduce technology difficulty and cost.Homogeneous phase hydrothermal method is same effectively simple, and the glucose solution of moderate concentration is subcritical with under supercritical water heat condition, and carbonization pyrolysis reduction to improve composite density, and improves the interface cohesion of ceramic matrix and carbon fiber.And take glucose as starting material, environmental protection, with low cost, reaction product environmental friendliness is pollution-free, adopts hydrothermal synthesis method to have the reaction times short, the features such as temperature is low, efficiency is high, energy-conserving and environment-protective.
The heat treatment time of later stage to matrix material is short and effective, can make biological carbon carbonization, and due to the biological carbon-coating of carbon fiber external sediment, thus can not have too many thermal damage to carbon fiber, the bonding strength of carbon fiber and carbon and molybdenum disilicide can improve in hot place; And make the hole of holding one's breath existed in carbon felt become ventilate, be conducive to subsequent process and improve composite density further.C/C-MoSi prepared by the present invention
2composite density is moderate, compact structure, C/C and MoSi
2interface cohesion is good.The present invention can obtain at low temperatures has that intensity is high and the C/C-MoSi that friction and wear behavior excellent, high-temperature oxidation resistance is good
2matrix material.Raw material of the present invention easily obtains, and preparation technology is simple, and easy and simple to handle, cost is low, and environmental friendliness is pollution-free.
Flake composite material size obtained by the present invention as anti-yaw damper structured material, high temperature friction sheet material, can have certain using value.The present invention prepares densification, has the C/C-MoSi of compact structure
2matrix material, is expected to improve C/C matrix material mechanical property under the high temperature conditions, is expected to the new breakthrough obtaining C/C matrix material high-temperature oxidation resistant, anti-yaw damper performance, significant in the application of high-temperature field to expansion C/C matrix material.
Accompanying drawing explanation
Fig. 1 is C/C-MoSi prepared by embodiment 1
2the XRD figure of matrix material;
Fig. 2 is C/C-MoSi prepared by embodiment 1
2composite material surface SEM schemes;
Fig. 3 is C/C-MoSi prepared by embodiment 1
2matrix material section SEM schemes.
Embodiment
Below in conjunction with drawings and Examples, the present invention is elaborated.
Embodiment 1:
1) select commercially available molybdenum disilicide powder (through dry ball milling 24h, median size controls at 1 ~ 3 μm), Virahol (purity >=99.8%), glucose (purity >=99%) is raw material;
2) first getting appropriate molybdenum disilicide powder 6g is scattered in 150mL Virahol, be mixed with the mixture that concentration is 40g/L, by mixture ultrasonic vibration (ultrasonic power is 800W) 50min, be then placed on magnetic stirring apparatus and stir 2h, obtain suspension;
3) be 0.2g/cm by density
3carbon fiber stereo fabric (manufacturer: Jiangsu Tianniao High Technology Co., Ltd.) to cut into diameter be 3cm, thickness is the disk of 0.5cm;
4) glucose solution disk being placed in 0.5mol/L carries out 180 DEG C of homogeneous phase hydrothermal treatment consists 6h, and deposited carbon layer on carbon fiber, plays a protective role to fiber, and promotes certain density, obtains C/C sample;
5) by step 4) the C/C sample prepared lies against in glass core Suction filtration device, and then suspension is poured in vacuum filtration Buchner filter, carry out suction filtration, vacuum pump is bled and is pressed onto-0.1MP, and rate of air sucked in required is 8 ~ 10L/min, and power is 180W, frequency 50Hz, voltage is 220V;
6) be in 0.5mol/L glucose solution by the sample after suction filtration in concentration, carry out homogeneous phase hydrothermal treatment consists 10h in 180 DEG C, obtain matrix material, improve composite density further, repeat hydrothermal treatment consists until the density of matrix material reaches 1.2g/cm
3;
7) open water heating kettle, take out sample, 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 oven, under argon shield at 1500 DEG C thermal treatment 1h, obtain laminar C/C-MoSi
2matrix material.
The C/C-MoSi for preparing of the present invention as seen from Figure 1
2the main component of matrix material is C and MoSi
2, the present invention prepares C/C-MoSi as seen from Figure 2
2composite material surface is comparatively fine and close, does not have multiple cracks and hole, even and smooth, as seen from Figure 3 C/C-MoSi of the present invention
2composite fiber is combined better with matrix.
