CN110483089A - A kind of density carbon/carbon composite and preparation method thereof - Google Patents
A kind of density carbon/carbon composite and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of density carbon/carbon composite and preparation method thereof.Described method includes following steps: using propylene as carbon source gas, carrying out density to carbon fiber substrate using CVD deposition, is heated up and deposited using gradient type, temperature range is 750-1100 DEG C；After the completion of density, matrix natural cooling；Organic solvent is uniformly mixed with resin, obtains dip compound；Under inert atmosphere, prefabricated carbon fiber is placed in dip compound impregnated three times-carbonize circular treatment；After the completion of processing, continues high temperature graphitization processing, obtain carbon/carbon composite.The method of the present invention prepares the carbon/carbon composite haveing excellent performance in conjunction with graphitization technique using multiple dipping-charing circular treatment.The method of the present invention prepares the carbon/carbon composite with high density, excellent mechanical performance in conjunction with graphitization technique using CVD deposition density, the dip compound containing PAA resin, multiple dipping-charing circular treatment.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of density carbon/carbon composite and preparation method thereof.
Background technique
Carbon/carbon composite (hereinafter referred to as C/C) is a kind of high temperature structural material, due to carbon/carbon composite
Component only has carbon, thus it has the advantages that such as charcoal and graphite material, and if its density is small, specific strength is high, the biography of ratio
Uniting, structural material is more superior, and (up to 2200 DEG C) its mechanical property mentions this composite material instead as the temperature rises
It is high.C/C composite is used widely on aerospace industry as superhigh temperature structural material.Density is reflection C/C
C/C composite that one of the important index of composite material superiority and inferiority, only density reache a certain level could obtain in engineering
To practical application.
Summary of the invention
The present invention provides a kind of preparation method of density carbon/carbon composite, and described method includes following steps:
(1) using propylene as carbon source gas, density is carried out to carbon fiber substrate using CVD deposition, is heated up and is deposited using gradient type, temperature
Spending range is 750-1100 DEG C；After the completion of CVD deposition density, by matrix natural cooling；
(2) after the completion of step (1), under inert atmosphere, the carbon fiber substrate is placed in and carries out impregnating-carbonizing in dip compound
Processing: dipping-charing process for the first time, 300-400 DEG C of dipping temperature, pressure 2-3MPa, dip time 3-6 hours, carbonization temperature
Constant temperature carbonizes 0.5-1 hours at 1000-1100 DEG C；For the first time after the completion of dipping-charing process, natural cooling cooling carries out second
Secondary dipping-charing process, 400-500 DEG C of dipping temperature, pressure 3-4MPa, dip time 3-6 hours, carbonization temperature 1100-
Constant temperature carbonizes 0.5-1 hours at 1200 DEG C；After the completion of second of dipping-charing process, natural cooling cooling carries out third time leaching
Stain-charing process, 500-600 DEG C of dipping temperature, pressure 3-4MPa, dip time 3-6 hours, 1100-1200 DEG C of carbonization temperature
Lower constant temperature carbonizes 1-2 hours；
It include organic solvent and resin in the dip compound；
(3) after the completion of step (2), continue high temperature graphitization processing, obtain carbon/carbon composite.
According to the technique and scheme of the present invention, the form of carbon fiber precast body described in step (1) is unlimited, and fiber skeleton can
Selected from least one of carbon cloth laminate, the perverse felt lamination of needle, the perverse felt mixing lamination of charcoal cloth-needle, charcoal felt etc..Wherein, the fibre
Tieing up percent by volume shared by Carbon fibe described in skeleton is 10-50%, such as 25-40%.
According to the technique and scheme of the present invention, in step (1), the diluent gas is nitrogen.
According to the technique and scheme of the present invention, in step (1), the atmosphere pressures in the deposition process are 2000-8000Pa,
It is preferred that 3000-7500 Pa.
According to the technique and scheme of the present invention, in step (1), the flow of the carbon source gas is 2.5-4.0m3/(m2H), excellent
Select 2.8-3.6m3/(m2·h)。
According to the technique and scheme of the present invention, in step (1), the gradient type heating deposition includes: that first stage temperature is
750-850 DEG C, handle 24-36h, atmosphere pressures 2500-3500Pa；Second stage temperature is 850-950 DEG C, handles 15-30h,
Atmosphere pressures 3500-5500Pa；Phase III temperature is 950-1100 DEG C, handles 24-36h, atmosphere pressures 6000-7500Pa.
