CN106187263B - The manufacturing method and C/C-SiC composite material component of C/C-SiC composite material component - Google Patents
The manufacturing method and C/C-SiC composite material component of C/C-SiC composite material component Download PDFInfo
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Abstract
The invention discloses a kind of manufacturing methods of C/C-SiC composite material component.The method of the present invention includes：Step 1, by carbon fiber powder and phenol-formaldehyde resin powder according to（3：7）~（7：3）Quality proportioning be sufficiently mixed；Step 2 carries out cold moudling to the obtained mixture of step 1, obtains biscuit；Step 3 successively carries out pre-oxidation treatment, carbonization treatment to the biscuit, obtains carbon base；Step 4 carries out reaction siliconising processing to the carbon base, obtains preliminary C/C-SiC composite material component；Step 5 prepares SiC coating on preliminary C/C-SiC composite material component surface, obtains final C/C-SiC composite material component.The invention also discloses a kind of C/C-SiC composite material components manufactured using the above method.Compared with prior art, the present invention can disposably obtain the C/C-SiC composite material component of near-net-shape, not need secondary operation substantially, and the manufacturing cycle is short, and manufacturing cost is low, and C/C-SiC composite material component obtained has excellent performance.
Description
Technical field
The present invention relates to a kind of manufacturing method of C/C-SiC composite material component and using the C/C- of this method manufacture
SiC ceramic matrix composite material component.
Background technique
C/C-SiC composite material, i.e. carbon fiber reinforced carbon and silicon carbide double matrix material, the material have density low, anti-
The advantages that oxidation susceptibility good, corrosion-resistant, excellent mechanical property and thermophysical property, be it is a kind of be able to satisfy 1650 DEG C use it is new
Type high-temperature structural material and functional material.Compared with traditional C/C composite material, due to being introduced in C/C-SiC composite material
SiC ceramic hard material not only effectively increases inoxidizability and coefficient of friction as matrix, but also significantly improves friction mill
Performance is damaged to the stability of extraneous surrounding medium (moisture, mould and greasy dirt etc.).
It is excellent mechanical behavior under high temperature, good thermal shock resistance as possessed by C/C-SiC composite material, highly thermally conductive
A series of excellent properties such as rate, low-expansion coefficient, good chemical stability, have been widely used in Aeronautics and Astronautics, army
The fields such as work, nuclear energy.The technique for preparing C/C-SiC composite material mature at present mainly have chemical vapor deposition, liquid Si infiltration,
Gas phase siliconising, ceramic precursor dipping-cracking and composite technology.The precast body of C/C-SiC composite material mainly have it is one-dimensional, two
Dimension, three peacekeeping multidimensional carbon fibre fabrics；The preparation process difference of C/C-SiC composite material, carbon base body and silicon carbide substrate contain
Amount is different.The available different types of composite material of the combination of different matrix and precast body meets specific use.
Since C/C-SiC composite material has good chemical stability and mechanical behavior under high temperature, can be used to prepare boat
Complex components used in the fields such as sky, space flight, military project, nuclear energy, such as the interphase heat exchanger of Estimation of Nuclear Hydrogen Production.It is such
Structure is complicated for component, size is larger, and structural intergrity requires height, according to two dimension, three-dimensional or multidimensional prefabricated carbon fiber
Body densifies, then long preparation period, preparation cost repeatedly through chemical vapor deposition or ceramic precursor dipping-cracking technology
It is high；More importantly, existing based on two dimension, three-dimensional or multidimensional carbon fiber precast body C/C-SiC composite material preparation process
It must be still machined after forming the material into, the component of required size and specification can be obtained, therefore, the portion more complex for structure
Part manufacture need to usually carry out a large amount of mechanical process to C/C-SiC composite board, and continuous carbon can be cut off by machining
Fiber causes the performance of material to damage；If causing the destruction of heat exchanger fin in addition, making a fault in process, need to report
Useless monolith C/C-SiC composite board, cost are higher.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and to provide a kind of C/C-SiC composite materials
The manufacturing method of component can disposably obtain the C/C-SiC composite material component of near-net-shape, not need secondary operation substantially,
Manufacturing cycle is short, and manufacturing cost is low, and C/C-SiC composite material component obtained has excellent performance.
