CN107673773A - The preparation method of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon - Google Patents
The preparation method of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon Download PDFInfo
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- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
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- C04B2235/5252—Fibers having a specific pre-form
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Abstract
The present invention provides a kind of preparation method of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon, successfully graphene oxide is introduced into the Carbon fibe precast body of C/SiC composites by hydrothermal chemistry reducing process, construct multi-component multi-dimension network structure, graphene Carbon fibe precast body is made, recycles chemical vapor infiltration (CVI) process deposits SiC matrix to prepare graphene and is modified C/SiC composites.Method provided by the invention makes graphene carry out self assembly with Carbon fibe precast body, with Carbon fibe bonding action occurs for graphene, construct the multi-component multi-dimension precast body with network structure being made up of two-dimensional graphene and Carbon fibe, to give full play to modifying function of the graphene to the performance such as the mechanics of C/SiC composites, high temperature resistant, wear-resisting, electromagnetic shielding, the advantages of using electronation self-assembly process and simple and controllable CVI techniques, it can effectively control grapheme material and the pattern and structure of SiC matrix.
Description
Technical field
The present invention relates to composite technology of preparing, and in particular to a kind of graphene Modified Activated Carbon is silicon carbide fiber reinforced compound
The preparation method of material.
Background technology
C/SiC composites are the composites of charcoal pricker dimension enhancing silicon carbide substrate, combine the good high temperature power of Carbon fibe
Learn the high-temperature oxidation resistance of performance and silicon carbide substrate.C/SiC composites are widely used as high temperature thermal structure material
In aerospace field, such as engine nozzle, aircraft brake piece, rocket motor nozzle, larynx lining, the space shuttle leading edge of a wing
Deng still, the use environment of each component is different, and its mechanical property requirements is also not quite similar.With the hair of aerospace flight vehicle
Exhibition, aerospace field propose higher to intensity of the carbon fibre reinforced ceramics based composites under extreme severe rugged environment and toughness
It is required that while, to having excellent mechanics, high temperature resistant concurrently with inhaling the structure of the performances such as ripple and the preparation of function integration material with setting
Meter also gradually proposes new requirement.Nano material compares block materials, has great specific surface area and more excellent mechanics
Performance, while the performances such as many special novel optics, electricity are shown, nano material is introduced into composite, can be effective
Improve the mechanical properties such as its intensity and fracture toughness and some functional characteristics.Therefore, using nanometer technology, one is entered in nanoscale
Walking improved C/SiC composites comprehensive mechanical property and functional characteristic turns into a kind of feasible and effective method.
Graphene is a kind of individual layer two-dimensional nano by carbon atom by the side's assymetric crystal of Covalent bonding together formation rule six
Structural material, its own has the performances such as extremely superior mechanics, electricity, and intensity is far above Carbon fibe.In view of graphene is excellent
Good mechanical characteristic, graphene are introduced in the materials such as macromolecule and alloy as matrix dopants, to obtain with excellent
The composite of mechanical property.Ramanathan etc. adds functionalized graphite's alkene that the chemical groups such as hydroxyl, carboxyl are contained on surface
Enter into some polarity macromolecules, such as polymethyl-benzene e pioic acid methyl ester, it is compound to have prepared graphene/polymethyl-benzene olefin(e) acid formicester etc.
Material, research show that the mechanical property of polymethyl-benzene olefin(e) acid formicester can be effectively improved by adding the graphene of a small amount of functionalization, its
Enhancing effect is better than single-walled nanotube and expanded graphite alkene.2013, Sony corporation of Japan used chemical vapor deposition and transfer
Method prepare lightweight, high intensity, graphene/copper foil alloy material of obdurability.It is the high-specific surface area of graphene, excellent
The characteristics such as mechanical property become the preferable packing material for improving composite materials property.
At present, one-dimensional CNT activeness and quietness C/SiC composites are largely reported, and are still suffered from some and asked
Topic, and graphene is modified C/SiC composites and prepares nearly no report.
