CN104671817B - A kind of preparation method of the carbon fibre composite possessing cvd film - Google Patents
A kind of preparation method of the carbon fibre composite possessing cvd film Download PDFInfo
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- CN104671817B CN104671817B CN201510103893.7A CN201510103893A CN104671817B CN 104671817 B CN104671817 B CN 104671817B CN 201510103893 A CN201510103893 A CN 201510103893A CN 104671817 B CN104671817 B CN 104671817B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000835 fiber Substances 0.000 title claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005087 graphitization Methods 0.000 claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 17
- 239000011347 resin Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 230000004913 activation Effects 0.000 claims abstract description 13
- 238000005470 impregnation Methods 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000007792 gaseous phase Substances 0.000 claims abstract description 8
- 230000008021 deposition Effects 0.000 claims abstract description 7
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 35
- 239000004917 carbon fiber Substances 0.000 claims description 35
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 27
- 238000000498 ball milling Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- 238000000197 pyrolysis Methods 0.000 claims description 9
- -1 carbon fiber compound Chemical class 0.000 claims description 8
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 8
- 239000010445 mica Substances 0.000 claims description 8
- 229910052618 mica group Inorganic materials 0.000 claims description 8
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- 239000004215 Carbon black (E152) Substances 0.000 claims description 5
- 239000004695 Polyether sulfone Substances 0.000 claims description 5
- 229930195733 hydrocarbon Natural products 0.000 claims description 5
- 150000002430 hydrocarbons Chemical class 0.000 claims description 5
- 229920006393 polyether sulfone Polymers 0.000 claims description 5
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 4
- 125000000524 functional group Chemical group 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000005728 strengthening Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 238000004804 winding Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 150000001722 carbon compounds Chemical class 0.000 abstract description 10
- 238000001816 cooling Methods 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 125000000219 ethylidene group Chemical group [H]C(=[*])C([H])([H])[H] 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000011160 polymer matrix composite Substances 0.000 description 1
- 229920013657 polymer matrix composite Polymers 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
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- Ceramic Products (AREA)
Abstract
The present invention relates to the preparation method of a kind of carbon fibre composite possessing cvd film, comprise the steps: that 1 makes the preforming idiosome with height-oriented cone C/C composite；2 enhancing skeleton vacuum impregnation benzoxazine resins solution step 1 obtained also make required shape；3 carry out pressurization charing under nitrogen protection by processing, through step 2, the prepreg obtained；Impregnate high temperature resistant Econol resin solution again and fill space, carry out chemical gaseous phase deposition CVD afterwards；4 graphitization processing；5 fine and close carbon/carbon composite articles step 4 obtained carry out steam activation; after activation, under inert gas shielding, cooling obtains the high-purity carbon/carbon compound material possessing cvd film, possesses the density of high-purity carbon/carbon compound material of cvd film more than 2.58g/cm3, hot strength reaches more than 900MPa, and thermal conductivity is 450 480W/ (m K), and thermal diffusivity is 3.3cm2/s。
Description
Technical field
The present invention relates to the preparation method of a kind of Carbon Materials, particularly to the preparation method of a kind of carbon fibre composite.
Background technology
The inorganic non-metallic based composites that carbon/carbon (C/C) composite is made up of carbon fiber and carbon base body, its modulus is high, intensity is big, wear-resistant, corrosion-resistant, absorbing is good, particularly having heat endurance and the thermal shock resistance of excellence, at high temperature mechanical strength loss is little.Since the sixties develops, have become as a kind of new material of World High Technology field primary study and exploitation.At aerospace field, there is important using value, as aircraft brake sheet, the heatshield material of reentry vehicle, rocket nose cone, engine jet pipe, thrust chamber and combustion liner etc..
According to the type of the matrix precursor that composite densification process is used, the manufacture craft of carbon/carbon compound material mainly has two kinds of methods: one is that chemical gaseous phase deposits (CVD) method, and it is with hydrocarbon gas (CH4, C2H4, natural gas etc.) be matrix precursor, after these gases at high temperature produce pyrolytic reaction, C is deposited on precast body surface with the form of atom or drop or oozes in the space within long-pending precast body, this method can obtain the carbon/carbon compound material of preferable performance, higher density, and shortcoming is equipment complexity, fabrication cycle length, stock utilization low (only about 3%), cost height.Another kind of method is called liquid impregnation-carbonizatin method, and it is that these raw materials at high temperature occur series of complex chemical change to be converted into matrix carbon with thermoplastic bitumen or thermosetting resin as matrix precursor.This method is raw materials used cheap, and equipment is simple, fabrication cycle is short, thus the attention of many scientific workers in receiving world wide, become a focus of carbon/carbon compound material research.Introduce catalyst and thermosetting resin charcoal is carried out catalyzed graphitization, be a kind of effective ways improving phenolic resin carbon degree of graphitization.The report such as Li Chongjun adds pure boron as catalyst in resin carbon micro mist, graphitization temperature be 2100 DEG C, catalyst boron consumption less than 5.0wt% process conditions under, the degree of graphitization of resin carbon base carbon/carbon composite has reached 82%, and the carbon/carbon composite degree of graphitization at 2500 DEG C without catalyst just reaches 71%.This shows that boron all has obvious effect in terms of reducing graphitization temperature and improving degree of graphitization.The correlative study of the preparation technology of the most complete high-purity carbon/carbon compound material using liquid impregnation-charing method preparation to possess cvd film.