The present invention specifically uses following technical scheme to solve above-mentioned technical problem：
A kind of manufacturing method of C/C-SiC composite material component, includes the following steps：
Step 1, by carbon fiber powder and phenol-formaldehyde resin powder according to（3：7）~（7：3）Quality proportioning be sufficiently mixed；
Step 2 carries out cold moudling to the obtained mixture of step 1, obtains biscuit；
Step 3 successively carries out pre-oxidation treatment, carbonization treatment to the biscuit, obtains carbon base；
Step 4 carries out reaction siliconising processing to the carbon base, obtains preliminary C/C-SiC composite material component；
Step 5 prepares SiC coating on preliminary C/C-SiC composite material component surface, and it is multiple to obtain final C/C-SiC
Condensation material component.
Preferably, carbon fiber powder and phenol-formaldehyde resin powder are sufficiently mixed using the method for ball milling mixing.
Preferably, the particle length of the carbon fiber powder is 100~500mm, and the particle size of the phenol-formaldehyde resin powder is
75~100mm.
Preferably, the treatment temperature of the pre-oxidation treatment is 230 ~ 280 oC.The work of further preferred pre-oxidation treatment
Skill condition is specific as follows：With 3 ~ 7oThe heating rate of C/h is warming up to 160 oC keeps the temperature 10 ~ 20h；Again with 8 ~ 12 oThe heating of C/h
Rate is warming up to 230 ~ 280 oC keeps the temperature 10 ~ 20h；With 20oThe rate of temperature fall of C/h cools down.
Preferably, the process conditions of the carbonization treatment are：It is warming up to 230 ~ 280 oC, heat preservation；It is continuously heating to 500 ~
700oC, heat preservation；It is further heated up to 1000oC, heat preservation；Cooling.The process conditions of further preferred carbonization treatment are：With 30 ~
80oThe heating rate of C/h is warming up to 230 ~ 280 oC, heat preservation；With 3 ~ 8oThe heating rate of C/h is warming up to 500~700oC, heat preservation；
Again with 30 ~ 80oThe heating rate of C/h is warming up to 1000oC, heat preservation；Cooling.
Preferably, reaction siliconising is carried out to the carbon base using liquid Si infiltration method to handle.
Preferably, SiC coating is prepared on preliminary C/C-SiC composite material component surface with vapor deposition method.
A kind of C/C-SiC composite material component is fabricated using any of the above technical solution the method.
Compared with prior art, technical solution of the present invention has the advantages that：
The present invention uses the mixture of carbon fiber powder and phenol-formaldehyde resin powder as raw material, and element is obtained in the way of cold moudling
The pore structure of base, gained biscuit is controllable, and the contraction distortion after carbonization is small, and craze and transfiguration is not easy in sintering process；Cooperation is corresponding
Cold pressing forming mould, can disposably obtain the C/C-SiC composite material component of near-net-shape, do not need cutting, grinding etc. two
Secondary machining, effectively reduces production cost, difficult using existing method particularly with nuclear energy heat exchanger, Aero-engine Bearing etc.
With the complexity of production or coarse scale structures component, it is of great significance；
With the prior art prepared by as C/C-SiC composite material, C/C-SiC composite material component produced by the present invention
With good chemical stability and mechanical behavior under high temperature, and due to not needing secondary machine, machining is avoided to material
Adverse effect caused by characteristic.