Such as：“Wang L,Hou F,Wang X,et al.Preparation and Mechanical Properties
of Continuous Carbon Nanotube Networks Modified C f/SiC Composite[J].Advances
in Materials Science&Engineering,2015,2015(12):1-7. " utilizes freeze-drying and precursor
Impregnating cracking technology prepares the modified C/SiC composites of CNT (CNTs).CNT (CNTs) prepared by this method changes
Property C/SiC composites, compared to the composite for not adding CNT, interface shear strength (ILSS) and Carbon fibe/carbon
The bending strength of nanometer tube composite materials adds 31% and 27% respectively.Excessive CNT (CNTs) is attached in the technique
On carbon fiber surface, space between the fibers is difficult to form tridimensional network, in matrices of composite material bridge joint effect compared with
It is small.
“Hu J,Dong S,Wu B,et al.Mechanical and thermal properties of Cf/SiC
composites reinforced with carbon nanotube grown in situ[J].Ceramics
International,2013,39(3):3387-3391. " is described in polymer impregnated and pyrolytic process, in D refraction statics
In-situ growing carbon nano tube on carbon cloth.The bending strength for the modified C/SiC composites of CNT (CNTs) that this method obtains
15% and 8.7% has been respectively increased with fracture toughness.There is very strong interface bond strength, carbon is received between CNT and matrix
Mitron is brittle fracture.Nitrate (the ferric nitrate, aluminum nitrate) catalyst introduced in the technique, there is corrosion to make to carbon fiber surface
With destroying carbon fiber surface structure, reduce the comprehensive mechanical property of composite.If in addition, in the product obtained this
A little metal ions can not be completely removed, and will influence the high-temperature oxidation resistant and Burning corrosion resistance energy of composite.
Patent " graphene is modified the preparation method of C/SiC heat-resistant composite materials " (Application No. 201611039259.2)
In, graphene has been made in two stages and has been modified C/SiC heat-resistant composite materials.First stage weaves surface-treated Carbon fibe
It is compound that thing is placed in graphene modified boron containing phenolic resin solution dipping, vacuum vibration, then by the Carbon fibe containing dipping solution
Carbon fibe precast body is made in braid solidification, Pintsch process；Obtained Carbon fibe precast body is placed in graphene and changed by second stage
Property precursor solution in dipping, vacuum vibration it is compound, then by containing dipping solution Carbon fibe precast body solidification, high anneal crack
Solution, second stage process is repeated several times graphene modification C/SiC composite blanks are made, finally by C/SiC composite hairs
Base carries out machining and graphene modification C/SiC heat-resistant composite material products is prepared.This method mainly utilizes organic precursor
Body Pintsch process is made graphene and is modified C/SiC heat-resistant composite materials, but organic precursor method Pintsch process may be anti-because cracking
The structural intergrity of graphene and Carbon fibe should be destroyed, reduces their mechanical properties as reinforcing material.In addition, the party
Method carries out that dipping precursor solution, solidification, Pintsch process is repeated several times, and preparation technology is sufficiently complex.
The content of the invention
In view of this, the present invention provides a kind of technique the simple and controllable silicon carbide fiber reinforced (C/ of graphene Modified Activated Carbon
SiC) the preparation method of composite, the Carbon fibe precast body of graphene oxide and surface functionalization is self-assembly of
Graphene-Carbon fibe precast body, it is prefabricated that SiC is then deposited into graphene-Carbon fibe using chemical vapor infiltration technique (CVI)
The graphene that multi-component multi-dimension is formed in body is modified C/SiC composites.
