CN105565837B - A kind of preparation method and applications of carbon ceramic composite material - Google Patents
A kind of preparation method and applications of carbon ceramic composite material Download PDFInfo
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D65/00—Parts or details
- F16D65/02—Braking members; Mounting thereof
- F16D65/12—Discs; Drums for disc brakes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D65/00—Parts or details
- F16D65/02—Braking members; Mounting thereof
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- C04B2235/77—Density
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D2200/00—Materials; Production methods therefor
- F16D2200/0034—Materials; Production methods therefor non-metallic
- F16D2200/0039—Ceramics
- F16D2200/0047—Ceramic composite, e.g. C/C composite infiltrated with Si or B, or ceramic matrix infiltrated with metal
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Abstract
The present invention relates to a kind of preparation method and applications of carbon ceramic composite material, in particular to the preparation method and applications of carbon ceramic composite material needed for a kind of high momentum delivery system is braked.Preparation method are as follows: with density be 1.2-1.5g/cm3C/C composite material be raw material；The raw material is placed in maceration extract I and is impregnated, after dipping, Pintsch process, repeated impregnations-Pintsch process operation are carried out under protective atmosphere, until obtaining density is 1.85-1.9g/cm3Carbon ceramic composite material；Then high-temperature process is carried out to gained carbon ceramic composite material, until the density of carbon ceramic composite material is down to 1.82-1.88g/cm3, obtain preform；Then preform is placed in maceration extract II, after the completion of dipping, is cracked under protective atmosphere, polished after cracking, repetitive cycling dipping-cracking-sanding operation is until obtaining density is 1.93-2.0g/cm3Carbon ceramic composite material finished product.
Description
Technical field
The present invention relates to a kind of preparation method and applications of carbon ceramic composite material, in particular to a kind of high momentum delivery system
The preparation method and applications of carbon ceramic composite material needed for controlling is dynamic.
Background technique
Currently, the brake disc on aircraft mainly has two class of C/C material and powdered metallurgical material.Powder metallurgy brake material
Material has the disadvantage that: being easily bonded under high temperature, weight is big, and heat fading is obvious, and elevated temperature strength decline, thermal shock resistance is poor, the longevity
It orders short etc..And C/C composite material brake disc is most developed early in the 1970s, with light weight under hot conditions,
The features such as high, high temperature resistant energy is strong, long service life can be carried, but since it is with oxidizable, the easy moisture absorption, hygrometric state coefficient of friction
It is low, the disadvantages of static friction coefficient is small.Meanwhile with the update of science and technology and aircraft, C/C brakes composite material increasingly
It is difficult to meet the needs of aircraft brake.It is therefore necessary to develop one kind to avoid disadvantages described above, the novel brake of high comprehensive performance
Hull composite material.
C/C-SiC composite material brake disc is a kind of high-performance brake material that twentieth century end grows up, due to tool
Have the following advantages: dry and wet state coefficient of friction is high and stablizes, running-in ability and excellent heat conductivity, and using load height, environmental suitability is strong
Deng.So C/C-SiC friction material is acknowledged as the brake material of new generation of 21st century great competitiveness.
CN102128225B discloses a kind of a kind of method that carbon pottery brake disc is prepared with reaction melting siliconising, and this method prepares carbon pottery and stops
Hull controllability is not strong, and component distributing is uneven, and the carbon pottery brake disc prepared, in braking process, abrasion loss is big, and curve is not
Surely, tail is stuck up greatly, and vibration is severe, influences other components of aircraft braking system.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of coefficient of friction is moderate, abrasion loss is few, curve is steady, vibration
The preparation method of small carbon ceramic composite material.
A kind of preparation method of carbon ceramic composite material of the present invention, includes the following steps:
Step 1
It is 1.2-1.5g/cm with density3C/C composite material be raw material；The raw material is placed in maceration extract I and is impregnated,
After dipping, Pintsch process, repeated impregnations-Pintsch process operation are carried out under protective atmosphere, until obtaining density is 1.85-
1.9g/cm3Carbon ceramic composite material；The maceration extract I is made of polymethyl silicane and styrene；The temperature of the Pintsch process
It is 1000-1300 DEG C；
Step 2
Under protective atmosphere, high-temperature process is carried out to carbon ceramic composite material obtained by step 1, until carbon ceramic composite material
Density is down to 1.82-1.88g/cm3, obtain preform；The temperature of the high-temperature process is 1450-1650 DEG C；
Step 3
Preform is placed in maceration extract II, after the completion of dipping, is cracked under protective atmosphere, is polished after cracking, weight
Multiple circulation dipping II-cracking of maceration extract-sanding operation is until obtaining density is 1.93-2.0g/cm3Carbon ceramic composite material finished product；
The maceration extract II is by silicon powder and polymethyl silicane 10-24:100 in mass ratio, preferably 10-20:100, further preferably
12:15-100 composition；The temperature of the cracking is 1200-1300 DEG C.
