CN110156485A - A kind of method of short cycle, low cost preparation high-performance carbon/carbon compound material - Google Patents
A kind of method of short cycle, low cost preparation high-performance carbon/carbon compound material Download PDFInfo
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Abstract
The invention discloses a kind of short cycles, the method for low cost preparation high-performance carbon/carbon compound material, belong to carbon fibre composite preparation technical field.This method, which uses, is electrically coupled chemical vapor deposition process (E-CVI) and liquid impregnation-carbonization technique (PIC) combination process preparation high-performance C/C composite material.Prepared high-performance, high density C/C composite density are up to 1.8~1.9g/cm3, manufacturing cycle is only 400~500 hours, and compared with traditional isothermal CVI technique, manufacturing cycle shortens 30~50%, and cost reduces about 1/2.Intermediate density C/C composite material (1.45~1.65g/cm prepared by the present invention3), commercial market demand can be met, manufacturing cycle is only 200~300 hours, and cost is only the 1/4~1/3 of isothermal CVI technique preparation cost.
Description
Technical field
The present invention relates to carbon fibre composite preparation technical fields, and in particular to a kind of short cycle, low cost preparation are high
The method of performance carbon/carbon compound material.
Background technique
Carbon/carbon compound material (C/C composite material) is used as a kind of advanced composite material, has both structural material and functional material
Double grading.It has high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, endurance, creep resistant, low-density and expansion system
Count a series of excellent properties such as small.Currently, having been widely used for aerospace field.Such as rocket tube larynx lining, fly
Machine brake disc, skid of magnetic suspension train plate etc..
The main preparation process of C/C composite material includes liquid impregnation cracking process (PIC technique) and chemical vapor infiltration
(CVI technique).Wherein liquid impregnation cracking process mainly uses pitch or resin to pass through impregnating by pressure repeatedly, carbonization for presoma
It is prepared with the processes such as high-temperature heat treatment.There are distinct disadvantage, i.e. precast body needs to soak repeatedly in precursor solution for this method
It stain and is carbonized in inert atmosphere, and repeatedly recycles dipping and not only damage fiber but also since the contraction of resin carbon matrix can be led
Cause final products delamination.CVI technique is a kind of special side to grow up on the basis of chemical vapor deposition (CVD) method
Method is: carbon fiber precast body is placed in cvd furnace using the common practices that CVI method prepares C/C composite material, gaseous carbon
Hydrogen compound is entered inside precast body by the modes such as spreading, flowing, and pyrolytic reaction occurs at a certain temperature, generates pyrolytic carbon
And fiber surface is deposited on coating form.Isothermal chemical vapor infiltration (ICVI) technique is the improvement to traditional CVI technique, is handle
Carbon fiber precast body is placed in isothermal chemical vapor deposition stove, and hydro carbons organic gas is passed through reaction zone, in certain pressure and
At a temperature of, make these gases that a series of chemical reaction occur, ultimately produces pyrocarbon in the hole of carbon fiber precast body
In.The shortcoming of isothermal CVI technique is to be difficult to prepare the highdensity C/C composite material of large scale, furthermore preparation process week
Phase is long and expensive.Such as preparing density is 1.60-1.70g/cm3C/C composite material about need 800~1000 hours, sink
It needs to open material surface hole by being repeatedly machined during product.
Therefore, the mechanical property of C/C composite material how is improved, material manufacturing cycle is shortened, reducing preparation cost becomes
Urgent problem.
Summary of the invention:
The purpose of the present invention is to provide a kind of short cycles, the method for low cost preparation high-performance carbon/carbon compound material, adopt
Electricity consumption coupling chemistry gas phase cementation process (Electromagnetic coupling chemical vapor infiltration,
E-CVI) the side combined with liquid impregnation-carbonization (precursor impregnation carbonization, PIC) technique
Method prepares high-performance C/C composite material, and short preparation period is at low cost.
