CN108218457A - A kind of SiC of the reinforcement containing nanometerfThe preparation method of/SiC ceramic matrix composite material - Google Patents

A kind of SiC of the reinforcement containing nanometerfThe preparation method of/SiC ceramic matrix composite material Download PDF

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CN108218457A
CN108218457A CN201810226153.6A CN201810226153A CN108218457A CN 108218457 A CN108218457 A CN 108218457A CN 201810226153 A CN201810226153 A CN 201810226153A CN 108218457 A CN108218457 A CN 108218457A
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sic
silicon carbide
composite material
nanometer
deposition
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CN108218457B (en
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黄小忠
阳海棠
岳建岭
黄奔
陆子龙
杜作娟
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Central South University
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Central South University
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Abstract

The invention discloses a kind of SiC of reinforcement containing nanometerfThe preparation method of/SiC ceramic matrix composite material, for solving existing preparation method poor controllability, the technical problems such as fibre damage is serious, electrophoretic deposition is uneven.Scheme improves electrophoretic deposition process using auxiliary electrode, nanometer reinforcement is rapidly and uniformly deposited on the boundary layer of silicon carbide fibre, by the accurate control that electrophoretic parameters realization is controlled to be distributed nanometer reinforcement in fiber interface layer, SiC is realized subsequently through techniques such as chemical vapor deposition and infiltration pyrolysisfThe densification of/SiC ceramic matrix composite material.Preparation method of the invention is simple, technique is controllable, low for equipment requirements, has good application value.Prepared SiCf/ SiC ceramic matrix composite material has excellent antioxygenic property and mechanical property.

Description

A kind of SiC of the reinforcement containing nanometerfThe preparation method of/SiC ceramic matrix composite material
Technical field
The present invention relates to ceramic matric composite field more particularly to a kind of SiC of reinforcement containing nanometerf/ SiC composite woods The preparation method of material
Background technology
Continuous carbofrax fibre enhancing ceramic matric composite (SiCf/ SiC) be grow up this beginning of the century receive weight Depending on a kind of high-temperature structural material, compared with other materials, it have low-density, high temperature resistant, anticorrosive, high intensity, high-modulus The advantages that, with the continuous improvement of technology of preparing, development is very rapid, is mainly used in hypersonic aircraft, aviation hair Motivation, fusion reactor and high temperature inhale numerous high-grade, precision and advanced fields such as wave.
But compared with high temperature alloy, SiCfThe mechanical properties such as the fracture toughness of/SiC ceramic matrix composite material be still limit its The bottleneck of advanced field application.How SiC is improvedfThe toughness and mechanical property of/SiC ceramic matrix composite material are Recent study work The research hotspot and emphasis of person.These researchs at present are concentrated mainly on that improve fibre property, optimization boundary layer performance, optimization compound Material preparation process and composite material subsequent heat treatment etc., and have in selection nano particle, nanofiber and nano wire etc. The nanometer reinforcement of effect improves SiCfThe research of/SiC ceramic matrix composite material toughness is simultaneously few.
Nanometer reinforcement can be effectively improved one-component ceramic performance by toughening mechanisms such as crack deflection and bridgings.Compound In material, nanometer reinforcement is introduced into as the second reinforcement in material matrix, can be carried out Strengthening and Toughening to microcell matrix, effectively be carried High matrix crack line extended capability.For example, SiC nanowire is a kind of nanometer reinforcement haveing excellent performance, tensile strength can reach 53.4GPa, much larger than SiC fibers and SiC whiskers.SiC nanowire is introduced into the brittleness base between scrim cloth with fiber interfascicular In body, crack propagation distance can be effectively increased, improves the brittleness of microcell matrix, improves the toughness of microcell matrix.
At present, in SiCfThe main method that nanometer reinforcement is introduced in/SiC ceramic matrix composite material is in situ synthesis, but such Method there are preparation process energy consumption is big, pollution is big, the period is long, and be difficult to control in preparation process, it is affected by environment it is apparent, set The shortcomings of standby requirement height and big fibre damage.