The preparation method of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon provided by the invention, including following step
Suddenly：
(1) preparation of dipping solution：The reduction added into the graphene oxide solution that concentration is 1mg/mL~10mg/mL
Agent, dipping solution is uniformly mixed so as to obtain, standby, the mass ratio of the reducing agent and graphene oxide is 1:1~1:10；
(2) preparation of surface functionalization Carbon fibe precast body：After Carbon fibe precast body is cleaned with acetone ultrasound, it is placed in
1h~4h is handled in high concentration nitric acid at 85 DEG C~95 DEG C, is put into after taking-up in the ethanol water that concentration is 5%~40%
Dialysis treatment at least 24h, then the Carbon fibe after dialysis treatment is taken out and dried at 40 DEG C~65 DEG C, produce surface functionalization
Carbon fibe precast body；
(3) preparation of multi-component multi-dimension graphene-Carbon fibe precast body：By obtained surface functionalization in step (2)
Carbon fibe precast body is placed in step (1) vacuum impregnation in obtained dipping solution and handles 0.5h~2h, then by after processing
Carbon fibe takes out hydrothermal chemistry reduction reaction 4h~6h at 70 DEG C~95 DEG C, and it is pre- to produce multi-component multi-dimension graphene-Carbon fibe
Body processed；
(4) preparation of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon：By obtained polynary more chis in step (3)
Spend graphene-Carbon fibe precast body and SiC matrix is deposited by chemical vapor infiltration, produce graphene Modified Activated Carbon fiber reinforcement carbon
SiClx composite；Wherein, chemical vapor infiltration depositing silicon silicon concrete technology step is as follows：
A, multi-component multi-dimension graphene-Carbon fibe precast body is placed in gaseous phase deposition stove, and will be evacuated in stove
2kPa~3kPa, inertia Ar is then passed through as 200mL/min~800mL/min using flow and is used as protective gas；
B, furnace temperature is risen to 1000 DEG C~1300 DEG C with 5 DEG C/min~10 DEG C/min programming rate, then using flow as
100mL/min~300mL/min is passed through H2, methyl trichlorosilane gas is passed through by 4g/h~20g/h of flow, while adjust stove
Interior pressure is that 2kPa~8kPa carries out deposition reaction, after deposition reaction 20h~120h, stops being passed through reacting gas into stove, makes
In-furnace temperature is down to room temperature naturally, that is, the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon is made；
Further, in the step (1), the graphene oxide solution is graphene oxide ethanol solution or graphite oxide
Aqueous solution；The reducing agent is ascorbic acid；
Further, described graphene oxide, ascorbic acid, ethanol and methyl trichlorosilane are that analysis is pure；The Ar,
H2It is more than 99.999% high-purity gas for purity.
Beneficial effects of the present invention：The present invention is prefabricated in Carbon fibe first with graphene oxide hydrothermal chemistry reduction reaction
Internal portion is self-assembly of three-dimensional network skeleton, and the graphene oxide-Carbon fibe for constructing multi-component multi-dimension network structure is prefabricated
Body, then SiC is deposited in graphene modified carbon fiber precast body using chemical vapor infiltration technique (CVI) and forms graphene
The silicon carbide fiber reinforced composite of Modified Activated Carbon (graphene is modified C/SiC composites).By drawing in C/SiC composites
Enter graphene, become a kind of graphene/Carbon fibe enhancing SiC based composites of multi-component multi-dimension, improve C/SiC and answer
The comprehensive mechanical property of condensation material；In addition, fracture mode, vesicular structure and the graphite of multiple dimensioned precast body enhancing composite
The excellent mechanics of alkene material, heat conduction and electric conductivity, improve the intensity of C/SiC composites, fracture toughness, anti-oxidant, resistance to
The performances such as high temperature, wear-resisting and electromagnetic shielding, to have the Aero-Space structure of excellent mechanics, high temperature resistant with inhaling the performances such as ripple concurrently
Preparation with function integration material provides new thinking with design.Meanwhile the present invention utilizes hydrothermal chemistry reduction self assembly work
The advantages of skill and simple and controllable CVI techniques, it can effectively control grapheme material and the pattern and structure of SiC matrix.
Brief description of the drawings
The present invention is further described with specific embodiment below in conjunction with the accompanying drawings.
Fig. 1 is flow chart of the method for the present invention；
Fig. 2 is the graphene -2D Carbon fibe precast body microscopic appearances prepared by embodiment one；
Fig. 3 is graphene-overall Carbon fibe precast body microscopic appearance prepared by embodiment two；
Fig. 4 is that graphene modification 2D Carbon fibes precast body enhancing carborundum (SiC) composite is micro- prepared by embodiment one
See pattern；
Fig. 5 is that graphene prepared by embodiment two is modified overall Carbon fibe precast body enhancing carborundum (SiC) composite
Microscopic appearance.
Embodiment
In following examples, gaseous phase deposition stove is constant-temperature oven.
