CN104212168A - Preparation method of SiC nanowire modified CF/PI composite material - Google Patents
Preparation method of SiC nanowire modified CF/PI composite material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K7/02—Fibres or whiskers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/10—Silicon-containing compounds
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a preparation method of a SiC nanowire modified CF/PI composite material. The method comprises the following steps: dipping carbon fibers through a Czochralski technology, preparing a SiC nanowire through a silicon powder evaporation technology, and preparing the carbon fiber reinforced polyimide (CF/PI) composite material through a compression molding technology. The method has the advantages of simplicity, easy operation and low cost. The SiC nanowire modified CF/PI composite material has the advantages of good corrosion and heat resistance, and substantially improved mechanical strength, and has very important practical application in the fields of heat-resistant aerospace materials and structure support materials.
Description
Technical field
The modified carbon fiber that the present invention relates to a kind of silicon carbide (SiC) nano wire strengthens the preparation method of polyimide (CF/PI) matrix material.
Background technology
Along with aerospace development, people to the high-temperature behavior of material and the requirement of mechanical property more and more higher, traditional metal materials has been difficult to meet the requirement of field of aerospace to the high-strength light character of material, and matrix material especially fibre reinforced based advanced composite material because of its high specific strength, high ratio modulus, designability, the advantage such as high temperature resistant, becomes space flight and aviation preferred material.
Compared to other polymer matrixes, polyimide (PI) has excellent thermostability, thermotolerance, erosion resistance etc., can meet existing satellite, aircraft etc. to the more and more higher requirement of material keeps long-term structural stability, and the pyrolysis product produced in operational process is little for environmental pollution.Therefore, fibre reinforced polyimide-based composite material has very large using value in space flight and aviation, military field.But the processing characteristics of polyimide is poor, carbon fiber surface is inertia in addition, and the interface be compounded to form is therefore more weak, and this causes very large restriction to the performance and application of carbon fiber reinforcement polyimide composite material.
In order to improve carbon fiber and polyimide matrix interface bond strength, need to carry out modification to carbon fiber.The domestic and international research to carbon fiber surface modification is at present a lot, and SiC material, because of many excellent characteristics such as it are high temperature resistant, radiation hardness, thermal expansivity are low, chemical stability good, mechanical property is high, is widely used for modified carbon fiber.Research shows, the elasticity of single SiC nanowire or nanometer rod and intensity are far longer than the intensity of bulk SiC crystal. in recent years, the mechanical property of SiC nanowire (rod) and application in the composite cause the attention of scientist again.Lieber study group utilizes the SiC nanometer rod of atomic force microscope to preparation to carry out mechanics performance determining, find that the Young's modulus of single SiC nanometer rod is 610 1 660GPa, close to theoretical expectation values (about 600GPa), the maximum deflection intensity 53.4GPa of SiC nanometer rod is the twice of micron whisker.The people such as Wang Zhonglin also record the Young's modulus of the coaxial nanostructure SiC of different diameter SiO2/SiC, and observe directly the superplasticity of SiC nanowire under scanning electron microscope.
Have about the patent of silicon carbide nanometer line at flexible substrate grown on carbon fibers at present, as CN102951919A discloses a kind of method that SiC nanowire grows in C/SiC matrix material, the method is that carbon fibre fabric is put in vacuum impregnation in Polycarbosilane solution, then Pintsch process obtains the ceramic matric composite of growth in situ SiC nanowire, it is abundant not that the method can cause carbon fibre fabric to flood, finally cause matrix material porosity high, affect its mechanical property.CN102828249A disclose a kind of can the method for grown on larger scale high-quality single-crystal silicon carbide nanowires array on flexible substrates, carbon fiber is as carbon source and substrate, and silica flour is as silicon source, and equipment is simple, cost is low, but the silicon carbide nanometer line of preparation reduces the mechanical property of carbon fiber.
