CN104591798A - Preparation method of electrophoretic deposition nano-wire strengthened and toughened SiC anti-oxidation coating - Google Patents
Preparation method of electrophoretic deposition nano-wire strengthened and toughened SiC anti-oxidation coating Download PDFInfo
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Abstract
The invention discloses a preparation method of an electrophoretic deposition nano-wire strengthened and toughened SiC anti-oxidation coating. By adopting the preparation method, the technical problem that an existing preparation method is poor in controllability can be solved. A technical scheme of the preparation method comprises the following steps: depositing nano-wires on the surface of a C/C composite material by using an electrophoretic process, also performing micro-oxidation treatment on the C/C composite material in advance to improve the surface structure so as to facilitate nano-wire deposition, and implementing precise control of the content and thicknesses of the nano-wires by virtue of the change of electrophoresis parameters; and preparing an SiC coating by virtue of chemical vapor deposition. SiC nano-wires subjected to electrophoretic deposition are uniform in distribution and controllable in thickness; the nano-wires are deposited in channels and pores which are formed in a micro-oxidation process to ensure that the coating can be well combined with a substrate, and thus the possibility of coating peeling failure can be reduced; the SiC nano-wires can be used for strengthening and toughening the coating, and thus the performance of the coating can be improved; and meanwhile, because the sizes and numbers of cracks in the coating can be reduced by the SiC nano-wires, a channel for diffusing oxygen to enter the substrate can be blocked, so that the coating prepared by using the method disclosed by the invention is excellent in anti-oxidation performance.
Description
Technical field
The present invention relates to a kind of preparation method of oxidation resistant coating, particularly relate to a kind of preparation method of electrophoretic deposition nano wire highly malleablized SiC oxidation resistant coating.
Background technology
Charcoal/charcoal (C/C) matrix material has the mechanical property of carbon fibre reinforced composite excellence and the intrinsic resistance to elevated temperatures of carbon materials concurrently, thus as topmost high-temperature hot structured material, the every field such as space flight and aviation, national defense industry, biomedicine are widely used in.But C/C matrix material is very easily oxidized when high-temperature oxidation environment is on active service, seriously restricts it and further develop and good application.Because SiC coating can play effective protective effect to the C/C matrix material that aerobic environment is on active service, to ensure the performance of C/C matrix material, so be with a wide range of applications with the C/C matrix material of SiC coating.Because coating ruptures with substrate in conjunction with bad and coating fragility and causes the phenomenon of disbonding and material failure often to have generation.Correlative study is reported in be prepared coating procedure and introduces nano wire, effectively can improve substrate and coating adhesion and highly malleablized coating, and then raising coating protection performance.
Document 1 " Yanhui Chu; Hejun Li; Lu Li; et al.Oxidation protection of C/C composites byultra long SiC nanowire-reinforced SiC – Si coating.Corrosion Science; 2014; 84:204 ~ 208. " reports and prepares at C/C composite material surface the SiC-Si coating utilizing growth in situ ultralong SiC nanowires to strengthen, and significantly can improve the antioxidant property of material, is oxidized 160 hours only weightless 0.44% at 1500 DEG C.
Patent 1 " Li Hejun; Chen Zishan; Fu Qiangang, Chu Yanhui. a kind of nano wire strengthens the preparation method of SiC wear-resistant coating. application number 201310105833.X. China. " SiC coating that SiC nanowire strengthens makes the wear rate of material at 800 DEG C from 1.51 × 10 to utilize in situ synthesis to prepare
-3mm
3n
-1m
-1be reduced to 1.83 × 10
-4mm
3n
-1m
-1, reduce an order of magnitude.
Document 2 " Hejun Li; Yongjie Wang; Qiangang Fu; et al.SiC Nanowires Toughed HfCAblative Coating for C/C Composites.Journal of Materials Science and Technology; 2014; 4:1 ~ 7. " is after C/C composite material surface growth SiC nanowire, chemical vapour deposition (CVD) is used to prepare HfC coating, find that SiC nanowire can toughness reinforcing HfC coating, reduce linear ablative rate and the mass ablative rate of material, improve the ablation property of material.
The method introducing SiC nanowire in the preparation of C/C composite coating is mainly in situ synthesis, but these class methods have some limitations in coating preparation.Growth in situ nano wire generally needs sample to be imbedded powder or be placed in stove to pass into presoma, all at high temperature grows, and the power consumption of this growth technique is large, pollution is large, the cycle is long; Process of growth is harsh, too high to equipment requirements, extremely strong to process dependency to environmental requirement; And precisely cannot control the length, diameter, pattern etc. of single nano-wire, also well cannot control the distribution of nanowire growth, content and thickness.The poor controllability of growth in situ nano wire directly affects the barrier propterty of coated material, and its with high costs and unreliability that is technique determines that the method is difficult to be applicable to low cost preparation that is large-scale, shaped piece coating.