Embodiment one
The preparation method for the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon that the present embodiment provides, including following step
Suddenly：
(1) preparation of dipping solution：The 40mg added into the graphene oxide ethanol solution that 10ml concentration is 4mg/mL
Ascorbic acid, dipping solution is uniformly mixed so as to obtain, it is standby；
(2) preparation of surface functionalization Carbon fibe precast body：The 2D Carbon fibes precast body cleaned up ultrasound is cleaned
(at least it is cleaned by ultrasonic 10min) afterwards, is placed in the nitric acid that concentration is 68%, 2h is handled at 90 DEG C, being put into concentration after taking-up is
Dialysis treatment 24h in 5% ethanol water, then will be dried in 55 DEG C of baking ovens of 2D Carbon fibes precast body after dialysis treatment, i.e.,
Obtain surface functionalization Carbon fibe precast body；
(3) preparation of multi-component multi-dimension graphene-Carbon fibe precast body：By obtained surface functionalization in step (2)
Carbon fibe precast body is placed in step (1) vacuum impregnation in obtained dipping solution and handled, wherein, vacuum impregnation is handled specific
Method is as follows：Surface functionalization Carbon fibe precast body is put in vacuum impregnation room, vacuumizes 20min, then will be impregnated molten
Liquid is added in funnel, and control funnel liquid feed valve enters in impregnation chamber by solution, and 0.5h is impregnated after vacuumizing, and takes out the charcoal after dipping
Fiber, it is put into 70 DEG C of baking ovens, is taken out after hydrothermal chemistry reduction reaction 4h, it is prefabricated produces multi-component multi-dimension graphene-Carbon fibe
Body (see Fig. 2 graphene -2D Carbon fibe precast bodies microscopic appearance)；
(4) preparation of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon：By obtained polynary more chis in step (3)
Spend graphene-Carbon fibe precast body and SiC matrix is deposited by chemical vapor infiltration, produce graphene Modified Activated Carbon fiber reinforcement carbon
SiClx composite；Wherein, chemical vapor infiltration depositing silicon silicon concrete technology step is as follows：
A, multi-component multi-dimension graphene-Carbon fibe precast body is placed in gaseous phase deposition stove, and will be evacuated in stove
2kPa, inertia Ar is then passed through as 800mL/min using flow and is used as protective gas；
B, furnace temperature is risen to 1100 DEG C with 5 DEG C/min programming rate, is then passed through H by 200mL/min of flow2, with
Flow is that 10g/h is passed through methyl trichlorosilane gas (by controlling the gasification rate of methyl trichlorosilane liquid to realize control first
The ventilation flow rate of base trichlorosilane gas), while furnace pressure is adjusted as 6kPa progress deposition reactions, after deposition reaction 20h, stop
Reacting gas is only passed through into stove, in-furnace temperature is down to room temperature naturally, that is, it is silicon carbide fiber reinforced that graphene Modified Activated Carbon is made
Composite (is modified 2D Carbon fibes precast body enhancing carborundum (SiC) composite microscopic appearance) see Fig. 4 graphenes.
In the present embodiment, described graphene oxide, ascorbic acid, ethanol and methyl trichlorosilane are the pure (matter of analysis
Measure percentage composition >=99.8%), described Ar, H2It is more than 99.999% high-purity gas for purity.
It is raw materials used to be obtained by buying in the present embodiment.
Embodiment two
The preparation method for the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon that the present embodiment provides, including following step
Suddenly：
(1) preparation of dipping solution：The 20mg added into the graphene oxide water solution that 10ml concentration is 2mg/mL resists
Bad hematic acid, dipping solution is uniformly mixed so as to obtain, it is standby；
(2) preparation of surface functionalization Carbon fibe precast body：The overall Carbon fibe precast body ultrasound cleaned up is washed
After net (being at least cleaned by ultrasonic 10min), it is placed in the nitric acid that concentration is 68%, 2h is handled at 90 DEG C, concentration is put into after taking-up
For dialysis treatment 24h in 20% ethanol water, then the Carbon fibe after dialysis treatment is taken out and dried in 65 DEG C of baking ovens, i.e.,
Obtain surface functionalization Carbon fibe precast body；
(3) preparation of multi-component multi-dimension graphene-Carbon fibe precast body：By obtained surface functionalization in step (2)
Carbon fibe precast body is placed in step (1) vacuum impregnation in obtained dipping solution and handled, wherein, vacuum impregnation is handled specific
Method is as follows：Surface functionalization Carbon fibe precast body is put in vacuum impregnation room, vacuumizes 20min, then will be impregnated molten
Liquid is added in funnel, and control funnel liquid feed valve enters in impregnation chamber by solution, and 1h is impregnated after vacuumizing, and takes out the Carbon fiber after dipping