Summary of the invention
It is contemplated that overcome prior art not enough, purpose is to provide the preparation method of the simple and reproducible high heat conductivity carbon fiber polymer matrix composites of a kind of preparation technology, the most highly directional high heat conduction of the high-purity carbon/carbon compound material possessing cvd film prepared by the method, and along fibre length direction mechanical property be improved significantly.
For achieving the above object, the technical solution used in the present invention is: the preparation method of a kind of high purity carbon fibrous composite possessing cvd film: include following five steps:
(1) it is coated with sulfonic polyether sulfone at continuous filament yarn carbon fiber surface; the most under nitrogen protection in 1800-2000 DEG C of pyrolysis; to remove the oxygen-containing functional group of carbon fiber surface; expose carbon fiber nude surface; then pretreated continuous filament yarn carbon fiber winding is made the preformed blank with height-oriented cone carbon fibre composite, uses the preformed blank of this carbon fiber as strengthening skeleton；Wherein, the volume density of the preformed blank of described carbon fiber is at 1.0g/cm3Below；
According to preformed blank: silicon carbide powder: mica powder: the mass ratio of montmorillonite=2:1:1:1, weigh preformed blank respectively, granularity is the silicon carbide powder of 10-15 micron, mica powder, montmorillonite, by each raw material mixing and ball milling, while ball milling, add appropriate water, after ball milling 2h, obtain carbon fiber compound；
(2) the carbon fiber compound vacuum impregnation benzoxazine resins solution that step (1) obtained also makes required shape, the resin carbon under high-temperature process residual；Described vacuum impregnation temperature is 400-450 DEG C；
(3) carry out pressurization charing under nitrogen protection by processing, through step (2), the prepreg that obtains, i.e. 60～100MPa, at room temperature to 200 DEG C compression molding make blank of material；Under inert atmosphere protection, carbonize to 900～1000 DEG C and 900～1000 DEG C of constant temperature 1～2 hours with the speed of 15～20 DEG C/h；Impregnate high temperature resistant Econol resin solution again and fill space, carry out chemical gaseous phase deposition CVD afterwards；
(4) repeating step (3) 5-10 week after date makes it densified make primary products formed, by primary products formed under an argon atmosphere, 2400～2600 DEG C of preheatings are risen to 100～200 DEG C/h of speed, and be warming up to 3000-3500 DEG C of constant temperature 1～within 2 hours, carry out graphitization processing, graphitization internal furnace furnace pressure is at below 20MPa；Impregnate the most again, then CVD so that it is the most densified；In described step (4), CVD technique is that deposited preform is placed in the CVD stove of equal heat space, and hydrocarbon gas occurs the heavy carbon of pyrolysis in the porous preform of soaking, makes byproduct gas diffuse out.
(5) fine and close goods step (4) obtained carry out steam activation; after activation; cool down under inert gas shielding, obtain the high purity carbon fibrous composite possessing cvd film, described in possess the density of high purity carbon fibrous composite of cvd film more than 2.58g/cm3, hot strength reaches more than 900MPa, and thermal conductivity is 450-480W/ (m K), and thermal diffusivity is 3.3cm2/s。
Wherein, step (5) steam activation temperature is 750～900 DEG C, and water inlet speed is 0.5～20ml/min, and the time is 1.5～6 hours, and heating rate is 1～15 DEG C/min.
Chemical gaseous phase deposition in described step (3) and step (4) mainly has isothermal process, barometric gradient flow-route and temperature gradient processes three kinds.
Its feature of high-purity carbon/carbon compound material of prepared by the present invention possess cvd film is mainly to pre-process carbon fiber by sulfonic polyether sulfone, control pyrolysis temperature, pressurization carbonizes, impregnate high temperature resistant Econol resin and high temperature graphitization processes content and the form controlling pyrolytic carbon, to obtain the carbon/carbon compound material of higher heat-conductivity, high tensile and low thermal coefficient of expansion, low-friction coefficient.The carbon/carbon compound material that the inventive method prepares, has that low-friction coefficient, thermal stability be excellent, high intensity and an advantage such as wear-resisting.This have the advantage that technique is simple, workable, easy to make.
Detailed description of the invention
Feature and the effect of the present invention it is further elucidated with below by embodiment.