To achieve the above object, the technical solution adopted in the present invention is as follows:
A kind of method of short cycle, low cost preparation high-performance carbon/carbon compound material, this method are using E-CVI technique
Preparation C/C composite material is combined with PIC technique, this method comprises the following steps:
(1) preparation of boundary layer:
Carbon fiber precast body is placed in ICVI cvd furnace, using isothermal chemical vapor infiltration (Isothermal chemical
Vapor infiltration, ICVI) technique preparation pyrolysis carbon boundary layer, 0.3~2 μm of interfacial layer thickness；
(2) low-density C/C composite material is prepared using E-CVI；
(3) high-performance, high density C/C composite material are prepared using PIC technique:
In above-mentioned steps (1), the carbon fiber precast body uses 2D needling structure, 2.5D braiding structure, 3D braiding structure
Or puncturing structure is carefully compiled, wherein it is the most typical with 2D needling structure, generally using one layer of 12K (or 1K, 3K, 6K) PANCF without latitude
Cloth replaces laying with one layer of 12K PANCF net tire, and laminated cloth is 0/90 ° of laying, and 1.X+1.Y mode continuous needle forms.
In above-mentioned steps (1), the isothermal chemical vapor infiltration technological parameter are as follows: with Ar or N in unstrpped gas2For dilution
Gas, 0.01~0.5m of diluting gas flow3/ h, using liquefied natural gas, methane or propane as carbon-source gas, carbon-source gas flow
0.01~0.5m3/h；700~1100 DEG C of depositing temperature, sedimentation time 3-10h.
In above-mentioned steps (2), the process of the E-CVI are as follows: the sample with interfacial TCO layer prepared by step (1) is placed in band
Have in the chemical vapor deposition stove of water-cooling wall and direct-electrifying heating, fiber peripheral generate electromagnetic field, it is heat-insulated due to precast body
And the effect of outer gas stream and water-cooling wall, formation temperature gradient in precast body occur so that deposition is preferential at center, and by
It is gradually elapsed to two sides, reaction gas realizes fast deposition under the interaction of electromagnetic field, temperature field and fluid field.
In above-mentioned steps (2), during the E-CVI, with Ar or N2For diluent gas, diluting gas flow 0.01~
0.5m3/ h, using liquefied natural gas, methane or propane as carbon-source gas, 0.01~0.5m of carbon-source gas flow3/h；Depositing temperature
300~1100 DEG C, sedimentation time 5-50h.
Low-density C/C composite material prepared by above-mentioned steps (2), matrix center part are fine and close pyrolytic carbon layer, outside
Side is loose pyrolytic carbon layer, and material global density is controlled in 0.8~1.6g/cm3Between.
In above-mentioned steps (3), the process of the PIC technique are as follows: be placed in low-density C/C composite material obtained by step (2)
In vacuum pressure container, resin is impregnated into matrix using vacuum environment, which is known as vacuum-pressure dipping process；Through
After vacuum-pressure dipping process, then low temperature drying crosslinking curing and Pintsch process carbonisation are carried out, it is compound to obtain intermediate C/C
Material repeats vacuum-pressure dipping, low temperature drying crosslinking curing and Pintsch process carbonisation 5~15 times, finally
High density, high-performance C/C composite material are obtained, density domination is in 1.8~1.9g/cm3。
In the PIC technical process, need to carry out matrix when the rate of body weight gain of the intermediate C/C composite material≤3%
Machining or high temperature graphitization processing；0.5~2mm of the machining range scale, the high temperature graphitization processing are
Refer to and C/C composite material is handled into 1~2h under the conditions of 1800~2800 DEG C of temperature.
In the PIC technical process, resin used can be existing of dipping when being used to prepare C/C composite material
What resin, currently preferred resin are furane resins or phenolic resin.