First the present invention utilizes crystal pulling method, adopts the carbon fiber of the dispersion liquid dipping of expanded graphite as carbon source, then prepares the acid of SiC nanowire modified polyamide by silica flour method of evaporation, prepare CF/PI matrix material finally by compression molding method.Method abundant raw material source of the present invention, cost is lower, workable, and the CF/PI obtained not only has thermotolerance and the mechanical property of improvement, also has the interface cohesion situation of the CF/PI of improvement.
Summary of the invention
In first aspect, the invention provides the preparation method of the CF/PI matrix material of all excellent SiC nanowire modification of a kind of thermotolerance, radioprotective, mechanical property, described method comprises the steps:
1) step of crystal pulling method impregnation of carbon fibers is utilized, described step is: be scattered in by expanded graphite in organic solvent, ultrasonic preparation becomes finely dispersed graphite suspension, pulling coating machine is utilized to make described finely dispersed graphite suspension liquid be immersed in the surface of carbon cloth, subsequently in vacuum drying oven to dipping after described carbon cloth heat treated, obtain lift after carbon cloth;
2) silica flour method of evaporation prepares the step of SiC nanowire, and described step is: SiO powder is put into alumina crucible, then uses step 1) carbon cloth after the described lift that obtains covers, pushes down above carbon cloth with lid again; This reaction unit is put into tube furnace, is heated to 1200 DEG C-1600 DEG C under ar gas environment, insulation 2h-6h, naturally cools to room temperature;
3) step of prepreg is prepared, described step is: the diamines of drying is dissolved in N, in N-dimethylacetamide solvent, and in reaction vessel logical nitrogen, carry out after mechanical stirring to diamines all dissolves, in reaction vessel, adding dianhydride, be stirred to and dissolve completely, obtain the polyamic acid solution of brown color, utilize described polyamic acid solution to step 2) product flood, make prepreg;
4) compression molding method obtains the step of the carbon fiber reinforcement polyimide composite material of SiC nanowire modification, described step is: by step 3) prepreg that obtains is placed on preheating in Electric heat oven, make solvent evaporates wherein, preheating temperature is 80 DEG C, and the time is 5-10h; Then put it into and scribble in the mould of releasing agent, platen-press plate put into by mould, and adjustment pressure is 0.5-2MPa, is heated to 100 DEG C, 140 DEG C, 180 DEG C and 220 DEG C successively, and each stage insulation 1-3h; After being incubated, stop heating, naturally cooling, until temperature drops to room temperature, obtain the carbon fiber reinforcement polyimide composite material of SiC nanowire modification.
In second aspect, the invention provides the carbon fiber reinforcement polyimide composite material of the SiC nanowire modification prepared by the method for first aspect.
Beneficial effect
Method technological process safety of the present invention, without the need to expensive device, and operating process is simple; Step 2) the SiC nanowire purity that obtains is high and be distributed in carbon fiber top layer in bar-shaped.Thermotolerance, the strength and stiffness of the carbon fiber reinforcement polyimide composite material of SiC nanowire modification prepared according to the methods of the invention are all significantly improved.Matrix material of the present invention can be applicable to the fields such as aerospace heat-stable material and structural support material.
Accompanying drawing explanation
Fig. 1 is the step 1 of the inventive method) in the fundamental diagram of pulling machine that uses; Wherein 1 is electric motor, for pulling machine provides power; 2 is wire drawing, connects electric motor and substrate; 3 is Controlling System, can be used for regulating pull rate, and controls operation and the stopping of pulling machine; 4 is solution tank, conveniently puts into wherein by the container that solution is housed; 5 is beaker, holds coated solution; 6 is coated solution; 7 is fixture, is used for clamping substrate; 8 is substrate.
Fig. 2 is the step 2 according to the inventive method) prepare the setting drawing of SiC nanowire;
Fig. 3 is the temperature control figure of the CF/PI matrix material of preparation SiC nanowire modification.