Embodiment 2:
2) first getting appropriate molybdenum disilicide powder 5.25g is scattered in 150mL Virahol, be mixed with the mixture that concentration is 35g/L, by mixture ultrasonic vibration (ultrasonic power is 800W) 30min, be then placed on magnetic stirring apparatus and stir 2h, obtain suspension;
3) be 0.3g/cm by density
3carbon fiber stereo fabric (manufacturer: Jiangsu Tianniao High Technology Co., Ltd.) to cut into diameter be 4cm, thickness is the disk of 1cm;
4) glucose solution disk being placed in 0.75mol/L carries out 200 DEG C of homogeneous phase hydrothermal treatment consists 6h, and deposited carbon layer on carbon fiber, plays a protective role to fiber, and promotes certain density, obtains C/C sample;
5) by step 4) the C/C sample prepared lies against in glass core Suction filtration device, and then suspension is poured in vacuum filtration Buchner filter, carry out suction filtration, vacuum pump is bled and 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) by the sample after suction filtration in concentration be 0.75mol/L glucose solution in, carry out homogeneous phase hydrothermal treatment consists 12h in 200 DEG C, obtain matrix material, improve composite density further, repeat hydrothermal treatment consists until the density of matrix material reaches 1.37g/cm
3;
7) open water heating kettle, take out sample, 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 oven, under argon shield at 1500 DEG C thermal treatment 1h, obtain laminar C/C-MoSi
2matrix material.
Embodiment 3:
1) select commercially available molybdenum disilicide powder (through dry ball milling 24h, median size controls at 1 ~ 3 μm), Virahol (purity >=99.8%), glucose (purity >=99%) is raw material;
2) first getting appropriate molybdenum disilicide powder 6.75g is scattered in 150mL Virahol, be mixed with the mixture that concentration is 45g/L, by suspension ultrasonic vibration (ultrasonic power is 800W) 50min, be then placed on magnetic stirring apparatus and stir 2h, obtain suspension;
3) be 0.4g/cm by density
3carbon fiber stereo fabric to cut into diameter be 3cm, thickness is the disk of 2cm;
4) glucose solution disk being placed in 0.5mol/L carries out 190 DEG C of homogeneous phase hydrothermal treatment consists 8h, and deposited carbon layer on carbon fiber, plays a protective role to fiber, and promotes certain density, obtains C/C sample;
5) by step 4) the C/C sample prepared lies against in glass core Suction filtration device, and then suspension is poured in vacuum filtration Buchner filter, carry out suction filtration, vacuum pump is bled and 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) by the sample after suction filtration in concentration be 0.5mol/L glucose solution in, carry out homogeneous phase hydrothermal treatment consists 8h in 220 DEG C, obtain matrix material, improve composite density further, repeat hydrothermal treatment consists until the density of matrix material reaches 1.2g/cm
3;
7) open water heating kettle, take out sample, 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 oven, under argon shield at 1500 DEG C thermal treatment 1h, obtain laminar C/C-MoSi
2matrix material.
Embodiment 4:
1) select commercially available molybdenum disilicide powder (through dry ball milling 24h, median size controls at 1 ~ 3 μm), Virahol (purity >=99.8%), glucose (purity >=99%) is raw material;
2) first getting appropriate molybdenum disilicide powder 6g is scattered in 150mL Virahol, be mixed with the mixture that concentration is 40g/L, by mixture ultrasonic vibration (ultrasonic power is 800W) 40min, be then placed on magnetic stirring apparatus and stir 2h, obtain suspension;
3) be 0.2g/cm by density
3carbon fiber stereo fabric to cut into diameter be 4cm, thickness is the disk of 0.5cm;
4) glucose solution disk being placed in 1mol/L carries out 180 DEG C of homogeneous phase hydrothermal treatment consists 8h, and deposited carbon layer on carbon fiber, plays a protective role to fiber, and promotes certain density, obtains C/C sample;
5) by step 4) the C/C sample prepared is put in glass core Suction filtration device, and then suspension is poured in the funnel of vacuum filtration level land, carry out suction filtration, vacuum pump is bled and 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) by the sample after suction filtration in concentration be 1mol/L glucose solution in, carry out homogeneous phase hydrothermal treatment consists 10h in 200 DEG C, obtain matrix material, improve composite density further, repeat hydrothermal treatment consists until the density of matrix material reaches 1.47g/cm
3;
7) open water heating kettle, take out sample, 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 oven, under argon shield at 1500 DEG C thermal treatment 1h, obtain laminar C/C-MoSi
2matrix material.
