CN103266470A - Carbon fiber antioxidation coating and preparation method thereof - Google Patents
Carbon fiber antioxidation coating and preparation method thereof Download PDFInfo
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- CN103266470A CN103266470A CN2013101860369A CN201310186036A CN103266470A CN 103266470 A CN103266470 A CN 103266470A CN 2013101860369 A CN2013101860369 A CN 2013101860369A CN 201310186036 A CN201310186036 A CN 201310186036A CN 103266470 A CN103266470 A CN 103266470A
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Abstract
The invention discloses a carbon fiber antioxidation coating and a preparation method thereof. The carbon fiber antioxidation coating is a SiO2 doped SiC coating which is coated on the surface of a carbon fiber with a pyrocarbon coating, wherein the diameter of the carbon fiber is 6-8mu m. The preparation method of the SiO2 doped SiC coating comprises the following steps: based on a precursor impregnation and cracking method, by taking dimethylbenzene as solvent and ethyl orthosilicate doped polycarbosilane as a precursor, performing pressure impregnation on a carbon fiber preform with a pyrocarbon coating having a thickness of 400-700nm, performing curing treatment, and performing pyrolytic cracking. The thickness of the coating is less than 1mu m and is controllable; and the coating is smooth, complete, less prone to shed and simple in preparation process, and has better oxidation resistance.
Description
Technical field
The present invention relates to a kind of carbon fiber surface coating and preparation method thereof, particularly ORC of a kind of carbon fiber and preparation method thereof.
Background technology
Carbon fiber has high specific strength, high ratio modulus, low linear expansion coefficient, good series of advantages such as thermoelectricity capability, it is not only requisite structural material, resistant material, heat-barrier material and the special type function material of making rocket, guided missile, satellite space shuttle and space station, and be the lightweight of fighter plane, airline carriers of passengers, helicopter, the main fortifying fibre of high performance, thereby in high-tech industry, be used widely.But the oxidation that carbon fiber takes place in temperature is higher than 400 ℃ oxidation environment, mechanical property descends gradually, and this becomes the deadly defect that the restriction carbon fiber uses under higher temperature conditions.Simultaneously, carbon fiber is widely used in multiple composite as reinforcing material, and different composites proposes different requirements to the interface of fiber-matrix.Preparing coating at carbon fiber surface is to address the above problem the method that generally adopts.At present comparative maturity, the interface coating material that enters practical field have boron nitride (BN), carborundum (SiC) etc.Wherein, SiC has fusing point height, performance such as high temperature resistant, corrosion-resistant, anti-oxidant, thereby is widely used in composite and fiber coat.At present, the preparation method of SiC coating mainly contains chemical vapor deposition (CVD) method, precursor infiltration and pyrolysis (PIP) method, physical vapor deposition (PVD) method, sol-gel (Sol-Gel) method and in-situ reaction etc.Wherein, adopting the PIP method, is the technology comparative maturity that precursor prepares carbon fiber surface SiC coating with Polycarbosilane (PCS), has that technological temperature is low, a composition of goods and structure is controlled, equipment requires advantages such as low.Because contraction and thermal stress effect that the discharge of small-molecule substance produces, but coating is prone to crackle and obscission to PCS, influences its antioxygenic property in the Pintsch process process.
Summary of the invention
At above-mentioned the deficiencies in the prior art, the invention provides a kind of carbon fiber ORC and preparation method thereof, solved coating and be prone to crackle, easily come off, problem such as antioxygenic property is not high.
The present invention is by the following technical solutions:
A kind of carbon fiber ORC, described carbon fiber ORC is SiO
2The SiC coating of mixing, wherein, wherein, SiO
2Mass fraction be 1%～10%, SiO
2The SiC coating of mixing overlays on the carbon fiber surface of the prefabricated carbon fiber body of being with RESEARCH OF PYROCARBON (PyC) coating.
Further, described SiO
2The SiC coating layer thickness that mixes is greater than 0 and less than 1 μ m.
