CN104591798B - The preparation method of electrophoretic deposition nano wire Strengthening and Toughening SiC ORC - Google Patents

The preparation method of electrophoretic deposition nano wire Strengthening and Toughening SiC ORC Download PDF

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CN104591798B
CN104591798B CN201410841222.6A CN201410841222A CN104591798B CN 104591798 B CN104591798 B CN 104591798B CN 201410841222 A CN201410841222 A CN 201410841222A CN 104591798 B CN104591798 B CN 104591798B
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coating
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nanowire
deposition
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CN104591798A (en
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郭领军
黎云玉
刘宁坤
宋强
景伟
彭坚
李露
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Northwestern Polytechnical University
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Abstract

The invention discloses the preparation method of a kind of electrophoretic deposition nano wire Strengthening and Toughening SiC ORC, for solving the technical problem of existing preparation method poor controllability.Technical scheme is to utilize electrophoresis process to deposit nano wire at C/C composite material surface, and is processed by C/C composite low-level oxidation in advance and improve surface texture and be beneficial to nanowire deposition, changes, by electrophoretic parameters, the accurate control realized nano wire content with thickness.By chemical gaseous phase deposition preparation SiC coating.The SiC nanowire of electrophoretic deposition is evenly distributed and thickness is controlled;Coating can be combined well in hole by the gully that nanowire deposition is formed in low-level oxidation process with substrate, thus reduces the possibility occurring disbonding to lose efficacy;SiC nanowire can Strengthening and Toughening coating, thus improve coating performance;Simultaneously because SiC nanowire can reduce yardstick and the quantity of crackle in coating, blocking oxygen and diffuse into the passage of substrate, coating antioxygenic property prepared by the method is excellent.

Description

The preparation method of electrophoretic deposition nano wire Strengthening and Toughening SiC ORC
Technical field
The present invention relates to the preparation method of a kind of ORC, particularly relate to a kind of electrophoretic deposition nano wire Strengthening and Toughening The preparation method of SiC ORC.
Background technology
Charcoal/charcoal (C/C) composite has the excellent mechanical property of carbon fibre reinforced composite concurrently and carbon materials is intrinsic Resistance to elevated temperatures, thus as topmost high-temperature hot structural material, be widely used in space flight and aviation, national defense industry, The every field such as biomedicine.But, C/C composite is the most oxidized when high-temperature oxidation environment is on active service, seriously Restrict its development and good application further.The C/C composite being on active service aerobic environment because of SiC coating can play Effective protective action, to ensure the performance of C/C composite, so with the C/C composite wood of SiC coating Material is with a wide range of applications.Cause coating owing to coating is combined bad and coating fragility fracture with substrate Peel off and the phenomenon of material failure often has generation.Correlational study is reported in prepares coating procedure introducing nano wire, can be effective Improve substrate and coating adhesion Strengthening and Toughening coating, and then improve coating protection performance.
Document 1 " Yanhui Chu, Hejun Li, Lu Li, et al.Oxidation protection of C/C composites by Ultra long SiC nanowire-reinforced SiC Si coating.Corrosion Science, 2014,84:204~208. " Report and be prepared by, at C/C composite material surface, the SiC-Si coating that growth in situ ultralong SiC nanowires strengthens, can Significantly improve the antioxygenic property of material, at 1500 DEG C, aoxidize 160 hours only weightless 0.44%.
Patent 1 " Li Hejun, Chen Zishan, Fu Qiangang, Chu Yanhui. a kind of nano wire strengthens the preparation side of SiC wear-resistant coating Method. application number 201310105833.X. China. " utilize in situ synthesis prepare SiC nanowire strengthen SiC coating make Material wear rate at 800 DEG C is from 1.51 × 10-3mm3·N-1·m-1It is reduced to 1.83 × 10-4mm3·N-1·m-1, reduce An order of magnitude.
Document 2 " Hejun Li, Yongjie Wang, Qiangang Fu, et al.SiC Nanowires Toughed HfC Ablative Coating for C/C Composites.Journal of Materials Science and Technology,2014, 4:1~7. " after C/C composite material surface growth SiC nanowire, use chemical gaseous phase deposition (CVD) to prepare HfC Coating, find SiC nanowire can toughness reinforcing HfC coating, reduce the linear ablative rate of material and mass ablative rate, improve material The ablation property of material.