Specific embodiment
The shortcomings that for existing C/C-SiC composite material component manufacturing technology, the invention proposes a kind of completely new C/C-
The manufacturing method of SiC ceramic matrix composite material component uses the mixture of carbon fiber powder and phenol-formaldehyde resin powder as raw material, using being cold-pressed into
Type mode obtains biscuit, and the pore structure of gained biscuit is controllable, and the contraction distortion after carbonization is small, change not easy to crack in sintering process
Shape；Cooperate corresponding cold pressing forming mould, can disposably obtain the C/C-SiC composite material component of near-net-shape, not need to cut
The secondary machines such as cut, grind, effectively reducing production cost, and manufactured component have good chemical stability and
Mechanical behavior under high temperature.Specifically, the method for the present invention includes the following steps：
Step 1, by carbon fiber powder and phenol-formaldehyde resin powder according to（3：7）~（7：3）Quality proportioning be sufficiently mixed；
The present invention, as toughening phase, is because the modulus of carbon fiber is lower than the mould of silicon carbide ceramics phase using carbon fiber powder
Amount, meets the necessary condition of toughening.Meanwhile the length of fiber powder is greater than critical fibre length, can play increasing to a certain extent
Strong effect.The present invention is used as bonding agent using phenol-formaldehyde resin powder, volume contraction in carbonisation, and carbon fiber powder is when being carbonized
It can inhibit its contraction, reduce volume contraction ratio on the whole, reduce the risk of material cracks.
Wherein, the particle length of carbon fiber powder is preferably 100~500mm, and the particle size of the phenol-formaldehyde resin powder is preferred
For 75~100mm.
In order to be sufficiently mixed two kinds of materials, present invention preferably uses the methods of ball milling mixing, that is, utilize ball mill by carbon
Fiber powder and phenol-formaldehyde resin powder are sufficiently mixed.
Step 2 carries out cold moudling to the obtained mixture of step 1, obtains biscuit；
Corresponding molding die is designed according to the geomery of final component, is considered as producing in manufacturing process when designing mold
The shrinkage rates of product.In order to reduce following process as far as possible, the component of near-net-shape is obtained, it is preferred to use wearability, surface light
The better alloy mold of cleanliness.Molding machine can use hydraulic, air pressure or mechanical press according to actual needs.
Step 3 successively carries out pre-oxidation treatment, carbonization treatment to the biscuit, obtains carbon base；
Pre-oxidation treatment, the process conditions of carbonization treatment can refer to technological parameter in the prior art.The present invention is to pre- oxygen
Change processing, carbonization treatment technique be optimized.
The preferred process temperature of pre-oxidation treatment of the present invention is 230 ~ 280 oC.The work of further preferred pre-oxidation treatment
Skill condition is specific as follows：With 3 ~ 7oThe heating rate of C/h is warming up to 160 oC keeps the temperature 10 ~ 20h；Again with 8 ~ 12 oThe heating of C/h
Rate is warming up to 230 ~ 280 oC keeps the temperature 10 ~ 20h；With 20oThe rate of temperature fall of C/h cools down.
The preferred processing condition of carbonization treatment of the present invention is：It is warming up to 230 ~ 280 oC, heat preservation；It is continuously heating to 500 ~
700oC, heat preservation；It is further heated up to 1000oC, heat preservation；Cooling.The process conditions of further preferred carbonization treatment are：With 30 ~
80oThe heating rate of C/h is warming up to 230 ~ 280 oC, heat preservation；With 3 ~ 8oThe heating rate of C/h is warming up to 500~700oC, heat preservation；
Again with 30 ~ 80oThe heating rate of C/h is warming up to 1000oC, heat preservation；Cooling.
Step 4 carries out reaction siliconising processing to the carbon base, obtains preliminary C/C-SiC composite material component；
Reacting siliconising processing is existing mature technology, including liquid phase, gas phase, solid phase siliconising mode, and details are not described herein again.This
Invention preferred liquid phase siliconising processing method.
Step 5 prepares SiC coating on preliminary C/C-SiC composite material component surface, and it is multiple to obtain final C/C-SiC
Condensation material component；
The methods of existing physically or chemically vapor deposition, spraying can be used in the preparation of SiC coating, in order to more accurately control
The change in size of component processed, present invention preferably employs vapor deposition methods in preliminary C/C-SiC composite material component surface system
Standby SiC coating.