Further, the carbon fiber diameter of the prefabricated carbon fiber body of described band pyrocarbon coating is 6～8 μ m, and pyrocarbon coating thickness is 400～700nm.
The preparation method of above-mentioned carbon fiber ORC may further comprise the steps:
Step 1, Polycarbosilane and ethyl orthosilicate added stirring and dissolving makes precursor solution in the dimethylbenzene, wherein, the mass fraction of Polycarbosilane is 2.5%～20%, and the mass fraction of ethyl orthosilicate is 1.25%～20%;
Step 2, with the prefabricated carbon fiber body of the precursor solution pressure impregnation band pyrocarbon coating that obtains in the step 1, wherein impregnation pressure is 1～2.5Mpa, dip time 10～60min;
Step 3, the prefabricated carbon fiber body that obtains in the step 2 is cured processing, wherein, solidifying the temperature of handling is 160～220 ℃, and solidifying the atmosphere of handling is air, and solidifying the time of handling is 1～2h;
Step 4, the prefabricated carbon fiber body that obtains in the step 3 is carried out Pintsch process, wherein, cracking temperature is 1000～1300 ℃, heating rate is 2～10 ℃/min, cracking atmosphere is argon gas or vacuum, the cracking temperature retention time is 1～2h, and namely the carbon fiber surface at the prefabricated carbon fiber body of being with pyrocarbon coating prepares complete SiO
2The SiC coating of mixing.
Further, the carbon fiber diameter of the prefabricated carbon fiber body of band pyrocarbon coating is 6～8 μ m in the described step 2, and pyrocarbon coating thickness is 400～700nm.
Further, repeatedly circulation step two is to step 4, and wherein cycle-index is 1～4 time.
Principle of the present invention: ethyl orthosilicate high temperature produces glassy state SiO
2, pyroprocess can healed cracks.Simultaneously, the SiO that the doping ethyl orthosilicate produces in the precursor solution
2Improved the adhesive property between SiC coating and the PyC coating, so coating quality obviously improves, for the diffusion of oxygen provides obstacle, namely antioxygenic property improves.
Beneficial effect of the present invention: the present invention is at the complete SiO of PyC coat carbon fiber surface preparation
2The SiC coating of mixing has solved the problem that the PIP legal system is equipped with the SiC coating shedding.The antioxygenic property of coat carbon fiber obviously improves, and has solved interface wet ability and consistency problem between carbon fiber and some matrices of composite material simultaneously.The present invention prepares the method for ORC at the carbon fiber surface of prefabricated carbon fiber body, and simple and easy to do, cost is not high.Use this coat carbon fiber precast body can be compound with metal, pottery, polymer etc., obtain the good composite of antioxygenic property, reduced the coated monofilament carbon fiber and prepared composite material and fibrage process to the infringement of coating.
To sum up, the present invention is at the complete SiO of PyC coat carbon fiber surface preparation
2The SiC coating of mixing, coating layer thickness is less than 1 μ m, and controllable thickness, and coating is smooth complete, difficult drop-off, preparation technology is simple, has the good oxidization resistance energy.
Description of drawings
Fig. 1 is 8000 times stereoscan photograph of the PyC/SiC coat carbon fiber precast body of embodiment 1 preparation;
Fig. 2 is 8000 times stereoscan photograph of the PyC/SiC coat carbon fiber precast body of embodiment 5 preparations;
Fig. 3 is 20000 times stereoscan photograph of the PyC/SiC coat carbon fiber precast body of embodiment 5 preparations;
Fig. 4 is the PyC/SiC coat carbon fiber precast body of the embodiment 5 preparation surface sweeping electromicroscopic photograph behind 700 ℃ of oxidation 10min in air;
Fig. 5 is that no coating, PyC coating and the present invention are through the static oxidation curve of the carbon fiber of the PyC/SiC coating of different cracking temperature preparations.