Summary of the invention
In order to overcome the deficiency of existing preparation method's poor controllability, the invention provides a kind of preparation method of electrophoretic deposition nano wire highly malleablized SiC oxidation resistant coating.The method utilizes electrophoresis process at C/C composite material surface fast and low-cost depositing nano line, and the low-level oxidation process in advance of C/C matrix material is improved surface tissue be beneficial to nanowire deposition, change by electrophoretic parameters realizes the accurate control to nano wire content and thickness, then prepares SiC coating by chemical vapour deposition.The SiC nanowire of electrophoretic deposition is evenly distributed and thickness is controlled; Coating can be combined well with substrate by the gully that nanowire deposition is formed in low-level oxidation process in hole, thus reduces possibility disbonding occurring and lost efficacy; SiC nanowire can highly malleablized coating, thus improves coating performance; Simultaneously because SiC nanowire can reduce yardstick and the quantity of crackle in coating, block the passage that oxygen diffusion enters substrate, coating prepared by the method has excellent antioxidant property.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of electrophoretic deposition nano wire highly malleablized SiC oxidation resistant coating, is characterized in adopting following steps:
Step one, C/C matrix material is used water and dehydrated alcohol ultrasonic cleaning 5-10min respectively, be placed in air and dry or oven for drying;
Step 2, under atmospheric pressure environment, with 5-7 DEG C/min heat-up rate, resistance furnace temperature is risen to 500-550 DEG C from room temperature, the C/C matrix material processed through step one is placed in resistance furnace flat-temperature zone, insulation 100-300min, powered-down subsequently, naturally cool to room temperature, obtain the porous C/C composite of surface modification;
Step 3, be the technical grade SiC nanowire of 0.025-0.127% by mass percent, the resol of mass percent to be the analytical pure aluminum nitrate of 0.01-0.013% and mass percent be 0.127-0.254% joins ultrasonic stirring 2-5h in the Virahol of surplus, obtained homodisperse electrophoresis liquid;
Step 4, the C/C matrix material of porous surface step 2 prepared are placed in the electrophoresis chamber be connected with electrophoresis apparatus negative electrode and fix, the electrophoresis liquid that in electrophoresis chamber prepared by implantation step three, control operating voltage 10-70V, depositing time 30-180s, deposit rear taking-up, dry under 30-80 DEG C of condition, obtain the C/C matrix material that surface deposition has SiC nanowire;
Chemical vapor deposition stove put into by step 5, the C/C matrix material containing SiC nanowire step 4 prepared, and take trichloromethyl silane as presoma, adopts MTS-H
2-Ar sedimentary system prepares SiC coating, and wherein Ar gas is as diluent gas, H
2as reactant gases, MTS is placed in constant temperature waters by bubbling H
2bring in mixed gas tank and Ar and H
2enter together after mixing in Reaktionsofen and participate in reaction.Depositing operation is as follows: depositing temperature is 1100-1300 DEG C, and deposition pressure is 2000-4000Pa, and depositing time is 6-8h.Take out after cooling, obtain the C/C matrix material that surface preparation has the SiC coating of SiC nanowire.
The invention has the beneficial effects as follows: the present invention utilizes electrophoresis process at C/C composite material surface fast and low-cost depositing nano line, and the low-level oxidation process in advance of C/C matrix material is improved surface tissue be beneficial to nanowire deposition, change by electrophoretic parameters realizes the accurate control to nano wire content and thickness, then prepares SiC coating by chemical vapour deposition.The SiC nanowire of electrophoretic deposition is evenly distributed and thickness is controlled; Coating can be combined well with substrate by the gully that nanowire deposition is formed in low-level oxidation process in hole, thus reduces possibility disbonding occurring and lost efficacy; SiC nanowire can highly malleablized coating, thus improves coating performance; Simultaneously because SiC nanowire can reduce yardstick and the quantity of crackle in coating, block the passage that oxygen diffusion enters substrate, coating prepared by the method has excellent antioxidant property.The coating sample of preparation is all less than not containing the coating sample of SiC nanowire at 1200 DEG C and the oxidation weight loss at 1500 DEG C, and after 35 hours oxidation experiments, oxidative mass loss maximum is only 54% of the latter's rate of weight loss, and antioxidant property is remarkable.
Below in conjunction with the drawings and specific embodiments, the present invention is elaborated.
Accompanying drawing explanation
Fig. 1 is the C/C matrix material low-level oxidation body structure surface SEM photo prepared by embodiment 3;
Fig. 2 is the C/C composite material surface SEM photo of the electrophoretic deposition SiC nanowire prepared by embodiment 3;
Fig. 3 is the surperficial SEM photo of the SiC nanowire highly malleablized SiC coating prepared by embodiment 3;
Fig. 4 is the section SEM photo of the SiC nanowire highly malleablized SiC coating prepared by embodiment 3;
Fig. 5 is the SiC nanowire highly malleablized SiC coating prepared by embodiment 3, and not containing the oxidation weight loss correlation curve of SiC nanowire highly malleablized SiC coating at 1500 DEG C.