A kind of preparation method of carbon ceramic composite material of the present invention, density is 1.2-1.5g/cm in step 13C/C it is compound
Material is prepared by following proposal:
It is 0.5-0.55g/cm by density32.5D needle thorn Carbon fibe the whole network tire, be placed in cvd furnace, in protective atmosphere
Lower carry out chemical vapor deposition, until its density increases to 1.2-1.5g/cm3Afterwards, in 2300-2400 DEG C of high-temperature process 2-4h,
Obtaining the density is 1.2-1.5g/cm3C/C composite material；When the chemical vapor deposition, controlling air pressure in furnace is 2.0-
3.0KPa, temperature be 900~1000 DEG C, the volume ratio of control carbon-source gas and diluent gas is 1:5-1:1, and the carbon source is third
Alkene and/or natural gas.
A kind of preparation method of carbon ceramic composite material of the present invention, maceration extract I is by styrene and polymethyl silicane in step 1
Mass ratio, styrene: polymethyl silicane=10~20:100 composition；The average quality of the polymethyl silicane be 800~900,
Viscosity is 0.02~0.03cps.
It is 1.2-1.5g/cm by density in step 1 to promote gained end properties3C/C composite material be placed in
In maceration extract I, vacuum ultrasonic dipping is first carried out, is then carrying out pressurization ultrasonic immersing, after ultrasonic immersing of pressurizeing, in protective atmosphere
Under, it is carried out in 1000-1300 ° Pintsch process 2-3 hours (i.e. the time of single Pintsch process is 2-3 hours), then repeats to follow
Ring vacuum ultrasonic impregnates-pressurize the operation of ultrasonic immersing-Pintsch process until obtaining density is 1.85-1.9g/cm3Carbon pottery is compound
Material.
In industrial applications, in step 1, after Pintsch process, cools to room temperature with the furnace, take out sample afterwards, to sample table
After face is polished, repetitive cycling vacuum ultrasonic impregnates-pressurizes the operation of ultrasonic immersing-Pintsch process up to obtaining density and is
1.85‐1.9g/cm3Carbon ceramic composite material.
In step 1, when vacuum ultrasonic impregnates, the time of control single vacuum ultrasonic dipping is 2-3h, and control vacuum degree is
0.001MPa。
In step 1, pressurize ultrasonic immersing when, control single pressurization ultrasonic immersing time be 2-3h, control pressure be
2.5~3MPa.
In step 1, vacuum ultrasonic dipping and/or pressurization ultrasonic immersing control supersonic frequency are 80-100KHz.
In step 2, high-temperature process temperature is preferably 1550-1600 DEG C.
In step 2, when high-temperature process, first with 5-10 DEG C/min heating rate to after 1000 DEG C, then with 3-5 DEG C/min liter
Warm rate keeps the temperature 2-4h to after 1450 DEG C, then again with 2-3 DEG C/min heating rate to 1550 DEG C, keeps the temperature 2-3h, naturally drop
Temperature.
Protective atmosphere described in step 1 is selected from least one of nitrogen atmosphere, argon atmosphere.
Protective atmosphere described in step 2 is preferably argon atmosphere.
In order to promote the performance of final products, preform obtained by step 2 is impregnated into 30min in ethanol, it is then ultrasonic again
30min is cleaned, is taken out, after naturally dry to surface no liquid, is placed in baking oven in 60-80 DEG C of dry 1-3h.
In step 3, the granularity of silicon powder is 50-100nm, and purity is more than or equal to 97%, preferably greater than or equal to 99%.?
Heretofore described purity is quality purity.
In step 3, the dipping is vacuum impregnation, and control vacuum degree is less than or equal to 0.001MPa when vacuum impregnation.
In step 3, the protective atmosphere is selected from least one of nitrogen atmosphere, argon atmosphere.