The specific embodiment:
Below in conjunction with embodiment and accompanying drawing the present invention is done further explanation, should be appreciated that following examples only are intended to explanation, should not be regarded as limitation of the scope of the invention.
A kind of carbon fiber ORC is SiO
2The SiC coating of mixing, its thickness is greater than 0 μ m and less than 1 μ m, wherein SiO
2Mass fraction be 1%～10%.SiO
2The SiC coating of mixing overlays on the carbon fiber surface of prefabricated carbon fiber body of band RESEARCH OF PYROCARBON (PyC) coating, and wherein the carbon fiber diameter with the prefabricated carbon fiber body of pyrocarbon coating is 6～8 μ m, and pyrocarbon coating thickness is 400～700nm.
Adopt precursor infiltration and pyrolysis (PIP) method to prepare above-mentioned carbon fiber ORC, may further comprise the steps:
Step 1, Polycarbosilane and ethyl orthosilicate added stirring and dissolving makes precursor solution in the dimethylbenzene, wherein, the mass fraction of Polycarbosilane is 2.5%～20%, and the mass fraction of ethyl orthosilicate is 1.25%～20%;
Step 2, impregnating by pressure: with the prefabricated carbon fiber body of the precursor solution pressure impregnation band pyrocarbon coating that obtains in the step 1, adopt the mould pressurization to promote soaking into of precursor solution in the dipping process, wherein, the precursor solution height is greater than the height of prefabricated carbon fiber body, guarantee that pressure process can directly not pressurize to precast body, impregnation pressure is 1～2.5Mpa, dip time 10～60min, the carbon fiber diameter of the prefabricated carbon fiber body of band PyC coating is 6～8 μ m, adopt chemical vapor infiltration (CVI) method in prefabricated carbon fiber body preparation PyC coating, the PyC coating layer thickness is 400～700nm;
Step 3, curing are handled: the prefabricated carbon fiber body that obtains in the step 2 is cured processing, and wherein, solidifying the temperature of handling is 160～220 ℃, and the atmosphere of solidifying processing is air, and solidifying the time of handling is 1～2h;
Step 4, Pintsch process: the prefabricated carbon fiber body that obtains in the step 3 is carried out Pintsch process, wherein, cracking temperature is 1000～1300 ℃, heating rate is 2～10 ℃/min, cracking atmosphere is argon gas or vacuum, the cracking temperature retention time is 1～2h, and namely the carbon fiber surface at the prefabricated carbon fiber body of being with pyrocarbon coating prepares complete SiO
2The SiC coating of mixing, thickness is greater than 0 μ m and less than 1 μ m.
The prefabricated carbon fiber body of the present invention's process precursor solution impregnating by pressure treats that the prefabricated carbon fiber body is cooled to room temperature after solidifying processing and Pintsch process, repeat impregnating by pressure-curing processing-Pintsch process process, and this process can be carried out 1～4 time.Embodiment 1
Adopt mortar that PCS is worn into fine powder, can accelerate its rate of dissolution in solvent.PCS and ethyl orthosilicate (TEOS) are added in the dimethylbenzene by a certain percentage, stirring and dissolving, the preparation precursor solution, wherein the mass fraction of PCS is that the mass fraction of 10%, TEOS is 5%.The carbon fiber diameter of the prefabricated carbon fiber body of band PyC coating is 6～8 μ m, and the PyC coating layer thickness is 400～700nm.Adopted above-mentioned precursor solution pressure impregnation prefabricated carbon fiber body 20 minutes, pressure is 2Mpa.The prefabricated carbon fiber body was cured processing in 1.5 hours at 180 ℃ of air atmosphere constant temperature after taking out.Subsequently precast body is placed graphite crucible, together put into stove, used stove is atmosphere furnace; temperature rises to 1000 ℃ by room temperature with the speed of 4 ℃/min; be incubated 1 hour, under the argon gas atmosphere protection, carry out Pintsch process, thereby obtain SiO in PyC coat carbon fiber surface preparation
2The SiC coating of mixing.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 20～100nm, wherein SiO
2Mass fraction be 2%～5%.