Fig. 4 is the step 2 according to the embodiment of the present invention 1) the SEM figure of the SiC nanowire prepared.
Fig. 5 is the step 4 according to the embodiment of the present invention 1) the profile scanning figure of the CF/PI matrix material of SiC nanowire modification for preparing.
Embodiment
In one preferred embodiment, described step 1) in, pull rate when utilizing pulling coating machine described finely dispersed graphite suspension liquid to be immersed in carbon cloth surperficial is 2mm/min-5mm/min, and the lift time is 30min-2h.
In one preferred embodiment, described step 1) in, described organic solvent is selected from dehydrated alcohol, DMF and N,N-dimethylacetamide; The solid content of described graphite suspension is 3wt%-20wt%.
In one preferred embodiment, described step 2) in, the mass ratio of the SiO powder added and the carbon fiber after lifting is 1:3-1:10.
In one preferred embodiment, described step 2) in, described ar gas environment is: described tube furnace is evacuated to 2Pa, is then filled with argon gas to 400Pa, is again evacuated to 2Pa, and then is filled with argon gas to 400Pa, closes argon gas source.
In one preferred embodiment, described step 3) in, the carbon fiber content in described prepreg is 10wt%-50wt%.
In one preferred embodiment, described step 3) in, described diamines is 4,4 '-diaminodiphenyl oxide, described dianhydride is 3,3 ', 4,4 '-tetracarboxylic benzophenone acid anhydride, be further characterized in that, the mass ratio of described diamines and dianhydride is 1.02:1, and described diamines is dissolved in N, in the solution that N-dimethylacetamide solvent obtains, solid content is 8wt%-30wt%.
In one preferred embodiment, the preparation method of the CF/PI matrix material of SiC nanowire modification of the present invention comprises the steps:
1) crystal pulling method impregnation of carbon fibers is utilized
Measured amounts expanded graphite, is scattered in organic solvent, and ultrasonic 4-15h makes suspension.Utilize pulling coating machine by the surface of finely dispersed coated with graphite at carbon cloth (200mm × 50mm), pull rate is 2mm/min-5mm/min.Then carbon cloth is carried out heat treated in vacuum drying oven.Described pulling machine principle is see figure Fig. 1.
2) SiC nanowire is prepared
By a certain amount of SiO powder (purity 99.99%, mean particle size 73 μm, density 2.1g/cm
3) put into alumina crucible, then cover with the carbon cloth after dipping, push down with lid again above carbon cloth; Whole reaction unit puts into tube furnace, vacuumizes 2Pa, is then filled with argon gas to 400Pa, is again evacuated to 2Pa, and then is filled with argon gas to 400Pa, closes argon gas source.Be heated to 1200 DEG C-1600 DEG C, insulation 2h-6h, then naturally cools to room temperature.Step 2) reaction unit as Fig. 2.
3) prepreg is prepared
Take 4 of a certain amount of drying, 4 '-diaminodiphenyl oxide (ODA) is dissolved in N, in N-N,N-DIMETHYLACETAMIDE (DMAC) solvent (solid content is 8%-30%), and nitrogen is led in reaction vessel, carry out mechanical stirring to 4, after 4 '-diaminodiphenyl oxide all dissolves, according to 3, 3 ', 4, 4 '-tetracarboxylic benzophenone acid anhydrides: 4, the ratio of 4 '-diaminodiphenyl oxide=1.02:1 takes 3, 3 ', 4, 4 '-tetracarboxylic benzophenone acid anhydrides (BTDA), being divided by BTDA three times adds in reaction vessel, ensure to dissolve completely and stir 5-8h, obtain polyamic acid (PAA) solution of brown color.Last repeatedly homogeneous impregnation carbon cloth, makes prepreg.