In the PIC technical process, carries out vacuum-pressure dipping, low temperature drying crosslinking curing and Pintsch process and be carbonized
Journey specifically: firstly, resin is introduced into material internal using vacuum environment, vacuum degree≤- 0.1MPa keeps 1-3h；Then,
It is passed through Ar or N2And it is forced into 2~6MPa, keep 1-5h；Subsequently, 120-180 DEG C of crosslinking curing 5-10h；Finally, carbonization is split
Solution: 900 DEG C~1200 DEG C of carburizing temperature, carbonization time 8~15 hours.
The beneficial effects of the present invention are:
(1) present invention combines E-CVI, CVI and PIC technique, and preparing with density is 1.8~1.9g/cm3Between C/
C composite.E-CVI and CVI deposition process does not damage carbon fiber and the pyrolytic carbon boundary strength prepared is moderate.PIC technique
Further densification is so that material has 1%~2% porosity.Low porosity is but also resin carbon is closely tied with pyrolytic carbon
The conduction for being conducive to power is closed, the mechanical property of material is improved.
(2) present invention compared with conventional preparation techniques, prepared high-performance, high density C/C composite material (1.8~
1.9g/cm3), military markets demand can be met, manufacturing cycle is only 400~500 hours, and manufacturing cycle shortens 50%, cost
Only the 1/3 of CVI technique preparation cost.
(3) intermediate density C/C composite material (1.45~1.65g/cm prepared by the present invention3), commercial market can be met
Demand, manufacturing cycle are only 200~300 hours, and cost is only the 1/5 of CVI technique preparation cost.
(4) present invention is short cycle, the low cost preparation method of high-performance carbon/carbon compound material (C/C composite material), should
The implementation of method can expand such composite material aerospace, nuclear industry, electronics industry, Industry Furnace, auto industry into
Row application.
Detailed description of the invention
Fig. 1 is high-performance of the present invention, high density C/C composite material preparation flow.
Fig. 2 is 1 micro-structure diagram of embodiment；Wherein: (a) and (b) is the view for amplifying different multiples.
Fig. 3 is that embodiment 2 stretches and bending strength curve；Wherein: (a) tensile strength；(b) bending strength.
Specific embodiment
The present invention will be further described combined with specific embodiments below.
The present invention is the short cycle of high-performance carbon/carbon compound material (C/C composite material), low cost preparation method,
Preparation process is as follows:
(1) preparation of boundary layer
Using CVI technique, carbon fiber precast body is placed in ICVI furnace to the preparation for carrying out boundary layer, interfacial layer thickness range
0.3~2 μm.
(2) prepared by low-density C/C composite material
Using E-CVI technique, the carbon fiber precast body containing interfacial TCO layer is placed in the E-CVI furnace with water-cooling wall and is deposited
Pyrocarbon matrix, obtains low-density C/C composite material, and global density is controlled in 0.8~1.6g/cm3Between；
(3) preparation of high-performance, high density C/C composite material
Using PIC technique, step 2 gained low-density C/C composite material is placed in vacuum pressure container, vacuum ring is utilized
Resin is introduced into step 2 resulting materials matrix by border, by vacuum-pressure dipping, low temperature drying crosslinking curing, Pintsch process
C/C composite material is obtained after three steps that are carbonized, and the iterative cycles above process 5~15 times, finally obtains high density, high-performance C/
C composite, density domination is in 1.8~1.9g/cm3。
In above-mentioned steps 1,2D needling structure, 2.5D braiding structure, 3D braiding structure is can be used in the carbon fiber precast body
Or puncturing structure is carefully compiled, wherein it is the most typical with 2D needling structure, generally using one layer of 12K (or 1K, 3K, 6K) PANCF without latitude
Cloth replaces laying with one layer of 12K PANCF net tire, and laminated cloth is 0/90 ° of laying, and 1.X+1.Y mode continuous needle forms.
In above-mentioned steps 1, the fiber in the carbon fiber precast body can be using the carbon fiber for being any trade mark.