Embodiment 2
The difference of present embodiment and embodiment 1 is that the Pintsch process process adopts vacuum environment, and used stove is vacuum drying oven, is warming up to 1200 ℃ with the speed of 8 ℃/min, is incubated 1 hour.Other steps are identical with embodiment 1.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 20～100nm, wherein SiO
2Mass fraction be 2%～5%.
Embodiment 3
The difference of present embodiment and embodiment 1 is that the mass fraction of the PCS of modification in the precursor solution is that the mass fraction of 15%, TEOS is 10%.Other steps are identical with embodiment 1.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 50～240nm, wherein SiO
2Mass fraction be 2.4%～6%.
Embodiment 4
The difference of present embodiment and embodiment 3 is that cracking process adopts vacuum environment, and used stove is vacuum drying oven, is warming up to 1200 ℃ with the speed of 8 ℃/min, is incubated 1 hour.Other steps are identical with embodiment 3.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 50～240nm, wherein SiO
2Mass fraction be 2.4%～6%.
Embodiment 5
Adopt mortar that PCS is worn into fine powder, PCS and TEOS are added in the dimethylbenzene by a certain percentage, stirring and dissolving, the preparation precursor solution, wherein the mass fraction of PCS is that the mass fraction of 10%, TEOS is 5%.The prefabricated carbon fiber body of band PyC coating, the carbon fiber diameter is 6～8 μ m, the PyC coating layer thickness is 400～700nm.Adopted above-mentioned precursor solution pressure impregnation prefabricated carbon fiber body 20 minutes, pressure is 2Mpa.After the prefabricated carbon fiber body took out, 180 ℃ of air atmosphere constant temperature were cured processing in 1.5 hours.Subsequently precast body is placed graphite crucible, together put into stove, used stove is atmosphere furnace.Temperature rises to 1000 ℃ by room temperature with the speed of 4 ℃/min, is incubated 1 hour, carries out Pintsch process under the argon gas atmosphere protection.Repeat pressure impregnation-curings processing-Pintsch process 1 time, thereby at PyC coat carbon fiber surface preparation acquisition SiO
2The SiC coating of mixing.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 30～150nm, wherein SiO
2Mass fraction be 2%～5%.
Embodiment 6
The difference of this enforcement and embodiment 5 is that cracking process adopts vacuum environment, and used stove is vacuum drying oven, is warming up to 1200 ℃ with the speed of 8 ℃/min, is incubated 1 hour.Other steps are identical with embodiment 5.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 30～150nm, wherein SiO
2Mass fraction be 2%～5%.
Embodiment 7
The difference of present embodiment and embodiment 5 is that the mass fraction of PCS in the precursor solution is that the mass fraction of 6%, TEOS is 2%.Other steps are identical with embodiment 5.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 20～100nm, wherein SiO
2Mass fraction be 1.5%～3.7%.
Embodiment 8
The difference of this enforcement and embodiment 7 is that cracking process adopts vacuum environment, and used stove is vacuum drying oven, is warming up to 1200 ℃ with the speed of 8 ℃/min, is incubated 1 hour.Other steps are identical with the specific embodiment 7.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 20～100nm, wherein SiO
2Mass fraction be 1.5%～3.7%.Embodiment 9
The difference of present embodiment and embodiment 5 is cracking process, and temperature rises to 1000 ℃ with the speed of 4 ℃/min, is incubated 2 hours, carries out Pintsch process under the argon gas atmosphere protection.Other steps are identical with embodiment 5.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 30～150nm, wherein SiO in the SiC coating
2Mass fraction be 2%～5%.Embodiment 10
The difference of present embodiment and embodiment 6 is that cracking process adopts vacuum environment, is warming up to 1200 ℃ with the speed of 8 ℃/min, is incubated 2 hours.Other steps are identical with embodiment 6.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 30～150nm, wherein SiO
2Mass fraction be 2%～5%.