Embodiment 5:
1) select commercially available molybdenum disilicide powder (through dry ball milling 24h, median size controls at 1 ~ 3 μm), Virahol (purity >=99.8%), glucose (purity >=99%) is raw material;
2) first getting appropriate molybdenum disilicide powder 6.75g is scattered in 150mL Virahol, be mixed with the mixture that concentration is 45g/L, by mixture ultrasonic vibration (ultrasonic power is 800W) 30min, be then placed on magnetic stirring apparatus and stir 2.5h, obtain suspension;
3) be 0.4g/cm by density
3carbon fiber stereo fabric to cut into diameter be 3cm, thickness is the disk of 0.5cm;
4) glucose solution disk being placed in 0.75mol/L carries out 200 DEG C of homogeneous phase hydrothermal treatment consists 7h, and deposited carbon layer on carbon fiber, plays a protective role to fiber, and promotes certain density, obtains C/C sample;
5) by step 4) the C/C sample prepared is put in glass core Suction filtration device, and then suspension is poured in the funnel of vacuum filtration level land, carry out suction filtration, vacuum pump is bled and 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) by the sample after suction filtration in concentration be 0.75mol/L glucose solution in, carry out homogeneous phase hydrothermal treatment consists 12h in 180 DEG C, obtain matrix material, improve composite density further, repeat hydrothermal treatment consists until the density of matrix material reaches 1.38g/cm
3;
7) open water heating kettle, take out sample, 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 oven, under argon shield at 1500 DEG C thermal treatment 1h, obtain laminar C/C-MoSi
2matrix material.
Embodiment 6
1) the molybdenum disilicide powder of particle diameter 1 ~ 3 μm is scattered in Virahol and obtains mixture, in mixture, molybdenum disilicide powder concentration is 40g/L, by mixture ultrasonic vibration (ultrasonic power is 800W) 45min, be then placed on magnetic stirring apparatus and stir 3h, obtain suspension;
2) be 0.2g/cm by density
3carbon fiber stereo fabric to cut into diameter be 5cm, thickness is the disk of 3cm;
3) glucose solution disk being placed in 0.5mol/L carries out homogeneous phase hydrothermal treatment consists 6h at 220 DEG C, and deposited carbon layer on carbon fiber obtains C/C sample;
4) by step 3) the C/C sample prepared lies against in glass core Suction filtration device, and then suspension is poured in the funnel of vacuum filtration level land, carry out suction filtration; Suction filtration adopts vacuum pump to carry out, and vacuum pump is bled and is pressed onto-0.09MP, and rate of air sucked in required is 8L/min, and power is 180W, frequency 50Hz, and voltage is 220V;
5) sample after suction filtration is carried out homogeneous phase hydrothermal treatment consists 9h in the glucose solution of 0.5mol/L at 210 DEG C, and repeat homogeneous phase hydrothermal treatment consists until obtaining density is 1.5g/cm
3matrix material, then dry 2h in electric drying oven with forced convection and at 100 DEG C;
6) dried sample is put into vacuum oven, under argon shield, heat-treat 2h in 1400 DEG C, obtain laminar C/C-MoSi
2matrix material.
Embodiment 7
1) the molybdenum disilicide powder of particle diameter 1 ~ 3 μm is scattered in Virahol and obtains mixture, in mixture, molybdenum disilicide powder concentration is 45g/L, by mixture ultrasonic vibration (ultrasonic power is 800W) 35min, be then placed on magnetic stirring apparatus and stir 4h, obtain suspension;
2) be 0.4g/cm by density
3carbon fiber stereo fabric to cut into diameter be 6cm, thickness is the disk of 1cm;
3) glucose solution disk being placed in 1mol/L carries out homogeneous phase hydrothermal treatment consists 7h at 210 DEG C, and deposited carbon layer on carbon fiber obtains C/C sample;
4) by step 3) the C/C sample prepared lies against in glass core Suction filtration device, and then suspension is poured in the funnel of vacuum filtration level land, carry out suction filtration; Suction filtration adopts vacuum pump to carry out, and vacuum pump is bled and is pressed onto-0.09MP, and rate of air sucked in required is 10L/min, and power is 180W, frequency 50Hz, and voltage is 220V;
5) sample after suction filtration is carried out homogeneous phase hydrothermal treatment consists 10h in the glucose solution of 1mol/L at 190 DEG C, and repeat homogeneous phase hydrothermal treatment consists until obtaining density is 1.4g/cm
3matrix material, then dry 1h in electric drying oven with forced convection and at 60 DEG C;
6) dried sample is put into vacuum oven, under argon shield, heat-treat 1h in 1600 DEG C, obtain laminar C/C-MoSi
2matrix material.
On carbon fiber stereo fabric, adopt the carbon of hydro-thermal mode depositing dosed quantities in the present invention, suitably reduce fabric pore aperture, the density range of the C/C sample obtained is 0.2 ~ 0.5g/cm3; Due to deposit carbon, the density of C/C sample is slightly larger than the density of carbon fiber stereo fabric.