In contrast, electrophoretic deposition method has that simple for process, equipment requirement is low, the advantages such as at low cost, and passes through this side Method can accurately regulate and control content, thickness and microstructure of nanometer reinforcing phase etc..However electrophoretic deposition is relatively more suitable for leading Isoelectric substance is deposited, and since SiC fibers belong to insulating body, line resistance and surface resistance are big, often nanometer reinforcing phase are caused to disperse Phenomena such as uneven, excellent enhancing effect can not be obtained by eventually leading to.
Invention content
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of SiC of reinforcement containing nanometerf/ SiC is compound The preparation method of material.The SiC of gained reinforcement containing nanometerfIn/SiC ceramic matrix composite material, nanometer reinforcement is uniformly scattered in SiCfIn/SiC ceramic matrix composite material, can first mate improve composite material mechanical property.
To achieve these goals, the present invention provides following technical solution：
SiC fibers containing boundary layer or SiC fiber braids are fixed in metal plate A or graphite cake B and form work electricity Pole, metallic plate C or graphite cake D are used as to electrode, are placed in above-mentioned working electrode and to electrode the electrophoresis containing nanometer reinforcement In liquid, electrophoretic deposition nanometer reinforcement is carried out, electrophoretic deposition product is obtained, after the drying of electrophoretic deposition product, carries out CVI depositions SiC matrix is until material densification, the as SiC of the reinforcement containing nanometerf/ SiC ceramic matrix composite material；
During the electrophoretic deposition, working electrode to the distance to electrode is 10mm~50mm, and deposition voltage is 3V~50V, Sedimentation time is 1min~30min；
The nanometer reinforcement is SiC nano-powder or silicon carbide nanometer line；
The electrophoresis liquid of the silicon carbide-containing nano powder include SiC nano-powder, tetramethylammonium hydroxide, poly amic acid, Water, a concentration of 0.5g/L~60.0g/L of the SiC nano-powder, a concentration of 0.1g/L of tetramethylammonium hydroxide~ 1.5g/L, a concentration of 0.1g/L~5.0g/L of poly amic acid；The pH value of the electrophoresis liquid of the silicon carbide-containing nano powder for 9~ 12；
The electrophoresis liquid of the silicon carbide-containing nano wire is made of silicon carbide nanometer line, phenolic resin, aluminum nitrate, isopropanol, A concentration of 0.05g/L~1.0g/L of the silicon carbide nanometer line, a concentration of 0.05g/L~1.0g/L of phenolic resin, nitric acid A concentration of 0.05g/L~1.0g/L of aluminium.
Preferred scheme, the metal in the metal plate A are copper, and the metal in the metallic plate C is copper.
In the present invention, the working electrode is to the distance to electrode, refers to the metal sheet outer surface of electrode to work The distance of SiC fibers or SiC fiber braids outer surface on electrode.
Preferred scheme, when the nanometer reinforcement is SiC nano-powder, working electrode is anode, is the moon to electrode Pole；When the nanometer reinforcement is silicon carbide nanometer line, working electrode is cathode, is anode to electrode.
Preferred scheme, the electrophoresis liquid of the silicon carbide-containing nano wire with taking the mode to be, by silicon carbide nanometer line, phenolic aldehyde Resin, aluminum nitrate are added in isopropanol, stirring concussion 30min~120min in ultrasonic wave；The electricity of the silicon carbide-containing nano wire In swimming liquid, a concentration of 0.5g/L~1.0g/L of silicon carbide nanometer line, a concentration of 0.5g/L~1.0g/L of phenolic resin, nitric acid A concentration of 0.05g/L~0.25g/L of aluminium.Preferably, ultrasonic wave stirring concussion 60min~120min.
In the electrophoresis liquid of silicon carbide-containing nano wire, silicon carbide nanometer line is used as nanometer reinforcement, phenolic resin to be divided Powder, aluminum nitrate is as conductive ion compound.Conductive ion compound dissolves in the solution, forms cation and anion, Cation absorption is in nanowire surface, under the conditions of absorption adequately, between nano wire charge be identically formed it is mutually exclusive so that Nano wire is uniformly dispersed, and under the action of electrode, nano wire is by a lateral opposite side movement, deposition.