In above-mentioned steps 1, the ICVI technological parameter: with Ar or N in unstrpped gas2For diluent gas, diluent gas
0.01~0.5m of flow3/ h, using liquefied natural gas, methane or propane as carbon-source gas, 0.01~0.5m of carbon-source gas flow3/h；
700~1100 DEG C of depositing temperature, sedimentation time 3-10h.
In above-mentioned steps 2, the E-CVI working principle: being placed in direct-electrifying in the furnace with water-cooling wall for component and heat,
Fiber peripheral generates electromagnetic field, due to the heat-insulated and outer gas stream of precast body and the effect of water-cooling wall, formation temperature in precast body
Gradient occurs at center so that deposition is preferential, and gradually elapses to two sides, and reaction gas is in electromagnetic field, temperature field and stream
Fast deposition is realized under the interaction of body field.
In above-mentioned steps 2, the preparation process technological parameter of the low-density C/C composite material: with Ar or N2For dilution
Gas, 0.01~0.5m of flow3/ h, using liquefied natural gas, methane or propane as carbon-source gas, 0.01~0.5m of flow3/h；It is heavy
300~1100 DEG C of accumulated temperature degree, sedimentation time 5-50h.
In above-mentioned steps 3, selected resin be can be for making in the preparation process of the high density C/C composite material
Existing any resin of dipping when standby C/C composite material, currently preferred resin are furane resins or phenolic resin.
In above-mentioned steps 3, the PIC impregnating cracking technology process are as follows: resin is introduced by the first step using vacuum environment
Material internal, vacuum level requirements≤- 0.1MPa keep 1-3h to be then passed through Ar or N2And it is forced into 2~6MPa, keep 1-
5h；Third step, 120-180 DEG C of crosslinking curing 5-10h；Finally, carbonization cracking, 900 DEG C~1200 DEG C of carburizing temperature, carbonization time
8~15 hours.
In above-mentioned steps 3, the PIC impregnating cracking technology need to recycle repeatedly the process, until density reaches required value and is
Only.Need to carry out matrix machining or high temperature graphitization processing when the rate of body weight gain of intermediate C/C composite material≤3%,
It is recycled for the process.Wherein, machining 0.5~2mm of range scale, high temperature graphitization heat-treatment temperature range 2000~
2800 DEG C, 1~2h of time.
Embodiment 1:
By taking 400 × 100 × 15mm as an example, density 0.5g/cm32D Nomex；Pyrolytic carbon circle is prepared using ICVI technique
Surface layer, 900 DEG C of temperature, argon flow 0.2m3/ h, propane 0.15m3/ h, sedimentation time 5 hours；It is prepared using E-CVI technique low
Density C/C composite material, 700~1000 DEG C of temperature, argon flow 0.2m3/ h, propane 0.15m3/ h, sedimentation time 20 hours, system
Standby density of material 1.65g/cm3；High-performance, the preparation of high density C/C composite material are carried out using PIC technique, soaked by 8 periods
Stain cracking, by 2 times 2000 DEG C, 2h high-temperature heat treatment, infiltration pyrolysis specific process parameter are as follows: vacuum degree -0.1MPa, dipping pressure
Power 5MPa, 170 DEG C of solidification temperature, 1000 DEG C of cracking temperature of carbonization, heat preservation 1h, material final densities 1.90g/cm3, material always makes
Standby 350 hours periods.Fig. 2 is the micro-structure diagram for preparing C/C composite material.
Embodiment 2:
By taking 400 × 100 × 25mm as an example, density 0.5g/cm32D Nomex；Pyrolytic carbon circle is prepared using ICVI technique
Surface layer, 900 DEG C of temperature, argon flow 0.2m3/ h, propane 0.15m3/ h, sedimentation time 5 hours；It is prepared using E-CVI technique low
Density C/C composite material, 700~1000 DEG C of temperature, argon flow 0.2m3/ h, propane 0.15m3/ h, sedimentation time 30 hours, system
Standby density of material 1.55g/cm3；High-performance, the preparation of high density C/C composite material are carried out using PIC technique, soaked by 8 periods
Stain cracking, by 2 2000 DEG C of -2h high-temperature heat treatments, infiltration pyrolysis specific process parameter are as follows: vacuum degree -0.1MPa, dipping pressure
Power 5MPa, 170 DEG C of solidification temperature, 1000 DEG C of cracking temperature of carbonization, heat preservation 1h, material final densities 1.85g/cm3, material always makes
Standby 400 hours periods.Fig. 3 is the mechanical curves figure for preparing C/C composite material.