The present invention utilizes the feature of vacuum filtration-homogeneous phase hydrothermal deposition method, first makes MoSi by this simple experimental installation of vacuum filtration equipment
2particle infiltrates and deposits in low density carbon/carbon compound material, avoid the longer preparation technology of the methods such as polymer infiltration and pyrolysis and high temperature to the damage of carbon fiber, simultaneously, feature due to suction filtration can obtain the matrix material with gradient-structure, gradient composites can improve cohesive strength, reduce the unrelieved stress between differing materials and cracks deflection and bridge, and eliminate point of crossing, interface, greatly reduce technology difficulty and cost.Homogeneous phase hydrothermal method is same effectively simple, and the glucose solution of moderate concentration is subcritical with under supercritical water heat condition, and carbonization pyrolysis reduction to improve composite density, and improves the interface cohesion of ceramic matrix and carbon fiber.And take glucose as starting material, environmental protection, with low cost, reaction product environmental friendliness is pollution-free, adopts hydrothermal synthesis method to have the reaction times short, the features such as temperature is low, efficiency is high, energy-conserving and environment-protective.
The heat treatment time of later stage to matrix material is short and effective, can make biological carbon carbonization, and due to the biological carbon-coating of carbon fiber external sediment, thus can not have too many thermal damage to carbon fiber, the bonding strength of carbon fiber and carbon and molybdenum disilicide can improve in hot place; And make the hole of holding one's breath existed in carbon felt become ventilate, be conducive to subsequent process and improve composite density further.
Flake composite material size designed by the present invention as anti-yaw damper structured material, high temperature friction sheet material, can have certain using value.
The present invention prepares densification, has the C/C-MoSi of compact structure
2matrix material, is expected to improve C/C matrix material mechanical property under the high temperature conditions, is expected to the new breakthrough obtaining C/C matrix material high-temperature oxidation resistant, anti-yaw damper performance, significant in the application of high-temperature field to expansion C/C matrix material.
Claims (9)
1. a laminar C/C-MoSi
2the preparation method of matrix material, is characterized in that, comprises the following steps:
1) be scattered in by molybdenum disilicide powder in Virahol and obtain mixture, in mixture, molybdenum disilicide powder concentration is 35 ~ 45g/L, is stirred by mixture, obtains suspension;
2) carbon fiber stereo fabric is cut into disk;
3) disk is placed in glucose solution and at 180 ~ 220 DEG C, carries out homogeneous phase hydrothermal treatment consists 6 ~ 8h, deposited carbon layer on carbon fiber, obtain C/C sample;
4) by step 3) the C/C sample prepared lies against in glass core Suction filtration device, and then suspension is poured in the funnel of vacuum filtration level land, carry out suction filtration;
5) sample after suction filtration is carried out homogeneous phase hydrothermal treatment consists 8 ~ 12h in glucose solution at 180 ~ 220 DEG C, and repeat homogeneous phase hydrothermal treatment consists until obtaining density is 1.2 ~ 1.5g/cm
3matrix material, then dry;
6) dried sample is heat-treated 1 ~ 2h in 1400 ~ 1600 DEG C under argon shield, obtain laminar C/C-MoSi
2matrix material.
2. the laminar C/C-MoSi of one according to claim 1
2the preparation method of matrix material, is characterized in that, described step 1) in stir before by mixture ultrasonic vibration 30 ~ 50min; The time of stirring is 2 ~ 4h.
3. the laminar C/C-MoSi of one according to claim 1
2the preparation method of matrix material, is characterized in that, the median size of described molybdenum disilicide powder controls at 1 ~ 3 μm.
4. the laminar C/C-MoSi of one according to claim 1
2the preparation method of matrix material, is characterized in that, the density of described carbon fiber stereo fabric is 0.2 ~ 0.4g/cm
3.
5. the laminar C/C-MoSi of one according to claim 1
2the preparation method of matrix material, is characterized in that, the diameter of described disk is 2 ~ 6cm, and thickness is 0.5 ~ 3cm.
6. the preparation method of a kind of laminar C/C-MoSi2 matrix material according to claim 1, is characterized in that, described step 3) and step 5) in the concentration of glucose solution be 0.5 ~ 1mol/L.
7. the preparation method of a kind of laminar C/C-MoSi2 matrix material according to claim 1, is characterized in that, described suction filtration adopts vacuum pump to carry out, vacuum pump is bled and is pressed onto-0.09 ~-0.1MP, and rate of air sucked in required is 8 ~ 10L/min, and power is 180W, frequency 50Hz, voltage is 220V.
8. the preparation method of a kind of laminar C/C-MoSi2 matrix material according to claim 1, it is characterized in that, described drying is carried out in electric drying oven with forced convection; Thermal treatment is carried out in a vacuum furnace.
9. the preparation method of a kind of laminar C/C-MoSi2 matrix material according to claim 1 or 8, is characterized in that, the temperature of described drying is 60 ~ 100 DEG C, and the time is dry 2 ~ 5h.
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| CN105669232A (en) * | 2016-01-28 | 2016-06-15 | 陕西科技大学 | Preparation method of SiC modified C/C-MoSi2 composite material |
| CN105732123A (en) * | 2016-01-28 | 2016-07-06 | 陕西科技大学 | Preparation method of C/C-MoSi2 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 |
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