Preferred scheme, the electrophoresis liquid of the silicon carbide-containing nano powder with taking the mode to be, by SiC nano-powder, tetramethyl Base ammonium hydroxide, poly amic acid are added to the water, stirring concussion 30min~120min in ultrasonic wave；And it adds in n-butylamine and incites somebody to action The pH value of the electrophoresis liquid of SiC nano-powder is adjusted to 9~10, in the electrophoresis liquid of the silicon carbide-containing nano powder, nanometer silicon carbide A concentration of 5g/L~10g/L of powder, a concentration of 0.5g/L~1.5g/L of tetramethylammonium hydroxide, poly amic acid it is a concentration of 1g/L~3g/L.Preferably, ultrasonic wave stirring concussion 60min~120min.
In the electrophoresis liquid of silicon carbide-containing nano powder, SiC nano-powder is as nanometer reinforcement, poly amic acid conduct Dispersant, tetramethylammonium hydroxide are obtained equal as conductive ion compound, n-butylamine as pH adjusting agent by ultrasonic disperse The even electrophoresis liquid do not reunited.
Preferred scheme uses DC power supply during the electrophoretic deposition.
Preferred scheme, the temperature of electrophoretic deposition product drying is 50 DEG C~80 DEG C, the time for 120min~ 240min。
Preferred scheme, during the electrophoretic deposition, working electrode is to distance 10mm~30mm to electrode, deposition voltage 15V~30V, sedimentation time are 2min~10min.
Preferred scheme, the SiC fibers or SiC fiber braids containing boundary layer are selected from containing pyrolytic carbon (PyC) interface The SiC fibers of layer or SiC fiber braids.
As a further preference, the system of the SiC fibers or SiC fiber braids containing pyrolytic carbon (PyC) boundary layer Preparation Method is to be deposited on SiC fibers after pretreatment or SiC fiber braids by the way of chemical vapor deposition PyC boundary layers, the process conditions of deposition PyC boundary layers are, using propylene as carbon-source gas, argon gas is protective gas, depositing temperature It it is 780 DEG C~1100 DEG C, deposition pressure is 4000~8000Pa, and sedimentation time is 120~480min, and the flow of propylene is 0.1L/min~1.0L/min, the flow of argon gas is 0.5L/min~5.0L/min.
As further preferably, the depositing temperature of the deposition PyC boundary layers is 880 DEG C~980 DEG C, deposition pressure For 4000Pa~7000Pa, sedimentation time is 120min~240min, and the flow of propylene is 0.5L/min~1.0L/min, argon gas Flow be 1L/min~5L/min.
As further preferably, the pretreatment of the SiC fibers or SiC fiber braids is, under protective atmosphere SiC fibers or SiC fiber braids are heat-treated, the temperature of the heat treatment is 800 DEG C~1100 DEG C, heat treatment when Between for 10min~60min, the protective atmosphere is selected from nitrogen or argon gas.
Preferred scheme, the process conditions of the electrophoretic deposition product progress CVI deposition SiC matrixes of the drying are, described The process conditions that dry electrophoretic deposition product carries out CVI deposition SiC matrixes are, with trichloromethyl silane (MTS) for SiC matrix Presoma, hydrogen is carrier gas, and argon gas is diluent gas, and the flow of the MTS is 100~600g/h, and the flow of argon gas is 0.5L/min~3.0L/min, the flow of hydrogen is 0.2~0.8L/min；The depositing temperature is 1000 DEG C~1250 DEG C, is sunk It is 4000Pa~8000Pa to overstock power, and sedimentation time is 100min~480min.
It is further preferably, during the CVI depositions SiC matrix, the flow of the MTS is 200g/L~400g/L, argon gas Flow for 0.5L/min~3.0L/min, the flow of hydrogen is 0.4L/min~0.6L/min；The depositing temperature is 1000 DEG C~1150 DEG C, deposition pressure is 4000Pa~7000Pa, and sedimentation time is 300min~480min.
MTS, hydrogen, argon gas are first re-introduced into chemical vapor deposition stove by preferred scheme after mixing, carry out carbon The deposition of SiClx.