Embodiment 11
Adopt mortar that PCS is worn into fine powder, PCS and TEOS are added in the dimethylbenzene by a certain percentage, stirring and dissolving, the preparation precursor solution, wherein the mass fraction of PCS is that the mass fraction of 20%, TEOS is 20%.The prefabricated carbon fiber body of band PyC coating, the carbon fiber diameter is 6～8 μ m, the PyC coating layer thickness is 400～700nm.Adopted above-mentioned precursor solution pressure impregnation prefabricated carbon fiber body 60 minutes, pressure is 2.5Mpa.After the prefabricated carbon fiber body took out, 220 ℃ of air atmosphere constant temperature were cured processing in 2 hours.Subsequently precast body is placed graphite crucible, together put into stove, used stove is atmosphere furnace; temperature rises to 1300 ℃ by room temperature with the speed of 10 ℃/min; be incubated 1 hour, under the argon gas atmosphere protection, carry out Pintsch process, thereby obtain SiO in PyC coat carbon fiber surface preparation
2The SiC coating of mixing.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 60～400nm, wherein SiO
2Mass fraction be 3%～7.5%.
Embodiment 12
Adopt mortar that PCS is worn into fine powder, PCS and TEOS are added in the dimethylbenzene by a certain percentage, stirring and dissolving, the preparation precursor solution, wherein the mass fraction of PCS is that the mass fraction of 2.5%, TEOS is 1.25%.The prefabricated carbon fiber body of band PyC coating, fibre diameter is 6～8 μ m, the PyC coating layer thickness is 400～700nm.Adopted above-mentioned precursor solution pressure impregnation prefabricated carbon fiber body 10 minutes, pressure is 1Mpa.After the prefabricated carbon fiber body took out, 160 ℃ of air atmosphere constant temperature were cured processing in 1 hour.Subsequently precast body is placed graphite crucible, together put into stove, used stove is atmosphere furnace; temperature rises to 1300 ℃ by room temperature with the speed of 2 ℃/min; be incubated 1 hour, under the argon gas atmosphere protection, carry out Pintsch process, thereby obtain SiO in PyC coat carbon fiber surface preparation
2The SiC coating of mixing.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is about 10～50nm, wherein SiO
2Mass fraction be 2%～5%.
Embodiment 13
Adopt mortar that PCS is worn into fine powder, PCS and TEOS are added in the dimethylbenzene by a certain percentage, stirring and dissolving, the preparation precursor solution, wherein the mass fraction of PCS is that the mass fraction of 10%, TEOS is 5%.The prefabricated carbon fiber body of band PyC coating, the carbon fiber diameter is 6～8 μ m, the PyC coating layer thickness is 400～700nm.Adopted above-mentioned precursor solution pressure impregnation prefabricated carbon fiber body 20 minutes, pressure is 2Mpa.After the prefabricated carbon fiber body took out, 180 ℃ of air atmosphere constant temperature were cured processing in 1.5 hours.Subsequently precast body is placed graphite crucible, together put into stove, used stove is atmosphere furnace.Temperature rises to 1000 ℃ by room temperature with the speed of 4 ℃/min, is incubated 1 hour, carries out Pintsch process under the argon gas atmosphere protection.Repeat pressure impregnation-curings processing-Pintsch process 4 times, thereby at PyC coat carbon fiber surface preparation acquisition SiO
2The SiC coating of mixing.The SiO of present embodiment preparation
2The SiC coating layer thickness that mixes is 60～300nm, wherein SiO
2Mass fraction be 2%～5%.