Embodiment 3:
By taking 750 × 350 × 45mm as an example, density 0.5g/cm32D Nomex；Pyrolytic carbon circle is prepared using ICVI technique
Surface layer, 900 DEG C of temperature, argon flow 0.2m3/ h, propane 0.15m3/ h, sedimentation time 5 hours；It is prepared using E-CVI technique low
Density C/C composite material, 700~1000 DEG C of temperature, argon flow 0.2m3/ h, propane 0.15m3/ h, sedimentation time 40 hours, system
Standby density of material 1.45g/cm3；High-performance, the preparation of high density C/C composite material are carried out using PIC technique, soaked by 8 periods
Stain cracking, by 2 2000 DEG C of -2h high-temperature heat treatments, infiltration pyrolysis specific process parameter are as follows: vacuum degree -0.1MPa, dipping pressure
Power 5MPa, 170 DEG C of solidification temperature, 1000 DEG C of cracking temperature of carbonization, heat preservation 1h, material final densities 1.82g/cm3, material always makes
Standby 450 hours periods.
Claims (10)
1. a kind of method of short cycle, low cost preparation high-performance carbon/carbon compound material, it is characterised in that: this method is to use
It is electrically coupled chemical gaseous phase cementation process and is combined with liquid impregnation-carbonization technique and prepare carbon/carbon compound material, this method includes as follows
Step:
(1) preparation of boundary layer:
Using isothermal chemical gaseous phase cementation process, carbon fiber precast body is placed in ICVI cvd furnace to the preparation for carrying out boundary layer, boundary
0.3~2 μm of surface thickness；
(2) it uses and is electrically coupled chemical gaseous phase cementation process preparation low-density C/C composite material；
(3) high-performance, high density C/C composite material are prepared using liquid impregnation-carbonization technique.
2. the method for short cycle according to claim 1, low cost preparation high-performance carbon/carbon compound material, feature exist
In: in step (1), the carbon fiber precast body is punctured using 2D needling structure, 2.5D braiding structure, 3D braiding structure or thin compile
Structure replaces laying with the PANCF net tire of one layer of 12K with the PANCF laminated cloth of one layer of 12K, 1K, 3K or 6K；Laminated cloth is 0/
90 ° of layings, 1.X+1.Y mode continuous needle form.
3. the method for short cycle according to claim 1, low cost preparation high-performance carbon/carbon compound material, feature exist
In: in step (1), the isothermal chemical vapor infiltration technological parameter are as follows: with Ar or N in unstrpped gas2For diluent gas, dilution
0.01~0.5m of gas flow3/ h, using liquefied natural gas, methane or propane as carbon-source gas, carbon-source gas flow 0.01~
0.5m3/h；700~1100 DEG C of depositing temperature, sedimentation time 3-10h.
4. the method for short cycle according to claim 1, low cost preparation high-performance carbon/carbon compound material, feature exist
In: in step (2), the process for being electrically coupled chemical gaseous phase cementation process are as follows: the sample with interfacial TCO layer for preparing step (1)
It is placed in the chemical vapor deposition stove with water-cooling wall and direct-electrifying heats, fiber peripheral generates electromagnetic field, due to precast body
Heat-insulated and outer gas stream and water-cooling wall effect, formation temperature gradient in precast body occurs in so that deposition is preferential
The heart, and gradually elapsed to two sides, reaction gas realizes fast deposition under the interaction of electromagnetic field, temperature field and fluid field.