The principle of the present invention and advantage：
In the prior art, insulating body due to line resistance and surface resistance it is big, cause insulating body electrophoretic deposition exist not Uniform phenomenon.The present invention effectively improves the resistance problems of SiC fibers or SiC fiber braids using auxiliary electrode, in addition Using the electrophoresis liquid do not reunited of being uniformly dispersed, nanometer reinforcement is rapidly and uniformly deposited on the boundary layer of silicon carbide fibre；Afterwards It is continuous that SiC is realized by chemical vapor deposition and infiltration pyrolysis etc.fThe densification of/SiC ceramic matrix composite material, the nanometer reinforcement exist SiCfIt is uniformly dispersed in/SiC ceramic matrix composite material.
The present invention carries out nanometer using electrophoretic deposition in the SiC fibers containing PyC boundary layers or SiC fiber braids surface The deposition of reinforcement, by the improvement of auxiliary electrode, electrophoresis liquid ingredient, electrophoresis liquid dispersion performance, further combined with electrophoretic parameters, It realizes to nanometer reinforcement in the accurate control of the distribution of fiber surface, the nanometer reinforcement of electrophoretic deposition is in fiber interface layer table EDS maps are not reunited uniformly and thickness is controllable, and nano wire and boundary layer are well combined, and can be very good toughening boundary layer, improve boundary The inoxidizability and mechanical property of face layer；The quantity of crackle is reduced, increases the distance of crack propagation；In spike protein gene, play Good inhibition, SiC prepared by this methodf/ SiC ceramic matrix composite material has excellent antioxygenic property and mechanical property.With For silicon carbide nanometer line, SiC of the comparison without silicon carbide nanometer linef/ SiC ceramic matrix composite material, it is curved that this method prepares composite material Qu Qiangdu, elasticity modulus and fracture toughness have been respectively increased 90.1%, 73.2% and 65.8%, and mechanical property is promoted notable.
The preparation method of the present invention is simple, technique is controllable, low for equipment requirements, has good application value.
Description of the drawings
Electrophoretic deposition principle schematic used in Fig. 1 case study on implementation 3；
Auxiliary electrode schematic diagram used in Fig. 2 case study on implementation 1；
The scanning electron microscopic picture that prepared silicon carbide nanometer line deposits on silicon carbide fibre in Fig. 3 case study on implementation 1
The scanning electron microscopic picture of SiC nano-powder used in Fig. 4 case study on implementation 3；
The scanning electron microscopic picture of SiC nano-powder electrophoretic deposition cross section on fiber used in Fig. 5 case study on implementation 3；
SiC nano-powder electrophoretic deposition is in the scanning electron microscopic picture of fiber upper surface used in Fig. 6 case study on implementation 3；
Specific embodiment
It elaborates with reference to the accompanying drawings and detailed description to the present invention.
Embodiment 1：
Step 1: by 120 × 80 × 10mm3Silicon carbide fibre braided part under the conditions of nitrogen atmosphere, be warming up to 1000 DEG C, 30min is kept the temperature, room temperature is cooled to the furnace after heat preservation；
Step 2: the processed silicon carbide fibre braided part of step 1 is warming up to 980 DEG C in resistance furnace, argon gas atmosphere Under protection, using propylene as carbon source, 120min, deposition pressure 7000Pa are kept the temperature, the flow of propylene is 1L/min, the flow of argon gas For 5.0L/min.Fiber surface in silicon carbide fibre braided part prepares uniform pyrolytic carbon boundary layer.
Step 3: silicon carbide nanometer line is configured to finely dispersed electrophoresis liquid：Silicon carbide nanometer line content is 0.5g/L, Nitric acid aluminium content is 0.025g/L, and phenolic resin content 0.5g/L, solvent is isopropanol.By phenolic resin, aluminum nitrate, silicon carbide Nano wire is added sequentially in isopropanol, and ultrasonic oscillation 120min prepares homodisperse electrophoresis liquid.