In step 3, after the completion of dipping, under protective atmosphere, 180-250 DEG C of heat preservation 2- is first warming up to 5-10 DEG C/min
After 3h, then 5-10 DEG C/min is warming up to 450-600 DEG C of heat preservation 1-2h, is then warming up to 1000-1300 DEG C of heat preservation with 3-5 DEG C/min
1-2h completes primary cracking.
In step 1 and step 3, all polymethyl silicanes are prepared by following step；
Step A
Aluminium powder is added in sodium sand, under protective atmosphere, stirring obtains spare sodium sand；Al and Na in the spare sodium sand
Mass ratio is 1:12~1:15；The granularity of the aluminium powder is 30-50um, and the granularity of sodium sand is 0.5-10um；
Step B
By the molar ratio of Na and Si, Na:Si=2.5~1:2~1, which is matched, takes spare sodium sand and monomer；Under protective atmosphere, first
Sodium sand is fitted into reaction kettle, organic solvent is then added；Stirring, after being warming up to 70-85 DEG C, the list taken will be matched by dividing at least 2 times
Body instills in reaction kettle, and stirring carries out back flow reaction；Liquid after being reacted；The monomer is dichloro methyl silane；It is described organic
Solvent is selected from one of alkane, aromatic hydrocarbon, preferably toluene；Organic solvent and matching take the ratio between volume of monomer for 6:1~
8:1；
Step C
Under protective atmosphere, centrifugal treating is carried out to liquid after reaction obtained by step 2, centrifugation gained liquid is in protective atmosphere
It is lower to be handled through distillation, obtain polymethyl silicane.
Carbon ceramic composite material prepared by the present invention can be used with brake disc；It is used especially suitable for aeroplane brake discs.
Carbon ceramic composite material prepared by the present invention can also be used in brake disc needed for other high momentum delivery systems are braked.
Principle and advantage
Present invention employs PIP impregnating cracking technologies, the carbon pottery relative to existing reaction siliconising method (RMI) preparation at present
Brake disc, technique are more controllable.And the silicon carbide whisker granularity of PIP method preparation is 10nm or so, compared to the big crystal grain degree carbon of RMI preparation
SiClx is compared, and in friction process, can reduce the abrasion of the brake disc as caused by abrasive wear, the brake service life extends.Meanwhile
The carbon pottery brake disc of PIP method preparation, silicon carbide distribution is very uniform, and there is no the carbon pottery brake disc silicon carbide of CVI and RMI method preparation
The big problem of distribution gradient, friction curve is steady, with small vibration.
The present invention use precursor polymethyl silicane, polymethyl silicane high-temperature split product Silicon-rich, the addition of styrene, both
Supplemented with carbon source, make carbon silicon ratio 1:1, and improve the degree of cross linking of polymethyl silicane, increases ceramic yield, by 1550-1600
DEG C high-temperature process after, free silica with free carbon cmpletely react generate silicon carbide, without remaining free carbon and free silica
The braking quality of brake disc is influenced, ingredient and content are controllable, are convenient for industrialized production.
The present invention is by the density domination of carbon ceramic composite material obtained by step 1 between 1.85-1.9g/cm3, it is intended to very well
Control silicon carbide content.Silicon carbide is a kind of antifriction material, and content is too low and very few, can all influence the frictional property of brake disc
Energy.Carborundum content is excessively high, and brake disc coefficient of friction is very low, poor stop；Carborundum content is too low, and brake disc hardness is not
Enough, intolerant to abrasion, abrasion loss is big, and coefficient of friction is unstable, and the brake disc service life is short.Therefore, the carborundum content one of carbon pottery brake disc
As in 20%-40%.Therefore, in the present invention, 1.2-1.5g/cm is selected3C/C brake disc green body, ceramic to density is
1.85-1.9g/cm3, i.e. carborundum content can be very good the content of control silicon carbide between 22%-35%, in guarantee brake
Under the premise of the coefficient of friction of hull, the abrasion loss of brake disc is reduced well.
The present invention is mixed using nanoscale silicon powder and polymethyl silicane, is handled brake panel surface.Purpose is
Increase a certain amount of silicon in brake disc.Silicon increases the material that rubs as a kind of, and micro silicon has one to the coefficient of friction of carbon pottery brake disc
Quantitative raising, and not will increase the abrasion loss of brake disc substantially.In this patent, using polymethyl silicane, pass through Vaccum Permeating
The mode of stain introduces nanoscale silicon powder, is on the one hand to fill up the unsound defect in PIP method surface, improves the cause of brake panel surface
Density improves the thermal coefficient on surface；On the other hand, polymethyl silicane is silicon carbide in 1200 DEG C or so pyrolysis products and dissociates
Silicon, will not introduce cracking carbon, and the silicon carbide that cracks and silicon carbide before are same silicon carbide, there is preferable combine by force
Degree, combines silicon powder preferably with brake disc.