In prepared by C/C composite coating, introduce the method for SiC nanowire be mainly in situ synthesis, but this type of Method has some limitations in prepared by coating.Growth in situ nano wire it is generally required to imbed powder or put by sample Being passed through presoma in stove, the most at high temperature grow, the power consumption of this growth technique is big, it is big to pollute, the cycle is long;Grew Journey is harsh to environmental requirement, too high to equipment requirements, extremely strong to process dependency;And single nanometer cannot be precisely controlled The length of line, diameter, pattern etc., also cannot well control the distribution of nanowire growth, content and thickness.The most raw The poor controllability of long nano wire directly affects the barrier propterty of coating material, and its with high costs and technique is unreliable Property determines that the method is difficult to be applicable to low cost large-scale, shaped piece coating and prepares.
Summary of the invention
In order to overcome the deficiency of existing preparation method poor controllability, the present invention provides a kind of electrophoretic deposition nano wire tough Change the preparation method of SiC ORC.The method utilizes electrophoresis process at C/C composite material surface fast and low-cost Deposition nano wire, and C/C composite low-level oxidation in advance is processed improve surface texture and be beneficial to nanowire deposition, borrow That helps electrophoretic parameters changes the accurate control realized nano wire content with thickness, then passes through chemical gaseous phase deposition preparation SiC coating.The SiC nanowire of electrophoretic deposition is evenly distributed and thickness is controlled;Nanowire deposition is in low-level oxidation process shape Coating can be combined well in hole by the gully become with substrate, thus reduces the possibility occurring disbonding to lose efficacy; SiC nanowire can Strengthening and Toughening coating, thus improve coating performance;Split simultaneously because SiC nanowire can reduce in coating The yardstick of stricture of vagina and quantity, block oxygen and diffuse into the passage of substrate, and coating prepared by the method has the antioxygen of excellence Change performance.
The technical solution adopted for the present invention to solve the technical problems is: a kind of electrophoretic deposition nano wire Strengthening and Toughening SiC The preparation method of ORC, be characterized in use following steps:
Step one, by C/C composite respectively with water and dehydrated alcohol ultrasonic cleaning 5-10min, be placed in air and dry Or oven for drying;
Step 2, under atmospheric pressure environment, with 5-7 DEG C/min programming rate, resistance furnace temperature is risen to 500-550 DEG C from room temperature, will The C/C composite processed through step one is placed in resistance furnace flat-temperature zone, is incubated 100-300min, is then turned off power supply, Naturally cool to room temperature, obtain the porous C/C composite of surface modification;
Step 3, by technical grade SiC nanowire, mass percent that mass percent is 0.025-0.127% it is The analytical pure aluminum nitrate of 0.01-0.013% and the phenolic resin that mass percent is 0.127-0.254% join the different of surplus Ultrasonic stirring 2-5h in propanol, prepares homodisperse electrophoresis liquid;
Step 4, the C/C composite of porous surface step 2 prepared are placed in the electrophoresis being connected with electrophresis apparatus negative electrode Fixing in groove, in electrophoresis tank, the electrophoresis liquid of implantation step three preparation, controls running voltage 10-70V, sedimentation time 30-180s, takes out after having deposited, and dries under the conditions of 30-80 DEG C, and obtaining surface deposition has the C/C of SiC nanowire Composite;
Step 5, the C/C composite containing SiC nanowire step 4 prepared are put in chemical vapor deposition stove, With trichloromethyl silane as presoma, use MTS-H2-Ar sedimentary system prepares SiC coating, the wherein conduct of Ar gas Diluent gas, H2As reacting gas, MTS is placed in constant temperature waters by bubbling H2Bring in mixed gas tank and Ar And H2Reaction is participated in entering reacting furnace after mix homogeneously together.Depositing operation is as follows: depositing temperature is 1100-1300 DEG C, deposition pressure is 2000-4000Pa, and sedimentation time is 6-8h.Take out after cooling, obtain surface system Have the C/C composite of the SiC coating of SiC nanowire.