Step 4: silicon carbide braided part processed in step 2 is fixed on auxiliary electrode (copper electrode) as work Electrode, auxiliary electrode are connected with the cathode of DC power supply, and the anode connection copper electrode of power supply is used as to electrode, and working electrode is the moon Pole, the distance 10mm for being fixed on electrophoresis tank, anode and cathode for anode to electrode, pour into what is prepared in step 3 in electrophoresis tank Electrophoresis liquid, constant pressure deposition voltage are 30V, and sedimentation time 2min, electrophoretic deposition takes out braided part after the completion, dry in drying box Dry, temperature is 60 DEG C.
Step 5: the silicon carbide fibre braided part containing silicon carbide nanometer line prepared by step 4 is put into chemical vapor deposition In product stove, with trichloromethyl silane (MTS) for presoma, hydrogen is reaction gas, and argon gas is diluent gas, and MTS is in thermostatic tank In gas is introduced into chemical vapor deposition stove after mixing in mixed gas tank by Bubbling method, carry out the heavy of silicon carbide Product.Specific depositing operation is as follows：1150 DEG C, deposition pressure 4000Pa, sedimentation time 480min of depositing temperature, the stream of the MTS It measures as 400g/h, the flow of argon gas is 3L/min, and the flow of hydrogen is 0.6L/min, after furnace cooling, that is, prepares silicon carbide Nano wire enhances SiCf/ SiC ceramic matrix composite material.
Embodiment 2
Step 1: by 120 × 80 × 10mm3Silicon carbide fibre braided part under the conditions of nitrogen atmosphere, be warming up to 1000 DEG C, 30min is kept the temperature, room temperature is cooled to the furnace after heat preservation；
Step 2: the processed silicon carbide fibre braided part of step 1 is warming up to 880 DEG C in resistance furnace, argon gas atmosphere Under protection, using propylene as carbon source, 240min, deposition pressure 4000Pa are kept the temperature, the flow of propylene is 0.5L/min, the stream of argon gas It measures as 1L/min.Fiber surface in silicon carbide fibre braided part prepares uniform pyrolytic carbon boundary layer.
Step 3: silicon carbide nanometer line is configured to finely dispersed electrophoresis liquid：Silicon carbide nanometer line content be 1g/L, nitre Sour aluminium content is 0.05g/L, and phenolic resin content 1g/L, solvent is isopropanol.By phenolic resin, aluminum nitrate, nanometer silicon carbide Line is added sequentially in isopropanol, and ultrasonic oscillation 60min prepares homodisperse electrophoresis liquid.
Step 4: silicon carbide braided part processed in step 2 is attached on auxiliary electrode (copper electrode) as work electricity Pole, auxiliary electrode are connected with the cathode of DC power supply, and the anode connection copper electrode of power supply is used as to electrode, and working electrode is the moon Pole, the distance 30mm for being fixed on electrophoresis tank, anode and cathode for anode to electrode, pour into what is prepared in step 3 in electrophoresis tank Electrophoresis liquid, constant pressure deposition voltage are 15V, and sedimentation time 10min, electrophoretic deposition takes out braided part after the completion, in drying box Dry, temperature is 80 DEG C.
Step 5: the silicon carbide fibre braided part containing silicon carbide nanometer line prepared by step 4 is put into chemical vapor deposition In product stove, with trichloromethyl silane (MTS) for presoma, hydrogen is reaction gas, and argon gas is diluent gas, and MTS is in thermostatic tank In gas is introduced into chemical vapor deposition stove after mixing in mixed gas tank by Bubbling method, carry out the heavy of silicon carbide Product.Specific depositing operation is as follows：1000 DEG C, deposition pressure 7000Pa, sedimentation time 300min of depositing temperature, the stream of the MTS It measures as 200g/h, the flow of argon gas is 0.5L/min, and the flow of hydrogen is 0.4L/min, after furnace cooling, that is, prepares carbonization Silicon nanowires enhances SiCf/ SiC ceramic matrix composite material.