The carbon ceramic composite material of the method for the present invention preparation can be very good each component content and knot in control brake disc in a word
Structure distribution, coefficient of friction is high and stablizes, and abrasion loss is small, and without obvious vibration in brake process, brake cruve is steady, and anury is stuck up,
Fabrication cycle is short, preparation method is simply controllable, is suitble to industrialization production, special than being suitable for the high momentum delivery system systems such as aircraft
Brake disc needed for dynamic.
Detailed description of the invention
Attached drawing 1 is the pottery aeroplane brake discs sample of carbon prepared by embodiment 1.
Attached drawing 2 is the pottery aeroplane brake discs metallographic microscope of carbon prepared by embodiment 1.
Attached drawing 3 is the friction curve figure of the pottery aeroplane brake discs sample of carbon prepared by embodiment 1.
Attached drawing 4 is the XRD diagram of polymethyl silicane used in the embodiment of the present invention.
It can be seen that the macroscopic form and microstructure of finished product prepared by embodiment 1 from Fig. 1, Fig. 2.
It can be seen that from Fig. 3 friction curve figure in 7914rpm, the pressure of 196.19Kg, the mean force of 213.39Kg.cm
Under square, brake disc has a biggish coefficient of friction, and 0.34, and brake cruve is more steady, it is preferable that tail sticks up peak, illustrates that this brake disc has
There is excellent braking quality.
As can be seen from Figure 4: 2 θ=36.5 °, 60.1 °, 71.8 ° of diffraction maximum difference in the XRD spectra of polymethyl silicane
Belong to (111), (220), (311) crystal face diffraction of β-SiC, 2 θ=28.4,47.3,56.1 diffraction maximums belong to Si's respectively
(111), (220), (311) crystal face diffraction, while without apparent impurity diffraction maximum in XRD, it was demonstrated that polymethyl silicane is at 1200 DEG C
Lower pyrolysis product is β-SiC and silicon.
Specific embodiment:
In the present invention, the test condition of brake disc is 7900rpm in all embodiment and comparative examples, the pressure of 196Kg,
The average torque of 211Kg.cm, brake diagnostic test 20 times.
Embodiment 1
To be prepared in the embodiment of the present invention 1 carbon pottery aeroplane brake discs, it is raw materials used be density be 1.2-1.5g/cm3's
C/C composite material.Density is 1.2-1.5g/cm3C/C composite material the preparation method comprises the following steps:
Use density for 0.5-0.55g/cm32.5D needle thorn Carbon fibe the whole network tire, Carbon deposition to density be 1.3g/
cm3, under protective atmosphere, carry out 2300 DEG C of high-temperature process.Processing to obtain about 1.26g/cm by the dead size of aeroplane brake discs3
The C/C composite airplane brake disc green body of density.It is dilute with argon gas using propylene or natural gas as carbon source when carrying out Carbon deposition
Outgassing body, air pressure is 2.0-3.0KPa in control furnace when deposition, temperature is 900~1000 DEG C；When Carbon deposition, carbon-source gas with it is dilute
The volume ratio of outgassing body is 1:5-1:1.
Step 1
Configuration quality ratio, styrene: polymethyl silicane is the maceration extract of 20:100, by C/C composite airplane brake disc
Green body is put into metal impregnation tank, impregnates 1h, vacuum impregnation 2h using vacuum ultrasonic, and pressurize ultrasonic immersing 1h, impregnating by pressure 2h.
Maceration extract is released after the completion of dipping, and impregnated prefabricated component is put into graphite crucible and is fitted into vacuum sintering furnace, 1300 DEG C
Lower carry out Pintsch process keeps the temperature 3 hours, and overall process uses inert gas shielding.It has been sintered and has been down to room temperature, prefabricated component is subjected to table
It is repeated above-mentioned impregnation technology 6 times after the polishing of face, finally obtaining density is 1.85g/cm3Carbon pottery aeroplane brake discs prefabrication.
Vacuum ultrasonic impregnate when, control vacuum degree be less than 0.001MPa, pressurize ultrasonic immersing when, moulding pressure is
2.5MPa。
Step 3: carbon pottery brake disc high-temperature process.It is 1.85g/cm by density3Carbon pottery brake disc prefabrication carry out 1550
DEG C high-temperature process, obtaining density is 1.83g/cm3Carbon make pottery brake disc preform.