It does not need substantially further to be machined through C/C-SiC composite material component made from the above method, one
The aspect manufacturing cycle is short, and manufacturing cost is low；On the other hand, machining adverse effect brought to material property is avoided, therefore
The chemical stability and mechanical behavior under high temperature of component are more preferable.Present invention is particularly suitable for nuclear energy heat exchanger, Aero-engine Bearings etc.
The manufacture of the complexity produced or coarse scale structures component is difficult to using existing method.
For the ease of public understanding, technical solution of the present invention is described further below in conjunction with specific embodiment.
Embodiment 1
Carbon fiber powder and phenol-formaldehyde resin powder are pressed 40：60 mass ratio is uniformly mixed and mixture is made, wherein carbon fiber powder
Particle size be 100 ~ 500mm, the particle size of phenol-formaldehyde resin powder is 75-100mm；With ball mill turning with 100 turns/min
Fast ball milling 1h, it is ensured that each component is uniformly mixed.
The mixture of carbon fiber powder and phenol-formaldehyde resin powder is put into alloy mold, using four-column hydraulic press cold moudling.
Briquetting pressure in the present embodiment is 10MPa, dwell time 30min.
The biscuit of above-mentioned cold moudling is put into Muffle furnace and carries out pre-oxidation treatment.When pre-oxidation, with 7oC/h, heating
To 160oC keeps the temperature 10h；With 12oThe heating rate of C/h is from 160oC rises to 250oC keeps the temperature 10h；Then with 20oC/h cooling.
Biscuit Jing Guo pre-oxidation treatment is placed in carbide furnace, when carbonization, with 50oThe heating rate of C/h rises to
250oC keeps the temperature 2h；With 5oThe heating rate of C/h is from 250oC rises to 500oC keeps the temperature 2h；With 50oThe heating rate of C/h is from 500oC
Rise to 1000oC keeps the temperature 1h；With 100oC/h is from 1000oC is down to room temperature；
Carbon base Jing Guo carbonization treatment is placed in progress liquid Si infiltration processing in high-temperature vacuum sintering furnace, in the true of 50Pa
Under empty condition, it is warming up to 1700oC keeps the temperature 1h；Cooling.
It will treated that C/C-SiC composite material component is placed in chemical vapor deposition stove deposits by liquid Si infiltration
SiC coating, 1200oC is passed through trichloromethyl silane, hydrogen, reacts 1h；Cooling.
The C/C-SiC composite material component obtained to manufacture is tested for the property：Density of material is 1.89g/cm3, bending
Intensity is 142.8MPa, cubical contraction 27% after carbonization.
Embodiment 2：
Carbon fiber powder and phenol-formaldehyde resin powder are pressed 50：50 mass ratio is uniformly mixed and mixture is made, wherein carbon fiber powder
Particle size be 100 ~ 500mm, the particle size of phenol-formaldehyde resin powder is 75-100mm；With ball mill turning with 100 turns/min
Fast ball milling 1h, it is ensured that each component is uniformly mixed.
The mixture of carbon fiber powder and phenol-formaldehyde resin powder is put into alloy mold, using four-column hydraulic press cold moudling.
Pressure is 10MPa, dwell time 30min.
The biscuit of above-mentioned cold moudling is put into Muffle furnace and carries out pre-oxidation treatment.When pre-oxidation, with 5oC/h, heating
To 160oC keeps the temperature 10h；With 10oThe heating rate of C/h is from 160oC rises to 250oC keeps the temperature 10h；Then with 20oC/h cooling.
Biscuit Jing Guo pre-oxidation treatment is placed in carbide furnace, when carbonization, with 50oThe heating rate of C/h rises to
250oC keeps the temperature 2h；With 5oThe heating rate of C/h is from 250oC rises to 550oC keeps the temperature 2h；With 50oThe heating rate of C/h is from 550oC
Rise to 1000oC keeps the temperature 1h；With 100oC/h is from 1000oC is down to room temperature；
Carbon base Jing Guo carbonization treatment is placed in progress liquid Si infiltration processing in high-temperature vacuum sintering furnace, in the true of 50Pa
Under empty condition, it is warming up to 1700oC keeps the temperature 1h；Cooling.