According to the technique and scheme of the present invention, in step (2), the organic solvent is tetrahydrofuran, toluene or N, N- diformazan
Base formamide, the resin are PAA resin.Further, the mass volume ratio of the PAA resin and organic solvent is 1:8-
16, such as 1:10-13.
According to the technique and scheme of the present invention, in step (2), the heating rate of the dipping is 1-2 DEG C/min.
According to the technique and scheme of the present invention, in step (2), the heating rate of the charing is 1-2 DEG C/min.
Preferred technical solution according to the present invention, dipping-charing process for the first time described in step (2), dipping temperature 330-
Constant temperature carbonizes 0.5-1 hours at 380 DEG C, pressure 2-3MPa, dip time 3-4 hours, 1040-1080 DEG C of carbonization temperature.
Preferred technical solution according to the present invention, second of dipping-charing process, dipping temperature described in step (2)
Constant temperature carbonizes 1 hour at 420-470 DEG C, pressure 3.2-3.8MPa, dip time 4-6 hours, 1130-1180 DEG C of carbonization temperature.
Preferred technical solution according to the present invention, dipping-charing process for the third time described in step (2), dipping temperature
Constant temperature carbonizes 2 hours at 520-580 DEG C, pressure 3.2-3.8MPa, dip time 4-6 hours, 1130-1180 DEG C of carbonization temperature.
According to the technique and scheme of the present invention, the temperature of graphitization processing described in step (3) is 2200-2400 DEG C, processing
Time is 2-3 hours.
According to the technique and scheme of the present invention, the inert atmosphere is nitrogen, argon gas or helium.
The present invention also provides carbon/carbon composites prepared by the above method.
Beneficial effects of the present invention:
The method of the present invention uses CVD deposition density, the dip compound containing PAA resin, multiple dipping-charing circular treatment,
In conjunction with graphitization technique, the carbon/carbon composite with high density, excellent mechanical performance is prepared.Thermal gradient deposit density, with
And repeatedly in dipping-charing circulating treatment procedure, strict temperature control gradient and time, carbonization temperature and time and pressure,
The density of obtained carbon/carbon composite is high, and porosity is low, excellent in mechanical performance.
Raw material according to the present invention is easy to get, and simple process is with short production cycle, and production cost is low.
Specific embodiment
Further detailed description is done to technology of the invention below in conjunction with specific embodiment.It should be appreciated that following
Embodiment is merely illustrative the ground description and interpretation present invention, and is not necessarily to be construed as limiting the scope of the invention.All bases
In the range of the technology that above content of the present invention is realized is encompassed by the present invention is directed to protect.
Unless otherwise indicated, raw materials and reagents used in the following embodiment are commercial goods, or can be by
Perception method preparation.
Embodiment 1
The preparation method of carbon/carbon composite includes the following steps:
(1) using propylene as carbon source gas, the flow of carbon source gas is 3.0m3/(m2H), nitrogen is as diluent gas, using CVD
To carbon fiber substrate, (fiber skeleton is carbon cloth laminate to deposition, and Carbon fibe percent by volume is 25%) to carry out density, using gradient type
Heating deposition: first stage temperature is 780 DEG C, handles 30h, atmosphere pressures 3000Pa；Second stage temperature is 900 DEG C, processing
25h, atmosphere pressures 4500Pa；Phase III temperature is 1000 DEG C, handles 36h, atmosphere pressures 7500Pa；CVD deposition density is complete
Cheng Hou, by matrix natural cooling；
(2) n,N-Dimethylformamide is uniformly mixed with PAA resin according to volume mass 8:1(mL/g), obtains dipping mixing
Object；
(3) after the completion of step (1), under nitrogen atmosphere, prefabricated carbon fiber is placed in the dip compound of step (2) and is soaked
Stain-charing process: dipping-charing process for the first time, 350 DEG C of dipping temperature, pressure 2MPa, dip time 5 hours, carbonization temperature
Constant temperature carbonizes 1 hour at 1050 DEG C；For the first time after the completion of dipping-charing process, natural cooling cooling carries out second of dipping-charcoal
Change is handled, and constant temperature carbonizes 1 hour at 450 DEG C of dipping temperature, pressure 4MPa, dip time 6 hours, 1150 DEG C of carbonization temperature；The
After the completion of double-steeping-charing process, natural cooling cooling carries out third time dipping-charing process, 550 DEG C of dipping temperature, presses
Power 4MPa, constant temperature carbonizes 1 hour at dip time 5 hours, 1200 DEG C of carbonization temperature；
Wherein, the heating rate for impregnating and carbonizing is 1 DEG C/min；
(4) after the completion of step (3), continue high temperature graphitization processing, 2300 DEG C of processing times of temperature are 2.6 hours, are obtained
Carbon/carbon composite.