The PyC/SiC coat carbon fiber precast body that embodiment 1 and embodiment 5 are prepared carries out ESEM, as Fig. 1～3.Doping SiO among Fig. 1
2Very thin of SiC coating, the doping SiO among Fig. 2
2The SiC coating obviously thicken, simultaneously on the carbon fiber of the complete coating band of coating PyC, do not have defectives such as obvious crackle, cavity, as seen, repetition pressure impregnation-curing processing-Pintsch process step can increase coating layer thickness, simultaneously, can fill last layer doping SiO
2The SiC coating in crackle and cavity, improve coating quality.The SEM of higher multiple shows that the SiC coating is very complete among Fig. 3, does not have gross imperfections such as obvious crackle and cavity.The PyC/SiC coat carbon fiber precast body that embodiment 5 is prepared carries out the single pass Electronic Speculum after 700 ℃ of oxidation 10min again in air, as described in Figure 4.Carbon fiber and PyC coating interface generation oxidation, but this moment, coating was still more complete, can hinder the diffusion of oxygen.The present invention has carried out static oxidation to carbon fiber and the present invention of uncoated carbon fiber, PyC coating through the PyC/SiC coat carbon fiber (embodiment 5 and 6) of different cracking temperature preparations, and its curve map is seen Fig. 5.As can be seen from the figure, the antioxygenic property of PyC coat carbon fiber and PyC/SiC coat carbon fiber obviously improves, and initial oxidation temperature obviously increases, and wherein the antioxygenic property of PyC/SiC coat carbon fiber is best, initial oxidation temperature is the highest, and oxidation rate obviously descends.Simultaneously, the antioxygenic property height of the coat carbon fiber of 1000 ℃ of cracking of 1200 ℃ of ratios, this be because, the coating of 1200 ℃ of cracking is crystal structure, antioxidative stabilizer is higher; And the coating of 1000 ℃ of cracking is amorphous state, and antioxidative stabilizer is relatively poor.
Claims (6)
1. a carbon fiber ORC is characterized in that, described carbon fiber ORC is SiO
2The SiC coating of mixing, wherein, SiO
2Mass fraction be 1%～10%, SiO
2The SiC coating of mixing overlays on the carbon fiber surface of the prefabricated carbon fiber body of being with pyrocarbon coating.
2. carbon fiber ORC according to claim 1 is characterized in that, described SiO
2The SiC coating layer thickness that mixes is greater than 0 μ m and less than 1 μ m.
3. carbon fiber ORC according to claim 1 is characterized in that, the carbon fiber diameter of the prefabricated carbon fiber body of described band pyrocarbon coating is 6～8 μ m, and pyrocarbon coating thickness is 400～700nm.
4. a method for preparing the described carbon fiber ORC of claim 1 is characterized in that, may further comprise the steps:
Step 1, Polycarbosilane and ethyl orthosilicate added stirring and dissolving makes precursor solution in the dimethylbenzene, wherein, the mass fraction of Polycarbosilane is 2.5%～20%, and the mass fraction of ethyl orthosilicate is 1.25%～20%;
Step 2, with the prefabricated carbon fiber body of the precursor solution pressure impregnation band pyrocarbon coating that obtains in the step 1, wherein impregnation pressure is 1～2.5Mpa, dip time 10～60min;
Step 3, the prefabricated carbon fiber body that obtains in the step 2 is cured processing, wherein, solidifying the temperature of handling is 160～220 ℃, and solidifying the atmosphere of handling is air, and solidifying the time of handling is 1～2h;
Step 4, the prefabricated carbon fiber body that obtains in the step 3 is carried out Pintsch process, wherein, cracking temperature is 1000～1300 ℃, heating rate is 2～10 ℃/min, cracking atmosphere is argon gas or vacuum, the cracking temperature retention time is 1～2h, and namely the carbon fiber surface at the prefabricated carbon fiber body of being with pyrocarbon coating prepares complete SiO
2The SiC coating of mixing.
5. the preparation method of carbon fiber ORC according to claim 4 is characterized in that, the carbon fiber diameter of the prefabricated carbon fiber body of band pyrocarbon coating is 6～8 μ m in the described step 2, and pyrocarbon coating thickness is 400～700nm.
6. the preparation method of carbon fiber ORC according to claim 4 is characterized in that, repeatedly circulation step two is to step 4, and wherein cycle-index is 1～4 time.
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