It will treated that C/C-SiC composite material component is placed in chemical vapor deposition stove sinks by liquid Si infiltration
Product SiC coating, 1200oC is passed through trichloromethyl silane, hydrogen, reacts 1h；Cooling.
This C/C-SiC composite material component is tested for the property：The density of material is 1.93g/cm3, bending strength
For 167.2MPa, cubical contraction 21% after carbonization.
Embodiment 3：
Carbon fiber powder and phenol-formaldehyde resin powder are pressed 60：40 mass ratio is uniformly mixed and mixture is made, wherein carbon fiber powder
Particle size be 100 ~ 500mm, the particle size of phenol-formaldehyde resin powder is 75-100mm；With ball mill turning with 100 turns/min
Fast ball milling 1h, it is ensured that each component is uniformly mixed.
The mixture of carbon fiber powder and phenol-formaldehyde resin powder is put into alloy mold, using four-column hydraulic press cold moudling.
Pressure is 10MPa, dwell time 30min.
The biscuit of above-mentioned cold moudling is put into Muffle furnace and carries out pre-oxidation treatment.When pre-oxidation, with 6oC/h, heating
To 160oC keeps the temperature 10h；With 8oThe heating rate of C/h is from 160oC rises to 250oC keeps the temperature 10h；Then with 20oC/h cooling.
The biscuit of carbon fiber powder and phenol-formaldehyde resin powder Jing Guo pre-oxidation treatment is placed in carbide furnace, when carbonization, with
80oThe heating rate of C/h rises to 250oC keeps the temperature 2h；With 10oThe heating rate of C/h is from 250oC rises to 600oC keeps the temperature 2h；With
80oThe heating rate of C/h is from 600oC rises to 1000oC keeps the temperature 1h；With 100oC/h is from 1000oC is down to room temperature；
Carbon base Jing Guo carbonization treatment is placed in progress liquid Si infiltration processing in high-temperature vacuum sintering furnace, in the true of 50Pa
Under empty condition, it is warming up to 1700oC keeps the temperature 1h；Cooling.
It will treated that C/C-SiC composite material is placed in chemical vapor deposition stove deposits by liquid Si infiltration
SiC coating, 1200oC is passed through trichloromethyl silane, hydrogen, reacts 1h；Cooling.
This C/C-SiC composite material component is tested for the property：The density of material is 1.95g/cm3, bending strength
For 173.1MPa, cubical contraction 18% after carbonization.
Embodiment 4：
Carbon fiber powder and phenol-formaldehyde resin powder are pressed 70：30 mass ratio is uniformly mixed and mixture is made, wherein carbon fiber powder
Particle size be 100 ~ 500mm, the particle size of phenol-formaldehyde resin powder is 75 ~ 100mm；With ball mill turning with 100 turns/min
Fast ball milling 1h, it is ensured that each component is uniformly mixed.
The mixture of carbon fiber powder and phenol-formaldehyde resin powder is put into alloy mold, using four-column hydraulic press cold moudling.
Pressure is 10MPa, dwell time 30min.
The biscuit of above-mentioned cold moudling is put into Muffle furnace and carries out pre-oxidation treatment.When pre-oxidation, with 3oC/h, heating
To 160oC keeps the temperature 10h；With 10oThe heating rate of C/h is from 160oC rises to 250oC keeps the temperature 10h；Then with 20oC/h cooling.