The invention has the beneficial effects as follows: the present invention utilizes electrophoresis process to deposit at C/C composite material surface fast and low-cost Nano wire, and C/C composite low-level oxidation in advance is processed improve surface texture and be beneficial to nanowire deposition, by electricity The change of swimming parameter realizes the accurate control to nano wire content with thickness, then passes through chemical gaseous phase and deposits preparation SiC Coating.The SiC nanowire of electrophoretic deposition is evenly distributed and thickness is controlled;Nanowire deposition is formed in low-level oxidation process Coating can be combined well in hole by gully with substrate, thus reduces the possibility occurring disbonding to lose efficacy;SiC Nano wire can Strengthening and Toughening coating, thus improve coating performance;Simultaneously because SiC nanowire can reduce crackle in coating Yardstick and quantity, block oxygen and diffuse into the passage of substrate, and coating prepared by the method has the non-oxidizability of excellence Energy.The coating sample of preparation does not contains the coating examination of SiC nanowire at 1200 DEG C with the oxidation weight loss at 1500 DEG C Sample, after 35 hours oxidation experiments, oxidative mass loss peak is only the 54% of the latter's weight-loss ratio, antioxygenic property Significantly.
With detailed description of the invention, the present invention is elaborated below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Fig. 1 is the C/C composite low-level oxidation body structure surface SEM photograph prepared by embodiment 3;
Fig. 2 is the C/C composite material surface SEM photograph of the electrophoretic deposition SiC nanowire prepared by embodiment 3;
Fig. 3 is the surface SEM photograph of the SiC nanowire Strengthening and Toughening SiC coating prepared by embodiment 3;
Fig. 4 is the section SEM photograph of the SiC nanowire Strengthening and Toughening SiC coating prepared by embodiment 3;
Fig. 5 is the SiC nanowire Strengthening and Toughening SiC coating prepared by embodiment 3, and without SiC nanowire Strengthening and Toughening SiC coating oxidation weight loss correlation curve at 1500 DEG C.
Detailed description of the invention
Following example are with reference to Fig. 1-5.
Embodiment 1:
Step 1, is ρ=1.75g/cm by density3The composite processing of C/C become 60 × 45 × 10mm3Sample, will C/C composite with water and dehydrated alcohol ultrasonic cleaning 5min, is placed in air and dries or oven for drying respectively;
Step 2, rises to 500 DEG C by resistance furnace temperature from room temperature with 5 DEG C/min programming rate under atmospheric pressure environment, will be through step The rapid one C/C composite processed is placed in resistance furnace flat-temperature zone, is incubated 300min, is then turned off power supply, natural cooling To room temperature, obtain the porous C/C composite of surface modification;
Step 3, takes 0.2g technical grade SiC nanowire (its average diameter is 80-120nm), the analytical pure nitric acid of 0.075g Aluminum and 1g phenolic resin dispersion in the analytical pure isopropanol of 1000ml (quality is 784g), ultrasonic disperse 2h, obtain Electrophoresis liquid;
Step 4, the C/C composite of porous surface step 2 prepared is placed in the electrophoresis tank being connected with electrophresis apparatus negative electrode In fixing, the electrophoresis liquid of implantation step 3 preparation in electrophoresis tank, control running voltage 10V, sedimentation time 180s, deposition Taking out after completing, dry under the conditions of 30 DEG C, obtaining surface deposition has the C/C composite of SiC nanowire;
Step 5, the C/C composite containing SiC nanowire step 4 prepared is put in chemical vapor deposition stove, with three Chloromethyl silane (MTS) is presoma, uses MTS-H2-Ar sedimentary system prepares SiC coating, the wherein conduct of Ar gas Diluent gas, H2As reacting gas, MTS is placed in constant temperature waters by bubbling H2Bring in mixed gas tank with Ar and H2 Reaction is participated in entering reacting furnace after mix homogeneously together.Depositing operation is as follows: depositing temperature is 1100 DEG C, deposition pressure Power is 4000Pa, and sedimentation time is 8h.Take out after cooling, obtain the C/C that surface preparation has the SiC coating of SiC nanowire Composite.
The SiC coating that electrophoresis SiC nanowire prepared by the present embodiment is tough is in the oxidation experiment of 1200 DEG C, and oxidation is lost It is heavily 7.4%, compares not notable at oxidation weight loss 16% antioxidant effect of 1200 DEG C containing the SiC coating of SiC nanowire.