Step 4: pyrocarbon pottery brake disc preform surface treatment.Brake disc preform surface ash content is cleared up with ethyl alcohol
Completely, in mass ratio, silicon powder: polymethyl silicane 15:100 is configured to maceration extract, vacuum impregnation 2h, and dipping releases dipping after the completion
Impregnated preform is put into graphite crucible and is fitted into vacuum sintering furnace by liquid, and Pintsch process is carried out at 1300 DEG C, heat preservation
2 hours, overall process used inert gas shielding.It has been sintered and has been down to room temperature, repeated above-mentioned leaching after preform is carried out surface polishing
Stain technique 2-4 times, finally obtaining density is 1.95g/cm3Carbon pottery aeroplane brake discs.
Silicon powder is 50-100nm, and purity is more than or equal to 97%.
The carbon pottery brake disc component analysis of preparation:
Carborundum content: 32.8%
Silicone content: 2.5%
Cracking carbon content: 0%
The carbon pottery aeroplane brake discs braking quality of preparation is as follows:
Average friction coefficient: 0.34 average single material abrasion: 0.00104mm
Average single antithesis abrasion: 0.0014mm.
Comparative example 1, other conditions are consistent with embodiment 1, only high with polymethyl silicane vacuum impregnation in step 4
Temperature treated carbon is made pottery brake disc preform, and finally obtaining density is 1.96g/cm3Carbon make pottery aeroplane brake discs.
The carbon pottery brake disc component analysis of preparation:
Carborundum content: 34.4%
Silicone content: 1.3%
Cracking carbon content: 0%
The carbon pottery aeroplane brake discs braking quality of preparation is as follows:
Average friction coefficient: 0.233
Average single material abrasion: 0.0015mm
Average single antithesis abrasion: 0.0017mm
Comparative example 2, other conditions are consistent with embodiment 1, in step 4, only use mass ratio, styrene: poly- methyl
Silane is the carbon pottery brake disc preform after the maceration extract vacuum impregnation high-temperature process of 100:20, and finally obtaining density is 1.94g/
cm3Carbon make pottery aeroplane brake discs.
The carbon pottery brake disc component analysis of preparation:
Carborundum content: 32.7%
Silicone content: 1.1%
Cracking carbon content: 1.1%
The carbon pottery aeroplane brake discs braking quality of preparation is as follows:
Average friction coefficient: 0.193
Average single material abrasion: 0.0037mm
Average single antithesis abrasion: 0.0045mm.
Illustrated by embodiment 1, comparative example 1, comparative example 2, the content of silicon, cracking carbon is to brake disc friction in carbon pottery brake disc
The braking qualities such as coefficient, wear amount have a significant impact.
Embodiment 2
To be prepared in the embodiment of the present invention 2 carbon pottery aeroplane brake discs, it is raw materials used be density be 1.2-1.5g/cm3's
C/C composite material.Density is 1.2-1.5g/cm3C/C composite material the preparation method comprises the following steps:
Use density for 0.5-0.55g/cm32.5D needle thorn Carbon fibe the whole network tire, Carbon deposition to density be 1.55g/
cm3, under protective atmosphere, carry out 2300 DEG C of high-temperature process.Processing to obtain about 1.5g/cm by the dead size of aeroplane brake discs3It is close
The C/C composite airplane brake disc green body of degree.It is dilution with argon gas using propylene or natural gas as carbon source when carrying out Carbon deposition
Gas, air pressure is 2.0-3.0KPa in control furnace when deposition, temperature is 900~1000 DEG C；When Carbon deposition, carbon-source gas and dilution
The volume ratio of gas is 1:5-1:1.
Step 1
Configuration quality ratio, styrene: polymethyl silicane is the maceration extract of 15:100, by C/C composite airplane brake disc
Green body is put into metal impregnation tank, impregnates 1h, vacuum impregnation 2h using vacuum ultrasonic, and pressurize ultrasonic immersing 1h, impregnating by pressure 2h.
Maceration extract is released after the completion of dipping, and impregnated prefabricated component is put into graphite crucible and is fitted into vacuum sintering furnace, 1200 DEG C
Lower carry out Pintsch process keeps the temperature 2.5 hours, and overall process uses inert gas shielding.It has been sintered and has been down to room temperature, prefabricated component has been carried out
It is repeated above-mentioned impregnation technology 6 times after the polishing of surface, finally obtaining density is 1.9g/cm3Carbon pottery aeroplane brake discs prefabrication.