Embodiment 1:
(1) it is coated with sulfonic polyether sulfone at continuous filament yarn carbon fiber surface; the most under nitrogen protection in 800 DEG C of pyrolysis; to remove the oxygen-containing functional group of carbon fiber surface; expose carbon fiber nude surface; then pretreated continuous filament yarn carbon fiber winding is made the preformed blank with height-oriented cone carbon fibre composite, uses the preformed blank of this carbon fiber as strengthening skeleton；Wherein, the volume density of the preformed blank of described carbon fiber is 0.6g/cm3；
According to preformed blank: silicon carbide powder: mica powder: the mass ratio of montmorillonite=2:1:1:1, weighing granularity respectively is the silicon carbide powder of 10-15 micron, mica powder, montmorillonite, by each raw material mixing and ball milling, while ball milling, add appropriate water, after ball milling 2h, obtain carbon fiber compound；
(2) the carbon fiber compound vacuum impregnation benzoxazine resins solution that step (1) obtained also makes required shape, the resin carbon under high-temperature process residual；Described vacuum impregnation temperature is 400-450 DEG C；
(3) carrying out pressurization charing under nitrogen protection by processing, through step (2), the prepreg obtained, i.e. at 60MPa, room temperature to 200 DEG C, blank of material is made in compression molding；Under inert atmosphere protection, carbonize to 900 DEG C and 900 DEG C of constant temperature 1 hour with the speed of 15 DEG C/h；Epoxy resin-impregnated solution fills space again, carries out chemical gaseous phase deposition CVD afterwards, repeats (3) 5 all after dates of step and makes it densified make primary products formed；
(4) by primary products formed under an argon atmosphere, rising to 2400 DEG C of preheatings with 100 DEG C/h of speed, and be warming up to 3000 DEG C of constant temperature and within 1 hour, carry out graphitization processing, graphitization internal furnace furnace pressure is at below 20MPa；Impregnate the most again, then CVD so that it is the most densified；In described step (4), CVD technique is that deposited preform is placed in the CVD stove of equal heat space, and hydrocarbon gas occurs the heavy carbon of pyrolysis in the porous preform of soaking, makes byproduct gas diffuse out；
(5) fine and close goods step (4) obtained carry out steam activation; steam activation temperature is 750 DEG C; water inlet speed is 0.5ml/min; time is 1.5 hours; heating rate is 1 DEG C/min, after activation, cools down under inert gas shielding; obtain the high purity carbon fibrous composite possessing cvd film, described in possess cvd film the density of high purity carbon fibrous composite be 3.022g/cm3, hot strength reaches 980MPa, and thermal conductivity is 450W/ (m K), and thermal diffusivity is 3.3cm2/s。
Embodiment 2:
(1) it is coated with sulfonic polyether sulfone at continuous filament yarn carbon fiber surface; the most under nitrogen protection in 1200 DEG C of pyrolysis; to remove the oxygen-containing functional group of carbon fiber surface; expose carbon fiber nude surface; then pretreated continuous filament yarn carbon fiber winding is made the preformed blank with height-oriented cone carbon fibre composite, uses the preformed blank of this carbon fiber as strengthening skeleton；Wherein, the volume density of the preformed blank of described carbon fiber is at 1.0g/cm3；
According to preformed blank: silicon carbide powder: mica powder: the mass ratio of montmorillonite=2:1:1:1, weighing granularity respectively is the silicon carbide powder of 10-15 micron, mica powder, montmorillonite, by each raw material mixing and ball milling, while ball milling, add appropriate water, after ball milling 2h, obtain carbon fiber compound；
(2) the carbon fiber compound vacuum impregnation benzoxazine resins solution that step (1) obtained also makes required shape, the resin carbon under high-temperature process residual；Described vacuum impregnation temperature is 400-450 DEG C；
(3) carrying out pressurization charing under nitrogen protection by processing, through step (2), the prepreg obtained, i.e. at 100MPa, room temperature to 200 DEG C, blank of material is made in compression molding；Under inert atmosphere protection, carbonize to 1000 DEG C and constant temperature 1～2 hours with the speed of 20 DEG C/h；Epoxy resin-impregnated solution fills space again, carries out chemical gaseous phase deposition CVD afterwards, repeats (3) 10 all after dates of step and makes it densified make primary products formed；
(4) by primary products formed under an argon atmosphere, rising to 2600 DEG C of preheatings with 200 DEG C/h of speed, and be warming up to 3500 DEG C of constant temperature 1～within 2 hours, carry out graphitization processing, graphitization internal furnace furnace pressure is at below 20MPa；Impregnate the most again, then CVD so that it is the most densified；In described step (4), CVD technique is that deposited preform is placed in the CVD stove of equal heat space, and hydrocarbon gas occurs the heavy carbon of pyrolysis in the porous preform of soaking, makes byproduct gas diffuse out；
(5) goods that step (4) obtains are carried out steam activation; after activation; cool down under inert gas shielding, obtain the high purity carbon fibrous composite possessing cvd film, described in possess cvd film the density of high purity carbon fibrous composite be 3.58g/cm3, hot strength reaches 1000MPa, and thermal conductivity is 480W/ (m K), and thermal diffusivity is 3.3cm2/s。
To those skilled in the art, under this patent design and specific embodiment enlightenment, some deformation can directly derived from this patent disclosure and general knowledge or associate, it will be recognized by those of ordinary skill in the art that and may be used without additive method, or the replacement of conventional known technology in prior art, and the equivalence of feature changes or modifies, mutually different combination between feature, the such as change of Carbon fibe K number, the change in the range of generally of the concrete technology parameter, etc. unsubstantiality change, equally it is employed, this patent representation function and effect can be realized, citing expansion is described in detail the most one by one, belong to this patent protection domain.