Dimension, is put into 95 DEG C of baking ovens, is taken out after hydrothermal chemistry reduction reaction 4h, produce multi-component multi-dimension graphene-Carbon fibe precast body
(see Fig. 3 graphenes-overall Carbon fibe precast body microscopic appearance)；
(4) preparation of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon：By obtained polynary more chis in step (3)
Spend graphene-Carbon fibe precast body and SiC matrix is deposited by chemical vapor infiltration, produce graphene Modified Activated Carbon fiber reinforcement carbon
SiClx composite；Wherein, chemical vapor infiltration depositing silicon silicon concrete technology step is as follows：
A, multi-component multi-dimension graphene-Carbon fibe precast body is placed in gaseous phase deposition stove, and will be evacuated in stove
3kPa, inertia Ar is then passed through as 200mL/min using flow and is used as protective gas；
B, furnace temperature is risen to 1000 DEG C with 6 DEG C/min programming rate, is then passed through H by 200mL/min of flow2, with
Flow is that 10g/h is passed through methyl trichlorosilane gas (by controlling the gasification rate of methyl trichlorosilane liquid to realize control first
The ventilation flow rate of base trichlorosilane gas), while furnace pressure is adjusted as 8kPa progress deposition reactions, after deposition reaction 20h, stop
Reacting gas is only passed through into stove, in-furnace temperature is down to room temperature naturally, that is, it is silicon carbide fiber reinforced that graphene Modified Activated Carbon is made
Composite (is modified overall Carbon fibe precast body enhancing carborundum (SiC) composite microscopic appearance) see Fig. 5 graphenes.
In the present embodiment, described graphene oxide, ascorbic acid, ethanol and methyl trichlorosilane are the pure (matter of analysis
Measure percentage composition >=99.8%), described Ar, H2It is more than 99.999% high-purity gas for purity.
It is raw materials used to be obtained by buying in the present embodiment.
Embodiment three
The preparation method for the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon that the present embodiment provides, including following step
Suddenly：
(1) preparation of dipping solution：The 1mg added into the graphene oxide water solution that 10ml concentration is 1mg/mL is anti-bad
Hematic acid, dipping solution is uniformly mixed so as to obtain, it is standby；
(2) preparation of surface functionalization Carbon fibe precast body：The overall Carbon fibe precast body ultrasound cleaned up is washed
After net (being at least cleaned by ultrasonic 10min), concentration is placed in 68% nitric acid, 1h to be handled at 95 DEG C, being put into concentration after taking-up is
Dialysis treatment 24h in 40% ethanol water, then the Carbon fibe after dialysis treatment is taken out and dried in 40 DEG C of baking ovens, produce
Surface functionalization Carbon fibe precast body；
(3) preparation of multi-component multi-dimension graphene-Carbon fibe precast body：By obtained surface functionalization in step (2)
Carbon fibe precast body is placed in step (1) vacuum impregnation in obtained dipping solution and handled, wherein, vacuum impregnation is handled specific
Method is as follows：Surface functionalization Carbon fibe precast body is put in vacuum impregnation room, vacuumizes 20min, then will be impregnated molten
Liquid is added in funnel, and control funnel liquid feed valve enters in impregnation chamber by solution, and 2h is impregnated after vacuumizing, and takes out the Carbon fiber after dipping
Dimension, is put into 80 DEG C of baking ovens, is taken out after hydrothermal chemistry reduction reaction 5h, produce multi-component multi-dimension graphene-Carbon fibe precast body.
(4) preparation of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon：By obtained polynary more chis in step (3)
Spend graphene-Carbon fibe precast body and SiC matrix is deposited by chemical vapor infiltration, produce graphene Modified Activated Carbon fiber reinforcement carbon
SiClx composite；Wherein, chemical vapor infiltration depositing silicon silicon concrete technology step is as follows：
A, multi-component multi-dimension graphene-Carbon fibe precast body is placed in gaseous phase deposition stove, and will be evacuated in stove
2kPa, inertia Ar is then passed through as 400mL/min using flow and is used as protective gas；
B, furnace temperature is risen to 1300 DEG C with 10 DEG C/min programming rate, is then passed through H by 100mL/min of flow2, with
Flow is that 4g/h is passed through methyl trichlorosilane gas (by controlling the gasification rate of methyl trichlorosilane liquid to realize control methyl
The ventilation flow rate of trichlorosilane gas), while furnace pressure is adjusted as 2kPa progress deposition reactions, after deposition reaction 40h, stop
Reacting gas is passed through into stove, in-furnace temperature is down to room temperature naturally, that is, it is silicon carbide fiber reinforced multiple that graphene Modified Activated Carbon is made
Condensation material.