Vacuum ultrasonic impregnate when, control vacuum degree be less than 0.001MPa, pressurize ultrasonic immersing when, moulding pressure 3MPa.
Step 3: carbon pottery brake disc high-temperature process.It is 1.9g/cm by density3Carbon pottery brake disc prefabrication carry out 1500
DEG C high-temperature process, obtaining density is 1.88g/cm3Carbon make pottery brake disc preform.
Step 4: pyrocarbon pottery brake disc preform surface treatment.Brake disc preform surface ash content is cleared up with ethyl alcohol
Completely, in mass ratio, silicon powder: polymethyl silicane 12:100 is configured to maceration extract, vacuum impregnation 2h, and dipping releases dipping after the completion
Impregnated preform is put into graphite crucible and is fitted into vacuum sintering furnace by liquid, and Pintsch process is carried out at 1250 DEG C, heat preservation
2.5 hours, overall process used inert gas shielding.It has been sintered and has been down to room temperature, it will be repeatedly above-mentioned after preform progress surface polishing
Impregnation technology 2-4 times, finally obtaining density is 1.97g/cm3Carbon pottery aeroplane brake discs.
Silicon powder is 50-100nm, and purity is more than or equal to 97%.
The carbon pottery brake disc component analysis of preparation:
Carborundum content: 22.1%
Silicone content: 1.7%
Cracking carbon content: 0%
The carbon pottery aeroplane brake discs braking quality of preparation is as follows:
Average friction coefficient: 0.253 average single material abrasion: 0.0033mm
Average single antithesis abrasion: 0.0032mm.
Embodiment 3
To be prepared in embodiment 3 carbon pottery aeroplane brake discs, it is raw materials used be density be 1.2-1.5g/cm3C/C it is compound
Material.Density is 1.2-1.5g/cm3C/C composite material the preparation method comprises the following steps:
Use density for 0.5-0.55g/cm32.5D needle thorn Carbon fibe the whole network tire, Carbon deposition to density be 1.4g/
cm3, under protective atmosphere, carry out 2300 DEG C of high-temperature process.Processing to obtain about 1.37g/cm by the dead size of aeroplane brake discs3
The C/C composite airplane brake disc green body of density.It is dilute with argon gas using propylene or natural gas as carbon source when carrying out Carbon deposition
Outgassing body, air pressure is 2.0-3.0KPa in control furnace when deposition, temperature is 900~1000 DEG C；When Carbon deposition, carbon-source gas with it is dilute
The volume ratio of outgassing body is 1:5-1:1.
Step 1
Configuration quality ratio, styrene: polymethyl silicane is the maceration extract of 10:100, by C/C composite airplane brake disc
Green body is put into metal impregnation tank, impregnates 1h, vacuum impregnation 2h using vacuum ultrasonic, and pressurize ultrasonic immersing 1h, impregnating by pressure 2h.
Maceration extract is released after the completion of dipping, and impregnated prefabricated component is put into graphite crucible and is fitted into vacuum sintering furnace, 1000 DEG C
Lower carry out Pintsch process keeps the temperature 3 hours, and overall process uses inert gas shielding.It has been sintered and has been down to room temperature, prefabricated component is subjected to table
It is repeated above-mentioned impregnation technology 6 times after the polishing of face, finally obtaining density is 1.88g/cm3Carbon pottery aeroplane brake discs prefabrication.
Vacuum ultrasonic impregnate when, control vacuum degree be less than 0.001MPa, pressurize ultrasonic immersing when, moulding pressure is
2.6MPa。
Step 3: carbon pottery brake disc high-temperature process.It is 1.88g/cm by density3Carbon pottery brake disc prefabrication carry out 1600
DEG C high-temperature process, obtaining density is 1.84g/cm3Carbon make pottery brake disc preform.
Step 4: pyrocarbon pottery brake disc preform surface treatment.Brake disc preform surface ash content is cleared up with ethyl alcohol
Completely, in mass ratio, silicon powder: polymethyl silicane 14:100 is configured to maceration extract, vacuum impregnation 2h, and dipping releases dipping after the completion
Impregnated preform is put into graphite crucible and is fitted into vacuum sintering furnace by liquid, and Pintsch process is carried out at 1200 DEG C, heat preservation
3 hours, overall process used inert gas shielding.It has been sintered and has been down to room temperature, repeated above-mentioned leaching after preform is carried out surface polishing
Stain technique 2-4 times, finally obtaining density is 1.94g/cm3Carbon pottery aeroplane brake discs.