Claims (3)
1. the preparation method of the carbon fibre composite possessing cvd film, it is characterised in that: include following five steps:
(1) it is coated with sulfonic polyether sulfone at continuous filament yarn carbon fiber surface; the most under nitrogen protection in 1800-2000 DEG C of pyrolysis; to remove the oxygen-containing functional group of carbon fiber surface; expose carbon fiber nude surface; then pretreated continuous filament yarn carbon fiber winding is made the preformed blank with height-oriented cone carbon fibre composite, uses the preformed blank of this carbon fiber as strengthening skeleton；Wherein, the volume density of the preformed blank of described carbon fiber is at 1.0g/cm3Below；
According to preformed blank: silicon carbide powder: mica powder: the mass ratio of montmorillonite=2:1:1:1, weigh preformed blank respectively, granularity is the silicon carbide powder of 10-15 micron, mica powder, montmorillonite, by each raw material mixing and ball milling, while ball milling, add appropriate water, after ball milling 2h, obtain carbon fiber compound；
(2) the carbon fiber compound vacuum impregnation benzoxazine resins solution that step (1) obtained also makes required shape, the resin carbon under high-temperature process residual；Described vacuum impregnation temperature is 400-450 DEG C；
(3) carry out pressurization charing under nitrogen protection by processing, through step (2), the prepreg that obtains, i.e. 60～100MPa, at room temperature to 200 DEG C compression molding make blank of material；Under inert atmosphere protection, carbonize to 900～1000 DEG C and 900～1000 DEG C of constant temperature 1～2 hours with the speed of 15～20 DEG C/h；Impregnate high temperature resistant Econol resin solution again and fill space, carry out chemical gaseous phase deposition CVD afterwards；
(4) repeating step (3) 5-10 week after date makes it densified make primary products formed, by primary products formed under an argon atmosphere, 2400～2600 DEG C of preheatings are risen to 100～200 DEG C/h of speed, and be warming up to 3000-3500 DEG C of constant temperature 1～within 2 hours, carry out graphitization processing, graphitization internal furnace furnace pressure is at below 20MPa；Impregnate the most again, then CVD so that it is the most densified；
In described step (4), CVD technique is that deposited preform is placed in the CVD stove of equal heat space, and hydrocarbon gas occurs the heavy carbon of pyrolysis in the porous preform of soaking, makes byproduct gas diffuse out；
(5) goods that step (4) obtains are carried out steam activation; after activation; cool down under inert gas shielding, obtain the high purity carbon fibrous composite possessing cvd film, described in possess the density of high purity carbon fibrous composite of cvd film more than 2.58g/cm3, hot strength reaches more than 900MPa, and thermal conductivity is 450-480W/ (m K), and thermal diffusivity is 3.3cm2/s。
The preparation method of the carbon fibre composite possessing cvd film the most according to claim 1, it is characterized in that: step (5) steam activation temperature is 750～900 DEG C, water inlet speed is 0.5～20ml/min, and the time is 1.5～6 hours, and heating rate is 1～15 DEG C/min.
The preparation method of the carbon fibre composite possessing cvd film the most according to claim 1, it is characterised in that: the chemical gaseous phase deposition in step (3) and step (4) has isothermal process, barometric gradient flow-route and temperature gradient processes three kinds.
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| RU2750300C1 (en) * | 2020-12-28 | 2021-06-25 | "Волгоградский государственный технический университет" (ВолгГТУ) | Method for producing carbon-graphite composite material |
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| CN102826867A (en) * | 2012-09-13 | 2012-12-19 | 湖南省鑫源新材料股份有限公司 | Carbon/carbon composite material flat plate preparation method |
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| RU2750300C1 (en) * | 2020-12-28 | 2021-06-25 | "Волгоградский государственный технический университет" (ВолгГТУ) | Method for producing carbon-graphite composite material |
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