4) carbon fiber reinforcement polyimide composite material of SiC nanowire modification is obtained
The prepreg prepared is placed on preheating in Electric heat oven, makes solvent evaporates wherein, preheating temperature is 80 DEG C, and the time is 5-10h; Then put it into and scribble in the mould of releasing agent, platen-press plate put into by mould, and adjustment pressure is 0.5-2MPa, according to Fig. 3 design temperature and soaking time.After being incubated, stop heating, naturally cooling, until temperature drops to room temperature.
Wherein, organic solvent is preferably from dehydrated alcohol, DMF (DMF) and DMAC; Graphite suspension solid content is 3%-20%, and the lift time is 30min-2h; SiO powder quality: carbon fiber quality (after lift)=1:3-1:10; In prepreg, carbon fiber content is 10%-50%, a small amount of oxygen of the growth needs due to SiC nanowire, so carry out sintering reaction under partial vacuum.
Embodiment:
Below in conjunction with embodiment, explanation is further explained to method of the present invention.Protection scope of the present invention is not limited to these embodiments.
Embodiment 1:
1. utilize crystal pulling method impregnation of carbon fibers
Measure 2g expanded graphite, be scattered in 40ml dehydrated alcohol, ultrasonic 8h makes suspension.Utilize pulling coating machine by the surface of finely dispersed coated with graphite at carbon cloth (200mm × 50mm), with the pull rate of 2mm/min lift 1h.Then carbon cloth is placed in vacuum drying oven, takes out for subsequent use after 80 DEG C of insulation 5h.
2. prepare SiC nanowire
Measure SiO powder 2g (purity 99.99%, mean particle size 73 μm, density 2.1g/cm
3) put into alumina crucible, then cover with the carbon cloth after dipping, push down with lid again above carbon cloth; Whole reaction unit puts into tube furnace, is evacuated to 2Pa, then passes into argon shield, and argon flow amount is 100ml/min, closes argon gas source to during 400Pa.Be heated to 1400 DEG C, insulation 4h, then naturally cools to room temperature.
The SEM figure of the SiC nanowire obtained is shown in Fig. 4, can find out, the SiC nanowire purity of acquisition is high and be distributed in carbon fiber top layer in bar-shaped.
3. prepare prepreg
The ODA taking the drying of 12g is dissolved in the DMAC solvent of 110ml, and nitrogen is led in reaction vessel, carry out after mechanical stirring to diamines all dissolves, according to dianhydride: the ratio of diamines=1.02:1 takes BTDA, being divided by BTDA three times adds in reaction vessel, ensure to dissolve completely and stir 8h, obtain the polyamic acid PAA solution of brown color.Last repeatedly homogeneous impregnation carbon cloth, makes prepreg.
4. obtain the carbon fiber reinforcement polyimide composite material of SiC nanowire modification
The prepreg prepared is placed on preheating in Electric heat oven, makes solvent evaporates wherein, preheating temperature is 80 DEG C, and the time is 5h; Then put it into and scribble in the mould of releasing agent, platen-press plate put into by mould, and adjustment pressure is 0.5MPa, by Fig. 3 design temperature and soaking time.After being incubated, stop heating, naturally cooling, until temperature drops to room temperature.
The profile scanning figure of the carbon fiber reinforcement polyimide composite material of the SiC nanowire modification that step 4 obtains as shown in Figure 5.
Embodiment 2
1. utilize crystal pulling method impregnation of carbon fibers
Measure 3g expanded graphite, be scattered in 60mlDMF solvent, ultrasonic 10h makes suspension.Utilize pulling coating machine by the surface of finely dispersed coated with graphite at carbon cloth (200mm × 50mm), with the pull rate of 3mm/min lift 1h.Then carbon cloth is placed in vacuum drying oven, takes out for subsequent use after 80 DEG C of insulation 6h.