Silicon powder is 50-100nm, and purity is more than or equal to 97%.
The carbon pottery brake disc component analysis of preparation:
Carborundum content: 27.3%
Silicone content: 2%
Cracking carbon content: 0%
The carbon pottery aeroplane brake discs braking quality of preparation is as follows:
Average friction coefficient: 0.293 average single material abrasion: 0.0023mm
Average single antithesis abrasion: 0.0028mm.
Claims (9)
1. a kind of preparation method of carbon ceramic composite material, it is characterised in that include the following steps:
Step 1
It is 1.2-1.5g/cm with density3C/C composite material be raw material；The raw material is placed in maceration extract I and is impregnated, is impregnated
Afterwards, Pintsch process, repeated impregnations-Pintsch process operation are carried out under protective atmosphere, until obtaining density is 1.85-1.9g/cm3
Carbon ceramic composite material；The maceration extract I is made of polymethyl silicane and styrene；The temperature of the Pintsch process is 1000-
1300℃；
The maceration extract I is by styrene and polymethyl silicane mass ratio, styrene: polymethyl silicane=10~20:100 composition；
The average quality of the polymethyl silicane is 800~900, viscosity is 0.02~0.03cps；
Step 2
Under protective atmosphere, high-temperature process is carried out to carbon ceramic composite material obtained by step 1, until the density of carbon ceramic composite material
It is down to 1.82-1.88g/cm3, obtain preform；The temperature of the high-temperature process is 1450-1650 DEG C；
In step 2, when high-temperature process, first with 5-10 DEG C/min heating rate to after 1000 DEG C, then heated up speed with 3-5 DEG C/min
Rate keeps the temperature 2-4h to after 1450 DEG C, then again with 2-3 DEG C/min heating rate to 1550 DEG C -1600 DEG C, keeps the temperature 2-3h, natural
Cooling；
Step 3
Preform is placed in maceration extract II, after the completion of dipping, is cracked under protective atmosphere, is polished after cracking, repetition follows
Ring dipping II-cracking of maceration extract-sanding operation is until obtaining density is 1.93-2.0g/cm3Carbon ceramic composite material finished product；It is described
Maceration extract II is made of silicon powder and polymethyl silicane in mass ratio 10-24: 100；The temperature of the cracking is 1200-1300 DEG C；
Density is 1.2-1.5g/cm in step 13C/C composite material be to be prepared by following proposal:
It is 0.5-0.55g/cm by density32.5D needle thorn Carbon fibe the whole network tire, be placed in cvd furnace, under protective atmosphere into
Row chemical vapor deposition, until its density increases to 1.2-1.5g/cm3Afterwards, it in 2300-2400 DEG C of high-temperature process 2-4h, obtains
The density is 1.2-1.5g/cm3C/C composite material；When the chemical vapor deposition, controlling air pressure in furnace is 2.0-
3.0KPa, temperature be 900~1000 DEG C, the volume ratio of control carbon-source gas and diluent gas is 1: 5-1: 1, and the carbon source is third
Alkene and/or natural gas.
2. a kind of preparation method of carbon ceramic composite material according to claim 1, it is characterised in that:, will be close in step 1
Degree is 1.2-1.5g/cm3C/C composite material be placed in maceration extract I, first carry out vacuum ultrasonic dipping, then pressurize again
Ultrasonic immersing, pressurize ultrasonic immersing after, under protective atmosphere, in 1000-1300 DEG C progress Pintsch process 2-3 hours, then weigh
Multiple circulating vacuum ultrasonic immersing-pressurization ultrasonic immersing-Pintsch process operation is until obtaining density is 1.85-1.9g/cm3Carbon pottery
Composite material.
3. a kind of preparation method of carbon ceramic composite material according to claim 2, it is characterised in that: in step 1, vacuum
When ultrasonic immersing, the time of control single vacuum ultrasonic dipping is 2-3h, and control vacuum degree is 0.001MPa；In step 1, add
When pressing ultrasonic immersing, the time of control single pressurization ultrasonic immersing is 2-3h, and control pressure is 2.5~3MPa.