5. the method for short cycle according to claim 4, low cost preparation high-performance carbon/carbon compound material, feature exist
In: it is described to be electrically coupled in chemical vapor infiltration technical process in step (2), with Ar or N2For diluent gas, diluting gas flow
0.01~0.5m3/ h, using liquefied natural gas, methane or propane as carbon-source gas, 0.01~0.5m of carbon-source gas flow3/h；Deposition
300~1100 DEG C of temperature, sedimentation time 5-50h.
6. the method for short cycle according to claim 5, low cost preparation high-performance carbon/carbon compound material, feature exist
In: low-density C/C composite material prepared by step (2), matrix center part are fine and close pyrolytic carbon layer, and outside is loose
Pyrolytic carbon layer, material global density are controlled in 0.8~1.6g/cm3Between.
7. the method for short cycle according to claim 1, low cost preparation high-performance carbon/carbon compound material, feature exist
In: in step (3), the process of the liquid impregnation-carbonization technique are as follows: be placed in low-density C/C composite material obtained by step (2)
In vacuum pressure container, resin is impregnated into matrix using vacuum environment, which is known as vacuum-pressure dipping process；Through
After vacuum-pressure dipping process, then low temperature drying crosslinking curing and Pintsch process carbonisation are carried out, it is compound to obtain intermediate C/C
Material repeats vacuum-pressure dipping, low temperature drying crosslinking curing and Pintsch process carbonisation 5~15 times, finally
High density, high-performance C/C composite material are obtained, density domination is in 1.8~1.9g/cm3。
8. the method for short cycle according to claim 7, low cost preparation high-performance carbon/carbon compound material, feature exist
In: in the liquid impregnation-Carbonization technology processing, need when the rate of body weight gain of the intermediate C/C composite material≤3% to matrix
Carry out machining or high temperature graphitization processing；0.5~2mm of the machining range scale, at the high temperature graphitization
Reason refers to handles C/C composite material 1~2h under the conditions of 1800~2800 DEG C of temperature.
9. the method for short cycle according to claim 7, low cost preparation high-performance carbon/carbon compound material, feature exist
In: in the liquid impregnation-Carbonization technology processing, resin used can be dipping when being used to prepare C/C composite material
Existing any resin, currently preferred resin are furane resins or phenolic resin.
10. the method for short cycle according to claim 7, low cost preparation high-performance carbon/carbon compound material, feature exist
In: in the liquid impregnation-Carbonization technology processing, carry out vacuum-pressure dipping, low temperature drying crosslinking curing and Pintsch process carbon
Change process specifically: firstly, resin is introduced into material internal using vacuum environment, vacuum degree≤- 0.1MPa keeps 1-3h；
Then, it is passed through Ar or N2And it is forced into 2~6MPa, keep 1-5h；Subsequently, 120-180 DEG C of crosslinking curing 5-10h；Finally, high
Anneal crack solution carbonization: 900 DEG C~1200 DEG C of carburizing temperature, carbonization time 8~15 hours.
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| CN110877983A (en) * | 2019-12-26 | 2020-03-13 | 内蒙古航天红岗机械有限公司 | Preparation method of C/C composite material |
| CN111635242A (en) * | 2020-06-09 | 2020-09-08 | 中南大学 | Rapid preparation method and application of high-density revolving body carbon/carbon composite material |
| CN113292351A (en) * | 2021-04-25 | 2021-08-24 | 航天材料及工艺研究所 | Preparation method of quasi-isotropic carbon cloth needle-punched carbon/carbon composite material |
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| CN111635242A (en) * | 2020-06-09 | 2020-09-08 | 中南大学 | Rapid preparation method and application of high-density revolving body carbon/carbon composite material |
| CN113292351A (en) * | 2021-04-25 | 2021-08-24 | 航天材料及工艺研究所 | Preparation method of quasi-isotropic carbon cloth needle-punched carbon/carbon composite material |
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