The biscuit of carbon fiber powder and phenol-formaldehyde resin powder Jing Guo pre-oxidation treatment is placed in carbide furnace, when carbonization, with
30oThe heating rate of C/h rises to 250oC keeps the temperature 2h；With 5oThe heating rate of C/h is from 250oC rises to 700oC keeps the temperature 2h；With
50oThe heating rate of C/h is from 700oC rises to 1000oC keeps the temperature 1h；With 100oC/h is from 1000oC is down to room temperature；
Carbon base Jing Guo carbonization treatment is placed in progress liquid Si infiltration processing in high-temperature vacuum sintering furnace, in the true of 50Pa
Under empty condition, it is warming up to 1700oC keeps the temperature 1h；Cooling.
It will treated that C/C-SiC composite material component is placed in chemical vapor deposition stove sinks by liquid Si infiltration
Product SiC coating, 1200oC is passed through trichloromethyl silane, hydrogen, reacts 1h；Cooling.
This C/C-SiC composite material component is tested for the property：The density of material is 2.01g/cm3, bending strength
For 193.1MPa, cubical contraction 13% after carbonization.
According to above-described embodiment it is found that the density and bending of the C/C-SiC composite material component of the method for the present invention manufacture
Intensity is all satisfied the rigors of interphase heat exchanger.It can be seen that from aforementioned four embodiment, when carbon fiber powder and phenolic resin
The mass ratio of powder is 70:When 30, density of material and bending strength highest, volume contraction minimum.
Claims (10)
1. a kind of manufacturing method of C/C-SiC composite material component, which is characterized in that include the following steps：
Step 1, by carbon fiber powder and phenol-formaldehyde resin powder according to（3：7）~（7：3）Quality proportioning be sufficiently mixed；
Step 2 carries out cold moudling to the obtained mixture of step 1, obtains biscuit；
Step 3 successively carries out pre-oxidation treatment, carbonization treatment to the biscuit, obtains carbon base；
Step 4 carries out reaction siliconising processing to the carbon base, obtains preliminary C/C-SiC composite material component；
Step 5 prepares SiC coating on preliminary C/C-SiC composite material component surface, obtains final C/C-SiC composite wood
Expect component.
2. method as described in claim 1, which is characterized in that using the method for ball milling mixing by carbon fiber powder and phenol-formaldehyde resin powder
It is sufficiently mixed.
3. method as described in claim 1, which is characterized in that the particle length of the carbon fiber powder is 100~500mm, described
The particle size of phenol-formaldehyde resin powder is 75~100mm.
4. method as described in claim 1, which is characterized in that the treatment temperature of the pre-oxidation treatment is 230 ~ 280 oC。
5. such as claim 4 method, which is characterized in that the process conditions of the pre-oxidation treatment are specific as follows：With 3 ~ 7oC/h's
Heating rate is warming up to 160 oC keeps the temperature 10 ~ 20h；Again with 8 ~ 12 oThe heating rate of C/h is warming up to 230 ~ 280 oC, heat preservation 10 ~
20h；With 20oThe rate of temperature fall of C/h cools down.
6. method as described in claim 1, which is characterized in that the process conditions of the carbonization treatment are：It is warming up to 230 ~ 280oC, heat preservation；It is continuously heating to 500 ~ 700oC, heat preservation；It is further heated up to 1000oC, heat preservation；Cooling.
7. method as claimed in claim 6, which is characterized in that the process conditions of the carbonization treatment are specially：With 30 ~ 80oC/h
Heating rate be warming up to 230 ~ 280 oC, heat preservation；With 3 ~ 8oThe heating rate of C/h is warming up to 500~700oC, heat preservation；Again with
30~80oThe heating rate of C/h is warming up to 1000oC, heat preservation；Cooling.
8. method as described in claim 1, which is characterized in that carried out at reaction siliconising using liquid Si infiltration method to the carbon base
Reason.
9. method as described in claim 1, which is characterized in that using vapor deposition method in preliminary C/C-SiC composite material
Parts surface prepares SiC coating.
10. a kind of C/C-SiC composite material component, which is characterized in that manufactured using any one of claim 1~9 the method
It forms.
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| CN201610561827.9A CN106187263B (en) | 2016-07-18 | 2016-07-18 | The manufacturing method and C/C-SiC composite material component of C/C-SiC composite material component |
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