Embodiment 2:
Step 1, takes the composite sample being shaped as irregular abnormity C/C, by C/C composite respectively with water and Dehydrated alcohol ultrasonic cleaning 8min, is placed in air and dries or oven for drying;
Step 2, rises to 525 DEG C by resistance furnace temperature from room temperature with 6 DEG C/min programming rate under atmospheric pressure environment, will be through step The rapid one C/C composite processed is placed in resistance furnace flat-temperature zone, is incubated 200min, is then turned off power supply, natural cooling To room temperature, obtain the porous C/C composite of surface modification;
Step 3, takes 0.6g technical grade SiC nanowire (its average diameter is 80-120nm), the analytical pure nitric acid of 0.15g Aluminum and 1.5g phenolic resin dispersion in the analytical pure isopropanol (quality is 1176g) of 1500ml, ultrasonic disperse 3h, To electrophoresis liquid;
Step 4, the C/C composite of porous surface step 2 prepared is placed in the electrophoresis tank being connected with electrophresis apparatus negative electrode In fixing, the electrophoresis liquid of implantation step 3 preparation in electrophoresis tank, control running voltage 40V, sedimentation time 100s, deposition Taking out after completing, dry under the conditions of 50 DEG C, obtaining surface deposition has the C/C composite of SiC nanowire;
Step 5, the C/C composite containing SiC nanowire step 4 prepared is put in chemical vapor deposition stove, with three Chloromethyl silane (MTS) is presoma, uses MTS-H2-Ar sedimentary system prepares SiC coating, the wherein conduct of Ar gas Diluent gas, H2As reacting gas, MTS is placed in constant temperature waters by bubbling H2Bring in mixed gas tank with Ar and H2 Reaction is participated in entering reacting furnace after mix homogeneously together.Depositing operation is as follows: depositing temperature is 1200 DEG C, deposition pressure Power is 3000Pa, and sedimentation time is 7h.Take out after cooling, obtain the C/C that surface preparation has the SiC coating of SiC nanowire Composite.
The SiC coating that electrophoresis SiC nanowire prepared by the present embodiment is tough is in the oxidation experiment of 1200 DEG C, and oxidation is lost Being heavily 8.6%, compare the oxidation weight loss 16% that the SiC coating not containing SiC nanowire is at 1200 DEG C, antioxidant effect is notable.
Embodiment 3:
Step 1, becomes 25 × 20 × 5mm by the composite processing of C/C3Sample, by C/C composite respectively with water and Dehydrated alcohol ultrasonic cleaning 10min, is placed in air and dries or oven for drying;
Step 2, rises to 550 DEG C by resistance furnace temperature from room temperature with 7 DEG C/min programming rate under atmospheric pressure environment, will be through step The rapid one C/C composite processed is placed in resistance furnace flat-temperature zone, is incubated 100min, is then turned off power supply, natural cooling To room temperature, obtain the porous C/C composite of surface modification;
Step 3, take 2g technical grade SiC nanowire (its average diameter is 80-120nm), the analytical pure aluminum nitrate of 0.2g and 4g phenolic resin dispersion in the analytical pure isopropanol (quality is 1568g) of 2000ml, ultrasonic disperse 5h, obtain electrophoresis Liquid;
Step 4, the C/C composite of porous surface step 2 prepared is placed in the electrophoresis tank being connected with electrophresis apparatus negative electrode In fixing, the electrophoresis liquid of implantation step 3 preparation in electrophoresis tank, control running voltage 70V, sedimentation time 30s, deposition Taking out after completing, dry under the conditions of 80 DEG C, obtaining surface deposition has the C/C composite of SiC nanowire;
Step 5, the C/C composite containing SiC nanowire step 4 prepared is put in chemical vapor deposition stove, with three Chloromethyl silane (MTS) is presoma, uses MTS-H2-Ar sedimentary system prepares SiC coating, the wherein conduct of Ar gas Diluent gas, H2As reacting gas, MTS is placed in constant temperature waters by bubbling H2Bring in mixed gas tank with Ar and H2 Reaction is participated in entering reacting furnace after mix homogeneously together.Depositing operation is as follows: depositing temperature is 1300 DEG C, deposition pressure Power is 2000Pa, and sedimentation time is 6h.Take out after cooling, obtain the C/C that surface preparation has the SiC coating of SiC nanowire Composite.