2. prepare SiC nanowire
Measure SiO powder 3g (purity 99.99%, mean particle size 73 μm, density 2.1g/cm
3) put into alumina crucible, then cover with the carbon cloth after dipping, push down with lid again above carbon cloth; Whole reaction unit puts into tube furnace, vacuumizes 2Pa, is then filled with argon gas to 400Pa, is again evacuated to 2Pa, and then is filled with argon gas to 400Pa, closes argon gas source.Be heated to 1300 DEG C, insulation 6h, then naturally cools to room temperature.
3. prepare prepreg
The ODA taking the drying of 15g is dissolved in the DMAC solvent of 120ml, and nitrogen is led in reaction vessel, carry out after mechanical stirring to diamines all dissolves, according to dianhydride: the ratio of diamines=1.02:1 takes BTDA, being divided by BTDA three times adds in reaction vessel, ensure to dissolve completely and stir 6h., obtain the polyamic acid PAA solution of brown color.Last repeatedly homogeneous impregnation carbon cloth, makes prepreg.
4. obtain the carbon fiber reinforcement polyimide composite material of SiC nanowire modification
The prepreg prepared is placed on preheating in Electric heat oven, makes solvent evaporates wherein, preheating temperature is 80 DEG C, and the time is 6h; Then put it into and scribble in the mould of releasing agent, platen-press plate put into by mould, and adjustment pressure is 1MPa, by Fig. 3 design temperature and soaking time.After being incubated, stop heating, naturally cooling, until temperature drops to room temperature.
Embodiment 3:
1. utilize crystal pulling method impregnation of carbon fibers
Measure 4g expanded graphite, be scattered in 70mlDMF solvent, ultrasonic 12h makes suspension.Utilize pulling coating machine by the surface of finely dispersed coated with graphite at carbon cloth (200mm × 50mm), with the pull rate of 4mm/min lift 1.5h.Then carbon cloth is placed in vacuum drying oven, takes out for subsequent use after 80 DEG C of insulation 5.5h.
2. prepare SiC nanowire
Measure SiO powder 4g (purity 99.99%, mean particle size 73 μm, density 2.1g/cm
3) put into alumina crucible, then cover with the carbon cloth after dipping, push down with lid again above carbon cloth; Whole reaction unit puts into tube furnace, vacuumizes 2Pa, is then filled with argon gas to 400Pa, is again evacuated to 2Pa, and then is filled with argon gas to 400Pa, closes argon gas source.Be heated to 1500 DEG C, insulation 5h, then naturally cools to room temperature.
3. prepare prepreg
The ODA taking the drying of 18g is dissolved in the DMAC solvent of 130ml, and nitrogen is led in reaction vessel, carry out after mechanical stirring to diamines all dissolves, according to dianhydride: the ratio of diamines=1.02:1 takes BTDA, being divided by BTDA three times adds in reaction vessel, ensure to dissolve completely and stir 5h., obtain the polyamic acid PAA solution of brown color.Last repeatedly homogeneous impregnation carbon cloth, makes prepreg.
4. obtain the carbon fiber reinforcement polyimide composite material of SiC nanowire modification
The prepreg prepared is placed on preheating in Electric heat oven, makes solvent evaporates wherein, preheating temperature is 80 DEG C, and the time is 8h; Then put it into and scribble in the mould of releasing agent, platen-press plate put into by mould, and adjustment pressure is 1.6MPa, by Fig. 3 design temperature and soaking time.After being incubated, stop heating, naturally cooling, until temperature drops to room temperature.