In the present embodiment, described graphene oxide, ascorbic acid, ethanol and methyl trichlorosilane are the pure (matter of analysis
Measure percentage composition >=99.8%), described Ar, H2It is more than 99.999% high-purity gas for purity.
It is raw materials used to be obtained by buying in the present embodiment.
Example IV
The preparation method for the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon that the present embodiment provides, including following step
Suddenly：
(1) preparation of dipping solution：The 20mg added into the graphene oxide ethanol solution that 10ml concentration is 6mg/mL
Ascorbic acid, dipping solution is uniformly mixed so as to obtain, it is standby；
(2) preparation of surface functionalization Carbon fibe precast body：The 2D Carbon fibes precast body cleaned up ultrasound is cleaned
(at least it is cleaned by ultrasonic 10min) afterwards, is placed in the nitric acid that concentration is 68%, 4h is handled at 85 DEG C, being put into concentration after taking-up is
Dialysis treatment 36h in 15% ethanol water, then the Carbon fibe after dialysis treatment is taken out and dried in 65 DEG C of baking ovens, produce
Surface functionalization Carbon fibe precast body；
(3) preparation of multi-component multi-dimension graphene-Carbon fibe precast body：By obtained surface functionalization in step (2)
Carbon fibe precast body is placed in step (1) vacuum impregnation in obtained dipping solution and handled, wherein, vacuum impregnation is handled specific
Method is as follows：Surface functionalization Carbon fibe precast body is put in vacuum impregnation room, vacuumizes 20min, then will be impregnated molten
Liquid is added in funnel, and control funnel liquid feed valve enters in impregnation chamber by solution, and 1.5h is impregnated after vacuumizing, and takes out the charcoal after dipping
Fiber, it is put into 70 DEG C of baking ovens, is taken out after hydrothermal chemistry reduction reaction 6h, it is prefabricated produces multi-component multi-dimension graphene-Carbon fibe
Body.
(4) preparation of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon：By obtained polynary more chis in step (3)
Spend graphene-Carbon fibe precast body and SiC matrix is deposited by chemical vapor infiltration, produce graphene Modified Activated Carbon fiber reinforcement carbon
SiClx composite；Wherein, chemical vapor infiltration depositing silicon silicon concrete technology step is as follows：
A, multi-component multi-dimension graphene-Carbon fibe precast body is placed in gaseous phase deposition stove, and will be evacuated in stove
3kPa, inertia Ar is then passed through as 500mL/min using flow and is used as protective gas；
B, furnace temperature is risen to 1200 DEG C with 8 DEG C/min programming rate, is then passed through H by 300mL/min of flow2, with
Flow is that 12g/h is passed through methyl trichlorosilane gas (by controlling the gasification rate of methyl trichlorosilane liquid to realize control first
The ventilation flow rate of base trichlorosilane gas), while furnace pressure is adjusted as 4kPa progress deposition reactions, after deposition reaction 120h,
Stop being passed through reacting gas into stove, in-furnace temperature is down to room temperature naturally, that is, graphene Modified Activated Carbon fiber reinforcement carbonization is made
Silicon composite.
In the present embodiment, described graphene oxide, ascorbic acid, ethanol and methyl trichlorosilane are the pure (matter of analysis
Measure percentage composition >=99.8%), described Ar, H2It is more than 99.999% high-purity gas for purity.
It is raw materials used to be obtained by buying in the present embodiment.