Embodiment 3：
Step 1: by a branch of silicon carbide fibre of 10mm under the conditions of nitrogen atmosphere, 1000 DEG C are warming up to, keeps the temperature 30min, Cool to room temperature after heat preservation with the furnace；
Step 2: the processed silicon carbide fibre beam of step 1 is warming up to 980 DEG C in resistance furnace, argon gas atmosphere protection Under, using propylene as carbon source, 120min is kept the temperature, deposition pressure 7000Pa, the flow of propylene is 1L/min, and the flow of argon gas is 5L/min.Fiber surface in silicon carbide fibre braided part prepares uniform pyrolytic carbon boundary layer.
Step 3: SiC nano-powder is configured to finely dispersed electrophoresis liquid：Nanometer silicon carbide powder content be 5g/L, four Ammonium hydroxide 1.5g/L, poly amic acid 3g/L, solvent are distilled water, are pH adjusting agent with n-butylamine.It is 9 to adjust pH, By poly amic acid, tetramethyl Strong oxdiative ammonium, SiC nano-powder is added sequentially in distilled water, ultrasonic oscillation 120min, Prepare homodisperse electrophoresis liquid.
Step 4: silicon carbide fibre beam processed in step 2 is attached on auxiliary electrode (copper electrode) as work electricity Pole, auxiliary electrode are connected with the anode of DC power supply, and the cathode connection copper electrode of power supply is used as to electrode, and working electrode is sun Pole, the distance 10mm for being fixed on electrophoresis tank, anode and cathode for cathode to electrode, pour into what is prepared in step 3 in electrophoresis tank Electrophoresis liquid, constant pressure deposition voltage are 10V, and sedimentation time 10min, electrophoretic deposition takes out fibre bundle after the completion, in drying box Dry, temperature is 60 DEG C.
Step 5: the silicon carbide fibre beam containing SiC nano-powder prepared by step 4 is put into chemical vapor deposition stove In, with trichloromethyl silane (MTS) for presoma, hydrogen is reaction gas, and argon gas is diluent gas, and MTS leads in thermostatic tank It crosses Bubbling method to be introduced into gas in chemical vapor deposition stove after mixing in mixed gas tank, carries out the deposition of silicon carbide.Tool Body depositing operation is as follows：1150 DEG C, deposition pressure 7000Pa, sedimentation time 480min of depositing temperature, the flow of the MTS are 600g/h, the flow of argon gas is 3L/min, and the flow of hydrogen is 0.6L/min, after furnace cooling, that is, prepares nanometer silicon carbide Powder enhances SiCf/ SiC ceramic matrix composite material.
Comparative example 1
Remaining condition of the comparative example is same as Example 1, but the electrophoresis time used is 1min, the experimental results showed that, Only a smaller number of silicon carbide nanometer line is deposited on the surface of fiber, and there is no silicon carbide nanometer lines on most fiber.
Comparative example 2
Remaining condition of the comparative example is same as Example 1, but the deposition voltage used in electrophoretic deposition process for 90V.The experimental results showed that the deposition of silicon carbide nanometer line is concentrated mainly on the side of fiber, it is unevenly distributed and agglomeration is tight Weight.
Comparative example 3
Remaining condition of the comparative example is same as Example 1, but the silicon carbide in the electrophoresis liquid used in electrophoresis process The content of nano wire is only 0.005g/L.The result shows that the amount of the silicon carbide nanometer line adhered on fiber is well below implementation Example 1, the activeness and quietness effect that silicon carbide nanometer line plays also unobvious.
Comparative example 4
Remaining condition of the comparative example is same as Example 1, but in electrophoretic deposition working electrode to the distance to electrode 100mm, the results showed that, silicon carbide nanometer line only a small number of on fiber, and it is more serious to reunite.
Comparative example 5
Remaining condition of the comparative example is same as Example 3, but does not carry out deposition pyrolytic carbon before electrophoretic deposition process Technique, but electrophoretic deposition process is directly carried out after fiber braid degumming.As a result, it has been found that pyrolytic carbon and SiC nano-powder The effect toughening more single than SiC nano-powder of composite strengthening toughening it is better.
Performance test
SiC prepared by above-described embodiment and comparative examplefIt is tested for the property after/SiC ceramic matrix composite material is processed, gained Results of property is as shown in table 1.