Embodiment 2
The preparation method of carbon/carbon composite includes the following steps:
(1) using propylene as carbon source gas, the flow of carbon source gas is 3.5m3/(m2H), nitrogen is as diluent gas, using CVD
To carbon fiber substrate, (fiber skeleton is the perverse felt mixing lamination of charcoal cloth-needle to deposition, and Carbon fibe percent by volume is 30%) to be increased
Close, use gradient type heating deposition: first stage temperature handles 36h, atmosphere pressures 3500Pa for 800 DEG C；Second stage temperature
It is 950 DEG C, handles 30h, atmosphere pressures 5500Pa；Phase III temperature is 1100 DEG C, is handled for 24 hours, atmosphere pressures 7000Pa；
After the completion of CVD deposition density, by matrix natural cooling；
(2) n,N-Dimethylformamide is uniformly mixed with PAA resin according to volume mass 12:1(mL/g), obtains dipping mixing
Object；
(3) after the completion of step (1), under nitrogen atmosphere, prefabricated carbon fiber is placed in dip compound impregnate-charing at
Reason: dipping-charing process for the first time, it is permanent at 400 DEG C of dipping temperature, pressure 2MPa, dip time 5 hours, 1050 DEG C of carbonization temperature
Temperature charing 2 hours；For the first time after the completion of dipping-charing process, natural cooling cooling carries out second of dipping-charing process, dipping
Constant temperature carbonizes 1 hour at 400 DEG C of temperature, pressure 4MPa, dip time 4.5 hours, 1150 DEG C of carbonization temperature；Second of dipping-
After the completion of charing process, natural cooling cooling carries out third time dipping-charing process, 500 DEG C of dipping temperature, pressure 4MPa, soaks
Constant temperature carbonizes 2 hours at the stain time 6 hours, 1100 DEG C of carbonization temperature；
Wherein, the heating rate for impregnating and carbonizing is 1 DEG C/min；
(4) after the completion of step (3), continue high temperature graphitization processing, 2300 DEG C of processing times of temperature are 2 hours, obtain charcoal/
Carbon composite.
Embodiment 3
The preparation method of carbon/carbon composite includes the following steps:
(1) using propylene as carbon source gas, the flow of carbon source gas is 2.5m3/(m2H), nitrogen is as diluent gas, using CVD
To carbon fiber substrate, (fiber skeleton is carbon cloth laminate to deposition, and Carbon fibe percent by volume is 25%) to carry out density, using gradient type
Heating deposition: first stage temperature is 820 DEG C, handles 36h, atmosphere pressures 3500Pa；Second stage temperature is 920 DEG C, processing
For 24 hours, atmosphere pressures 5000Pa；Phase III temperature is 1050 DEG C, handles 30h, atmosphere pressures 7000Pa；CVD deposition density is complete
Cheng Hou, by matrix natural cooling；
(2) n,N-Dimethylformamide is uniformly mixed with PAA resin according to volume mass 10:1(mL/g), obtains dipping mixing
Object；
(3) after the completion of step (1), under nitrogen atmosphere, prefabricated carbon fiber is placed in dip compound impregnate-charing at
Reason: dipping-charing process for the first time, it is permanent at 380 DEG C of dipping temperature, pressure 2MPa, dip time 6 hours, 1100 DEG C of carbonization temperature
Temperature charing 1.5 hours；For the first time after the completion of dipping-charing process, natural cooling cooling carries out second of dipping-charing process, leaching
Constant temperature carbonizes 1.5 hours at 500 DEG C of stain temperature, pressure 3.5MPa, dip time 5 hours, 1180 DEG C of carbonization temperature；Second of leaching
After the completion of stain-charing process, natural cooling cooling, progress third time dipping-charing process, 600 DEG C of dipping temperature, pressure
3.5MPa, constant temperature carbonizes 1.5 hours at dip time 6 hours, 1180 DEG C of carbonization temperature；
Wherein, the heating rate for impregnating and carbonizing is 1.5 DEG C/min；
(4) after the completion of step (3), continue high temperature graphitization processing, 2300 DEG C of processing times of temperature are 3 hours, obtain charcoal/
Carbon composite.