Embodiment five
The preparation method for the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon that the present embodiment provides, including following step
Suddenly：
(1) preparation of dipping solution：The 50mg added into the graphene oxide ethanol solution that 10ml concentration is 10mg/mL
Ascorbic acid, dipping solution is uniformly mixed so as to obtain, it is standby；
(2) preparation of surface functionalization Carbon fibe precast body：The 2D Carbon fibes precast body cleaned up ultrasound is cleaned
(at least it is cleaned by ultrasonic 10min) afterwards, is placed in the nitric acid that concentration is 68%, 4h is handled at 85 DEG C, being put into concentration after taking-up is
Dialysis treatment 30h in 40% ethanol water, then the Carbon fibe after dialysis treatment is taken out and dried in 55 DEG C of baking ovens, produce
Surface functionalization Carbon fibe precast body；
(3) preparation of multi-component multi-dimension graphene-Carbon fibe precast body：By obtained surface functionalization in step (2)
Carbon fibe precast body is placed in step (1) vacuum impregnation in obtained dipping solution and handled, wherein, vacuum impregnation is handled specific
Method is as follows：Surface functionalization Carbon fibe precast body is put in vacuum impregnation room, vacuumizes 20min, then will be impregnated molten
Liquid is added in funnel, and control funnel liquid feed valve enters in impregnation chamber by solution, and 2h is impregnated after vacuumizing, and takes out the Carbon fiber after dipping
Dimension, is put into 95 DEG C of baking ovens, is taken out after hydrothermal chemistry reduction reaction 4h, produce multi-component multi-dimension graphene-Carbon fibe precast body.
(4) preparation of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon：By obtained polynary more chis in step (3)
Spend graphene-Carbon fibe precast body and SiC matrix is deposited by chemical vapor infiltration, produce graphene Modified Activated Carbon fiber reinforcement carbon
SiClx composite；Wherein, chemical vapor infiltration depositing silicon silicon concrete technology step is as follows：
A, multi-component multi-dimension graphene-Carbon fibe precast body is placed in gaseous phase deposition stove, and will be evacuated in stove
3kPa, inertia Ar is then passed through as 600mL/min using flow and is used as protective gas；
B, furnace temperature is risen to 1150 DEG C with 7 DEG C/min programming rate, is then passed through H by 200mL/min of flow2, with
Flow is that 20g/h is passed through methyl trichlorosilane gas (by controlling the gasification rate of methyl trichlorosilane liquid to realize control first
The ventilation flow rate of base trichlorosilane gas), while furnace pressure is adjusted as 5kPa progress deposition reactions, after deposition reaction 80h, stop
Reacting gas is only passed through into stove, in-furnace temperature is down to room temperature naturally, that is, it is compound that graphene Modified Activated Carbon fiber reinforcement SiC is made
Material.
In the present embodiment, described graphene oxide, ascorbic acid, ethanol and methyl trichlorosilane are the pure (matter of analysis
Measure percentage composition >=99.8%), described Ar, H2It is more than 99.999% high-purity gas for purity.
It is raw materials used to be obtained by buying in the present embodiment.
Embodiment six
The preparation method for the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon that the present embodiment provides, including following step
Suddenly：
(1) preparation of dipping solution：The 10mg added into the graphene oxide water solution that 10ml concentration is 8mg/mL resists
Bad hematic acid, dipping solution is uniformly mixed so as to obtain, it is standby；
(2) preparation of surface functionalization Carbon fibe precast body：The 2D Carbon fibes precast body cleaned up ultrasound is cleaned
(at least it is cleaned by ultrasonic 10min) afterwards, is placed in the nitric acid that concentration is 68%, 3h is handled at 90 DEG C, being put into concentration after taking-up is
Dialysis treatment 24h in 25% ethanol water, then the Carbon fibe after dialysis treatment is taken out and dried in 65 DEG C of baking ovens, produce
Surface functionalization Carbon fibe precast body；
(3) preparation of multi-component multi-dimension graphene-Carbon fibe precast body：By obtained surface functionalization in step (2)
Carbon fibe precast body is placed in step (1) vacuum impregnation in obtained dipping solution and handled, wherein, vacuum impregnation is handled specific
Method is as follows：Surface functionalization Carbon fibe precast body is put in vacuum impregnation room, vacuumizes 20min, then will be impregnated molten
Liquid is added in funnel, and control funnel liquid feed valve enters in impregnation chamber by solution, and 2h is impregnated after vacuumizing, and takes out the Carbon fiber after dipping
Dimension, is put into 85 DEG C of baking ovens, is taken out after hydrothermal chemistry reduction reaction 4h, produce multi-component multi-dimension graphene-Carbon fibe precast body.