Claims (9)
1. obtain a method for the carbon fiber reinforcement polyimide composite material of SiC nanowire modification, described method comprises the steps:
1) step of crystal pulling method impregnation of carbon fibers is utilized, described step is: be scattered in by expanded graphite in organic solvent, ultrasonic preparation becomes finely dispersed graphite suspension, pulling coating machine is utilized to make described finely dispersed graphite suspension liquid be immersed in the surface of carbon cloth, subsequently in vacuum drying oven to dipping after described carbon cloth heat treated, obtain lift after carbon cloth;
2) silica flour method of evaporation prepares the step of SiC nanowire, and described step is: SiO powder is put into alumina crucible, then uses step 1) carbon cloth after the described lift that obtains covers, pushes down above carbon cloth with lid again; This reaction unit is put into tube furnace, is heated to 1200 DEG C-1600 DEG C under ar gas environment, insulation 2h-6h, naturally cools to room temperature;
3) step of prepreg is prepared, described step is: the diamines of drying is dissolved in N, in N-dimethylacetamide solvent, and in reaction vessel logical nitrogen, carry out after mechanical stirring to diamines all dissolves, in reaction vessel, adding dianhydride, be stirred to and dissolve completely, obtain the polyamic acid solution of brown color, utilize described polyamic acid solution to step 2) product flood, make prepreg;
4) compression molding method obtains the step of the carbon fiber reinforcement polyimide composite material of SiC nanowire modification, described step is: by step 3) prepreg that obtains is placed on preheating in Electric heat oven, make solvent evaporates wherein, preheating temperature is 80 DEG C, and the time is 5-10h; Then put it into and scribble in the mould of releasing agent, platen-press plate put into by mould, and adjustment pressure is 0.5-2MPa, is heated to 100 DEG C, 140 DEG C, 180 DEG C and 220 DEG C successively, and each stage insulation 1-3h; After being incubated, stop heating, naturally cooling, until temperature drops to room temperature, obtain the carbon fiber reinforcement polyimide composite material of SiC nanowire modification.
2. the method for claim 1, it is characterized in that, described step 1) in, pull rate when utilizing pulling coating machine described finely dispersed graphite suspension liquid to be immersed in carbon cloth surperficial is 2mm/min-5mm/min, and the lift time is 30min-2h.
3. the method for claim 1, is characterized in that, described step 1) in, described organic solvent is selected from dehydrated alcohol, DMF and N,N-dimethylacetamide; Be further characterized in that, the solid content of described graphite suspension is 3wt%-20wt%.
4. the method for claim 1, is characterized in that, described step 2) in, the mass ratio of the SiO powder added and the carbon fiber after lifting is 1:3-1:10.
5. the method for claim 1, is characterized in that, described step 2) in, described ar gas environment is: described tube furnace is evacuated to 2Pa, is then filled with argon gas to 400Pa, is again evacuated to 2Pa, and then be filled with argon gas to 400Pa, close argon gas source.
6. the method for claim 1, is characterized in that, described step 3) in, the carbon fiber content in obtained prepreg is 10wt%-50wt%.
7. the method according to any one of claim 1-6, is characterized in that, described step 3) in, described diamines is 4,4 '-diaminodiphenyl oxide, and described dianhydride is 3,3 ', 4,4 '-tetracarboxylic benzophenone acid anhydride, is further characterized in that, the mass ratio of described diamines and dianhydride is 1.02:1, described diamines is dissolved in the solution that N,N-dimethylacetamide solvent obtains, and solid content is 8wt%-30wt%.
8. the carbon fiber reinforcement polyimide composite material of the SiC nanowire modification that the method according to any one of claim 1-7 obtains.
9. the purposes of carbon fiber reinforcement polyimide composite material in aerospace heat-stable material and structural support material field of SiC nanowire modification as claimed in claim 8.
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| CN110294632A (en) * | 2019-05-05 | 2019-10-01 | 上海大学 | A kind of preparation method of the carbon fiber three-dimensional fabric enhancing carbon-based double base matrix composite of polyimides- |
| CN112961383A (en) * | 2021-02-17 | 2021-06-15 | 中南大学 | Low-filler-content field-sensitive nonlinear conductive composite film and preparation method thereof |
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| CN109385039A (en) * | 2017-08-14 | 2019-02-26 | 王斌 | Carbon fiber-reinforced resin compounded mix manufacturing method |
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| CN104212168B (en) | 2017-01-11 |
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