Test case
The mechanical property of carbon/carbon composite obtained by embodiment 1-3 is tested, test foundation includes: shearing test reference
84 standard of ASTM D2344-, compression verification is referring to 81 standard of ASTMC695-.
Test result is as shown in table 1.
Table 1.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Final densities (g/cm3) | 1.89 | 1.92 | 1.90 |
| Bending strength (MPa) | 145.82 | 157.36 | 152.34 |
| Shearing strength (MPa) | 17.20 | 18.45 | 16.92 |
| Vertical fibers direction compression strength (MPa) | 255.32 | 260.75 | 256.88 |
| Parallel fibers direction compression strength (MPa) | 101.48 | 105.74 | 102.56 |
More than, embodiments of the present invention are illustrated.But the present invention is not limited to above embodiment.It is all this
Within the spirit and principle of invention, any modification, equivalent substitution, improvement and etc. done should be included in protection model of the invention
Within enclosing.
Claims (10)
1. a kind of preparation method of density carbon/carbon composite, described method includes following steps:
(1) using propylene as carbon source gas, density is carried out to carbon fiber substrate using CVD deposition, is heated up and is deposited using gradient type, temperature
Spending range is 750-1100 DEG C；After the completion of CVD deposition density, by matrix natural cooling；
(2) after the completion of step (1), under inert atmosphere, the carbon fiber substrate is placed in and carries out impregnating-carbonizing in dip compound
Processing: dipping-charing process for the first time, 300-400 DEG C of dipping temperature, pressure 2-3MPa, dip time 3-6 hours, carbonization temperature
Constant temperature carbonizes 0.5-1 hours at 1000-1100 DEG C；For the first time after the completion of dipping-charing process, natural cooling cooling carries out second
Secondary dipping-charing process, 400-500 DEG C of dipping temperature, pressure 3-4MPa, dip time 3-6 hours, carbonization temperature 1100-
Constant temperature carbonizes 0.5-1 hours at 1200 DEG C；After the completion of second of dipping-charing process, natural cooling cooling carries out third time leaching
Stain-charing process, 500-600 DEG C of dipping temperature, pressure 3-4MPa, dip time 3-6 hours, 1100-1200 DEG C of carbonization temperature
Lower constant temperature carbonizes 1-2 hours；
It include organic solvent and resin in the dip compound；
(3) after the completion of step (2), continue high temperature graphitization processing, obtain carbon/carbon composite.
2. preparation method according to claim 1, which is characterized in that the fiber bone of carbon fiber substrate described in step (1)
Frame is selected from least one of carbon cloth laminate, the perverse felt lamination of needle, the perverse felt mixing lamination of charcoal cloth-needle, charcoal felt.
3. preparation method according to claim 1, which is characterized in that in step (1), the diluent gas is nitrogen.
4. preparation method according to claim 1, which is characterized in that the atmosphere pressure in step (1), in the deposition process
Power is 2000-8000Pa.
5. preparation method according to claim 1, which is characterized in that in step (1), the flow of the carbon source gas is 2.5-
4.0m3/(m2·h)。
6. preparation method according to claim 1-5, which is characterized in that in step (1), the gradient type heating
Deposition includes: that first stage temperature is 750-850 DEG C, handles 24-36h, atmosphere pressures 2500-3500Pa；Second stage temperature
It is 850-950 DEG C, handles 15-30h, atmosphere pressures 3500-5500Pa；Phase III temperature is 950-1100 DEG C, handles 24-
36h, atmosphere pressures 6000-7500Pa.
7. preparation method according to claim 1, which is characterized in that in step (2), the organic solvent is tetrahydro furan
It mutters, toluene or n,N-Dimethylformamide, the resin are PAA resin.
8. preparation method according to claim 1, which is characterized in that in step (2), the heating rate of the dipping is 1-
2 DEG C/min, the heating rate of the charing is 1-2 DEG C/min.
9. preparation method according to claim 1, which is characterized in that in step (2), at graphitization described in step (3)
The temperature of reason is 2200-2400 DEG C, and the processing time is 2-3 hours.
10. the carbon/carbon composite that any one of claim 1-9 the method is prepared.
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Application publication date: 20191122 |