4. a kind of preparation method of carbon ceramic composite material according to claim 1, it is characterised in that:
In step 1, vacuum ultrasonic dipping and/or pressurization ultrasonic immersing control supersonic frequency are 80-100KHz；
In step 2, high-temperature process temperature is 1550-1600 DEG C.
5. a kind of preparation method of carbon ceramic composite material according to claim 1, it is characterised in that:
In step 3, the granularity of silicon powder is 50-100nm, and purity is more than or equal to 97%；
In step 3, the dipping is vacuum impregnation, and control vacuum degree is less than or equal to 0.001MPa when vacuum impregnation；
In step 3, the protective atmosphere is selected from least one of nitrogen atmosphere, argon atmosphere.
6. a kind of preparation method of carbon ceramic composite material according to claim 5, it is characterised in that:
In step 3, after the completion of dipping, under protective atmosphere, after being first warming up to 180-250 DEG C of heat preservation 2-3h with 5-10 DEG C/min,
5-10 DEG C again/min is warming up to 450-600 DEG C of heat preservation 1-2h, is then warming up to 1000-1300 DEG C of heat preservation 1-2h with 3-5 DEG C/min,
Complete primary cracking.
7. a kind of preparation method of carbon ceramic composite material according to claim 1, it is characterised in that:
In step 1 and step 3, all polymethyl silicanes are prepared by following step；
Step A
Aluminium powder is added in sodium sand, under protective atmosphere, stirring obtains spare sodium sand；The quality of Al and Na in the spare sodium sand
Than for 1:12~1:15；The granularity of the aluminium powder is 30-50um, and the granularity of sodium sand is 0.5-10um；
Step B
By the molar ratio of Na and Si, Na:Si=2.5~1:2~1, which is matched, takes spare sodium sand and monomer；Under protective atmosphere, first by sodium
Sand is fitted into reaction kettle, and organic solvent is then added；Stirring, after being warming up to 70-85 DEG C, dividing at least 2 times will drip with the monomer taken
Enter in reaction kettle, stir, carries out back flow reaction；Liquid after being reacted；The monomer is dichloro methyl silane；The organic solvent
Selected from one of alkane, aromatic hydrocarbon；Organic solvent and matching takes the ratio between volume of monomer for 6:1~8:1；
Step C
Under protective atmosphere, centrifugal treating is carried out to liquid after reaction obtained by step B, centrifugation gained liquid is under protective atmosphere through steaming
Processing is evaporated, polymethyl silicane is obtained.
8. a kind of application of the carbon ceramic composite material as prepared by claim 1-7 any one；It is characterized by: prepared carbon
The application of ceramic composite material includes being used as brake disc to use.
9. a kind of application of carbon ceramic composite material according to claim 8；It is characterized by: the carbon ceramic composite material
It is used using including being used as aeroplane brake discs.
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| CN105967714A (en) * | 2016-05-23 | 2016-09-28 | 苏州思创源博电子科技有限公司 | Preparation method of composite carbon pottery material |
| CN106090081A (en) * | 2016-06-18 | 2016-11-09 | 苏州思创源博电子科技有限公司 | A kind of preparation method of composite carbon ceramic material brake disc |
| CN106740136B (en) * | 2016-11-30 | 2019-04-23 | 北京天宜上佳高新材料股份有限公司 | A kind of production technology of carbon ceramic material and the slide plate as made from the material |
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| CN108558422B (en) * | 2018-01-12 | 2021-11-30 | 哈尔滨工业大学 | Preparation method of three-dimensional carbon fiber toughened ultrahigh-temperature ceramic matrix composite with high breaking power |
| CN109020595A (en) * | 2018-09-20 | 2018-12-18 | 湖南博望碳陶有限公司 | A kind of preparation method and applications of aluminium carbon ceramic composite material |
| CN109824376B (en) * | 2019-04-02 | 2020-03-17 | 安徽弘昌新材料有限公司 | High-performance carbon-ceramic friction welding stirring head and preparation method thereof |
| CN110372389B (en) * | 2019-07-30 | 2021-12-28 | 湖南博望碳陶有限公司 | Preparation method of carbon-ceramic automobile brake disc |
| CN111892416A (en) * | 2020-07-27 | 2020-11-06 | 贵阳天龙摩擦材料有限公司 | Preparation method of carbon-ceramic brake disc |
| CN112110741B (en) * | 2020-08-28 | 2022-04-22 | 湖南东映碳材料科技有限公司 | Preparation method of high-thermal-conductivity C/C-SiC composite material |
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