In SiC coating 1500 DEG C of oxidation experiments in atmosphere that electrophoresis SiC nanowire prepared by the present embodiment is tough, oxygen Changing weightlessness is 5.7%, compares the oxidation weight loss 20% that the SiC coating not containing SiC nanowire is at 1500 DEG C, antioxidant effect Significantly.
Fig. 1 is the stereoscan photograph after low-level oxidation processes surface of the C/C composite prepared by embodiment 3, permissible Finding out, C/C surface becomes relatively rough, there is substantial amounts of gully and pore structure, and the formation of this structure is beneficial to SiC nanowire deposition in electrophoresis process.
Fig. 2 is the stereoscan photograph after electrophoretic deposition SiC nanowire of the C/C composite prepared by embodiment 3, sees Examining discovery, SiC nanowire is covered in C/C surface, in random disordered arrangements.
Fig. 3 is the surface scan Electronic Speculum containing SiC nanowire redeposition SiC coating sample of the C/C surface prepared by embodiment 3 Photo, it is seen that SiC nanowire by graininess SiC coating bridges together, illustrates that coating is played tough effect by it.
Fig. 4 is the profile scanning electromicroscopic photograph of the SiC nanowire Strengthening and Toughening SiC coating prepared by embodiment 3, it is seen that SiC Coating has penetrated into C/C surface region below, and interface, without de-being stained with, without hole, illustrates that coating is good with matrix set.
Fig. 5 is containing and the oxidation weight loss song at the SiC coating 1500 DEG C without SiC nanowire prepared by embodiment 3 Line, it is seen that the coating weight-loss ratio containing SiC nanowire, significantly lower than the coating without SiC nanowire, illustrates to receive containing SiC The coating antioxidant effect of rice noodle is preferable;After 30 hours oxidation experiments, weightless less than 5%, it was demonstrated that antioxidant effect Significantly.

Claims (1)

1. the preparation method of an electrophoretic deposition nano wire Strengthening and Toughening SiC ORC, it is characterised in that comprise the following steps:
Step one, by C/C composite respectively with water and dehydrated alcohol ultrasonic cleaning 5-10min, be placed in air and dry or oven for drying;
Step 2, under atmospheric pressure environment, with 5-7 DEG C/min programming rate, resistance furnace temperature is risen to 500-550 DEG C from room temperature, the C/C composite processed through step one is placed in resistance furnace flat-temperature zone, insulation 100-300min, it is then turned off power supply, naturally cool to room temperature, obtain the porous C/C composite of surface modification;
Step 3, by technical grade SiC nanowire that mass percent is 0.025-0.127%, mass percent it is the analytical pure aluminum nitrate of 0.01-0.013% and phenolic resin that mass percent is 0.127-0.254% joins ultrasonic stirring 2-5h in the isopropanol of surplus, prepares homodisperse electrophoresis liquid;
Step 4, the C/C composite of porous surface step 2 prepared are placed in the electrophoresis tank being connected with electrophresis apparatus negative electrode fixing, the electrophoresis liquid of implantation step three preparation in electrophoresis tank, control running voltage 10-70V, sedimentation time 30-180s, take out after having deposited, drying under the conditions of 30-80 DEG C, obtaining surface deposition has the C/C composite of SiC nanowire;
Step 5, the C/C composite containing SiC nanowire step 4 prepared are put in chemical vapor deposition stove, with trichloromethyl silane as presoma, use MTS-H2-Ar sedimentary system prepares SiC coating, and wherein Ar gas is as diluent gas, H2As reacting gas, MTS is placed in constant temperature waters by bubbling H2Bring in mixed gas tank with Ar and H2Reaction is participated in entering reacting furnace after mix homogeneously together;Depositing operation is as follows: depositing temperature is 1100-1300 DEG C, and deposition pressure is 2000-4000Pa, and sedimentation time is 6-8h, takes out after cooling, obtains the C/C composite that surface preparation has the SiC coating of SiC nanowire.
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