1 SiC of tablef/ SiC ceramic matrix composite material performance test table
By the comparison of above-described embodiment and comparative example it is found that silicon carbide nanometer line activeness and quietness prepared by the present invention SiCf/ SiC ceramic matrix composite material has raising by a relatively large margin on bending strength, fracture toughness, tensile strength and elasticity modulus, But the raising in terms of density is not obvious；When especially silicon carbide nanometer line is as reinforcing material, the increased width of performance Degree is more notable.
Mechanics Performance Testing will be carried out after 1200 DEG C of oxidations in air prepared by above-described embodiment and comparative example, tied Fruit such as table 2.
2 SiC of tablefMechanical property in/SiC ceramic matrix composite material air after 1200 DEG C of oxidations
Pass through the comparison of embodiment and comparative example influence of mechanical property after 1200 DEG C of oxidations：It is prepared by inventing Uniform carburized silicon nanowires activeness and quietness SiCfThe antioxygenic property of/SiC ceramic matrix composite material is promoted it is obvious that in 1200 DEG C of oxygen After change, mechanical property has higher conservation rate.

Claims (10)

1. a kind of SiC of reinforcement containing nanometerfThe preparation method of/SiC ceramic matrix composite material, it is characterised in that：By the SiC containing boundary layer Fiber or SiC fiber braids, which are fixed on metal plate A or graphite cake B, forms working electrode, metallic plate C or graphite cake D conducts To electrode, by above-mentioned working electrode and electrode is placed in the electrophoresis liquid containing nanometer reinforcement, carries out electrophoretic deposition nanometer increasing Qiang Ti obtains electrophoretic deposition product, after the drying of electrophoretic deposition product, carries out CVI deposition SiC matrixes until material is fine and close, as The SiC of the reinforcement containing nanometerf/ SiC ceramic matrix composite material；
During the electrophoretic deposition, working electrode to distance 10mm~50mm to electrode, deposition voltage is 3V~50V, during deposition Between be 1min~30min；
The nanometer reinforcement is SiC nano-powder or silicon carbide nanometer line；
The electrophoresis liquid of the silicon carbide-containing nano powder includes SiC nano-powder, tetramethylammonium hydroxide, poly amic acid, water, A concentration of 0.5g/L~60.0g/L of the SiC nano-powder, a concentration of 0.1g/L~1.5g/L of tetramethylammonium hydroxide, A concentration of 0.1g/L~5.0g/L of poly amic acid；The pH value of the electrophoresis liquid of the silicon carbide-containing nano powder is 9~12；
The electrophoresis liquid of the silicon carbide-containing nano wire is made of silicon carbide nanometer line, phenolic resin, aluminum nitrate, isopropanol, described A concentration of 0.05g/L~1.0g/L of silicon carbide nanometer line, a concentration of 0.05g/L~1.0g/L of phenolic resin, aluminum nitrate A concentration of 0.005g/L~0.05g/L.
2. a kind of SiC of reinforcement containing nanometer according to claim 1fThe preparation method of/SiC ceramic matrix composite material, feature exist In：The electrophoresis liquid of the silicon carbide-containing nano wire is to add in silicon carbide nanometer line, phenolic resin, aluminum nitrate with mode is taken In isopropanol, stirring concussion 30min~120min in ultrasonic wave；In the electrophoresis liquid of the silicon carbide-containing nano wire, silicon carbide A concentration of 0.5g/L~1.0g/L of nano wire, a concentration of 0.5g/L~1.0g/L of phenolic resin, aluminum nitrate it is a concentration of 0.025g/L~0.05g/L.
3. a kind of SiC of reinforcement containing nanometer according to claim 1fThe preparation method of/SiC ceramic matrix composite material, feature exist In：The electrophoresis liquid of the silicon carbide-containing nano powder with taking the mode to be, by SiC nano-powder, tetramethylammonium hydroxide, poly- third Olefin(e) acid amine is added to the water, stirring concussion 30min~120min in ultrasonic wave；And n-butylamine is added in by the electricity of SiC nano-powder The pH value of liquid of swimming is adjusted to 9~10, in the electrophoresis liquid of the silicon carbide-containing nano powder, a concentration of 5g/L of SiC nano-powder~ A concentration of 0.5g/L~1.5g/L of 10g/L, tetramethylammonium hydroxide, a concentration of 1g/L~3g/L of poly amic acid.