(4) preparation of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon：By obtained polynary more chis in step (3)
Spend graphene-Carbon fibe precast body and SiC matrix is deposited by chemical vapor infiltration, produce graphene Modified Activated Carbon fiber reinforcement carbon
SiClx composite；Wherein, chemical vapor infiltration depositing silicon silicon concrete technology step is as follows：
A, multi-component multi-dimension graphene-Carbon fibe precast body is placed in gaseous phase deposition stove, and will be evacuated in stove
3kPa, inertia Ar is then passed through as 800mL/min using flow and is used as protective gas；
B, furnace temperature is risen to 1100 DEG C with 6 DEG C/min programming rate, is then passed through H by 300mL/min of flow2, with
Flow is that 15g/h is passed through methyl trichlorosilane gas (by controlling the gasification rate of methyl trichlorosilane liquid to realize control first
The ventilation flow rate of base trichlorosilane gas), while furnace pressure is adjusted as 6kPa progress deposition reactions, after deposition reaction 100h,
Stop being passed through reacting gas into stove, in-furnace temperature is down to room temperature naturally, that is, graphene Modified Activated Carbon fiber reinforcement carbonization is made
Silicon composite.
In the present embodiment, described graphene oxide, ascorbic acid, ethanol and methyl trichlorosilane are the pure (matter of analysis
Measure percentage composition >=99.8%), described Ar, H2It is more than 99.999% high-purity gas for purity.
It is raw materials used to be obtained by buying in the present embodiment.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
The present invention is described in detail good embodiment, it will be understood by those within the art that, can be to the skill of the present invention
Art scheme is modified or equivalent substitution, and without departing from the objective and scope of technical solution of the present invention, it all should cover at this
Among the right of invention.
Claims (3)
- A kind of 1. preparation method of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon, it is characterised in that：Comprise the following steps：(1) preparation of dipping solution：Reducing agent is added into the graphene oxide solution that concentration is 1mg/mL~10mg/mL, is mixed Even to obtain dipping solution, standby, the mass ratio of the reducing agent and graphene oxide is 1:1~1:10；(2) preparation of surface functionalization Carbon fibe precast body：After Carbon fibe precast body is cleaned with acetone ultrasound, it is placed in highly concentrated Spend and handle 1h~4h in nitric acid at 85 DEG C~95 DEG C, be put into the ethanol water that concentration is 5%~40% and dialyse after taking-up At least 24h is handled, then the Carbon fibe after dialysis treatment is taken out and dried at 40 DEG C~65 DEG C, produces surface functionalization Carbon fiber Tie up precast body；(3) preparation of multi-component multi-dimension graphene-Carbon fibe precast body：By obtained surface functionalization Carbon fiber in step (2) Dimension precast body is placed in step (1) vacuum impregnation 0.5h~2h in obtained dipping solution, then takes the Carbon fibe after dipping Go out hydrothermal chemistry reduction reaction 4h~6h at 70 DEG C~95 DEG C, produce multi-component multi-dimension graphene-Carbon fibe precast body；(4) preparation of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon：By obtained multi-component multi-dimension stone in step (3) Black alkene-Carbon fibe precast body deposits SiC matrix by chemical vapor infiltration, and it is silicon carbide fiber reinforced to produce graphene Modified Activated Carbon Composite；Wherein, chemical vapor infiltration depositing silicon silicon concrete technology step is as follows：A, multi-component multi-dimension graphene-Carbon fibe precast body is placed in gaseous phase deposition stove, and will be evacuated in stove 2kPa~ 3kPa, inertia Ar is then passed through as 200mL/min~800mL/min using flow and is used as protective gas；B, furnace temperature is risen to 1000 DEG C~1300 DEG C with 5 DEG C/min~10 DEG C/min programming rate, then using flow as 100mL/min~300mL/min is passed through H2, methyl trichlorosilane gas is passed through by 4g/h~20g/h of flow, while adjust stove Interior pressure is that 2kPa~8kPa carries out deposition reaction, after deposition reaction 20h~120h, stops being passed through reacting gas into stove, makes In-furnace temperature is down to room temperature naturally, that is, the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon is made.
- 2. the preparation method of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon according to claim 1, its feature It is：In the step (1), the graphene oxide solution is graphene oxide ethanol solution or graphene oxide water solution； The reducing agent is ascorbic acid.
- 3. the preparation method of the silicon carbide fiber reinforced composite of graphene Modified Activated Carbon according to claim 2, its feature It is：Described graphene oxide, ascorbic acid, ethanol and methyl trichlorosilane is that analysis is pure；Described Ar, H2It is big for purity In 99.999% high-purity gas.
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