4. a kind of SiC of reinforcement containing nanometer according to claim 1fThe preparation method of/SiC ceramic matrix composite material, feature exist In：The electrophoretic deposition process uses DC power supply, during the electrophoretic deposition, working electrode arrive to the distance of electrode be 10mm~ 30mm, deposition voltage are 15V~30V, and sedimentation time is 2min~10min.
5. a kind of SiC of reinforcement containing nanometer according to claim 1fThe preparation method of/SiC ceramic matrix composite material, feature exist In：The nanometer reinforcement is silicon carbide nanometer line.
6. a kind of SiC of reinforcement containing nanometer according to claim 1fThe preparation method of/SiC ceramic matrix composite material, feature exist In the SiC fibers or SiC fiber braids containing boundary layer are selected from the SiC fibers of the boundary layer containing PyC or SiC fibrages Part.
7. a kind of SiC of reinforcement containing nanometer according to claim 6fThe preparation method of/SiC ceramic matrix composite material, feature exist In the SiC fibers of the boundary layer containing PyC or the preparation method of SiC fiber braids are, by the way of chemical vapor deposition Deposition PyC boundary layers are carried out on SiC fibers after pretreatment or SiC fiber braids, deposit the technique item of PyC boundary layers Part is, using propylene as carbon-source gas, argon gas is protective gas, and depositing temperature is 780 DEG C~1100 DEG C, deposition pressure for 4000~ 8000Pa, sedimentation time are 120~480min, and the flow of propylene is 0.1L/min~1.0L/min, and the flow of argon gas is 0.5L/ Min~5.0L/min.
8. a kind of SiC of reinforcement containing nanometer according to claim 6fThe preparation method of/SiC ceramic matrix composite material, feature exist In the pretreatment of the SiC fibers or SiC fiber braids is, to SiC fibers or SiC fiber braids under protective atmosphere It is heat-treated, the temperature of the heat treatment is 800 DEG C~1100 DEG C, and time of heat treatment is 10min~60min, the guarantor It protects atmosphere and is selected from nitrogen or argon gas.
9. a kind of SiC of reinforcement containing nanometer according to claim 1fThe preparation method of/SiC ceramic matrix composite material, feature exist In the process conditions of the electrophoretic deposition product progress CVI deposition SiC matrixes of the drying are, using MTS as the forerunner of SiC matrix Body, hydrogen are carrier gas, and argon gas is diluent gas, and the flow of the MTS is 100~600g/h, and the flow of argon gas is 0.5L/min ~3.0L/min, the depositing temperature are 1000 DEG C~1250 DEG C, and deposition pressure is 4000Pa~8000Pa, and sedimentation time is 100min~480min.
10. a kind of SiC of reinforcement containing nanometer according to claim 9fThe preparation method of/SiC ceramic matrix composite material, feature It is, is first introduced into MTS, hydrogen, argon gas in chemical vapor deposition stove after mixing, then carries out the deposition of silicon carbide.
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CN111069726A (en) * 2018-10-19 2020-04-28 天津大学 Carbon-carbon composite material and metal brazing connection method based on electrophoretic deposition of SiC nanowires
CN111069726B (en) * 2018-10-19 2021-04-30 天津大学 Carbon-carbon composite material and metal brazing connection method based on electrophoretic deposition of SiC nanowires
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CN112408986A (en) * 2020-11-04 2021-02-26 南昌航空大学 Preparation method of SiC/SiC micro composite material with two-dimensional nano interface coating
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CN112876257A (en) * 2021-01-27 2021-06-01 中国核动力研究设计院 SiCfTwo-layer composite cladding tube made of/SiC composite material and preparation method thereof
CN112876257B (en) * 2021-01-27 2022-05-17 中国核动力研究设计院 SiCfTwo-layer composite cladding tube made of/SiC composite material and preparation method thereof

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