Embodiment
Following examples are with reference to Fig. 1-5.
Embodiment 1:
Density is ρ=1.75g/cm by step 1
3the composite processing of C/C become 60 × 45 × 10mm
3sample, C/C matrix material is used respectively water and dehydrated alcohol ultrasonic cleaning 5min, is placed in air and dries or oven for drying;
Step 2, rises to 500 DEG C by resistance furnace temperature from room temperature with 5 DEG C/min heat-up rate under atmospheric pressure environment, and the C/C matrix material processed through step one is placed in resistance furnace flat-temperature zone, insulation 300min, powered-down subsequently, naturally cools to room temperature, obtains the porous C/C composite of surface modification;
Step 3, get 0.2g technical grade SiC nanowire (its mean diameter is 80-120nm), the analytical pure aluminum nitrate of 0.075g and 1g phenolic resin dispersion in the analytical pure Virahol of 1000ml (quality is 784g), ultrasonic disperse 2h, obtains electrophoresis liquid;
Step 4, the C/C matrix material of porous surface step 2 prepared is placed in the electrophoresis chamber be connected with electrophoresis apparatus negative electrode and fixes, the electrophoresis liquid that in electrophoresis chamber prepared by implantation step 3, control operating voltage 10V, depositing time 180s, deposit rear taking-up, dried under 30 DEG C of conditions, obtain the C/C matrix material that surface deposition has SiC nanowire;
Step 5, chemical vapor deposition stove put into by the C/C matrix material containing SiC nanowire step 4 prepared, and with trichloromethyl silane (MTS) for presoma, adopts MTS-H
2-Ar sedimentary system prepares SiC coating, and wherein Ar gas is as diluent gas, H
2as reactant gases, MTS is placed in constant temperature waters by bubbling H
2bring in mixed gas tank and Ar and H
2enter together after mixing in Reaktionsofen and participate in reaction.Depositing operation is as follows: depositing temperature is 1100 DEG C, and deposition pressure is 4000Pa, and depositing time is 8h.Take out after cooling, obtain the C/C matrix material that surface preparation has the SiC coating of SiC nanowire.
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 weight loss is 7.4%, and the SiC coating compared not containing SiC nanowire is remarkable at oxidation weight loss 16% antioxidant effect of 1200 DEG C.
Embodiment 2:
Step 1, gets the composite sample that shape is irregular special-shaped C/C, C/C matrix material is used respectively 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 heat-up rate under atmospheric pressure environment, and the C/C matrix material processed through step one is placed in resistance furnace flat-temperature zone, insulation 200min, powered-down subsequently, naturally cools to room temperature, obtains the porous C/C composite of surface modification;
Step 3, get 0.6g technical grade SiC nanowire (its mean diameter is 80-120nm), the analytical pure aluminum nitrate of 0.15g and 1.5g phenolic resin dispersion in the analytical pure Virahol (quality is 1176g) of 1500ml, ultrasonic disperse 3h, obtains electrophoresis liquid;
Step 4, the C/C matrix material of porous surface step 2 prepared is placed in the electrophoresis chamber be connected with electrophoresis apparatus negative electrode and fixes, the electrophoresis liquid that in electrophoresis chamber prepared by implantation step 3, control operating voltage 40V, depositing time 100s, deposit rear taking-up, dried under 50 DEG C of conditions, obtain the C/C matrix material that surface deposition has SiC nanowire;
Step 5, chemical vapor deposition stove put into by the C/C matrix material containing SiC nanowire step 4 prepared, and with trichloromethyl silane (MTS) for presoma, adopts MTS-H
2-Ar sedimentary system prepares SiC coating, and wherein Ar gas is as diluent gas, H
2as reactant gases, MTS is placed in constant temperature waters by bubbling H
2bring in mixed gas tank and Ar and H
2enter together after mixing in Reaktionsofen and participate in reaction.Depositing operation is as follows: depositing temperature is 1200 DEG C, and deposition pressure is 3000Pa, and depositing time is 7h.Take out after cooling, obtain the C/C matrix material that surface preparation has the SiC coating of SiC nanowire.
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 weight loss is 8.6%, compare not containing the SiC coating of SiC nanowire at the oxidation weight loss 16% of 1200 DEG C, antioxidant effect is remarkable.
Embodiment 3:
Step 1, becomes 25 × 20 × 5mm by the composite processing of C/C
3sample, C/C matrix material is used respectively 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 heat-up rate under atmospheric pressure environment, and the C/C matrix material processed through step one is placed in resistance furnace flat-temperature zone, insulation 100min, powered-down subsequently, naturally cools to room temperature, obtains the porous C/C composite of surface modification;
Step 3, get 2g technical grade SiC nanowire (its mean diameter is 80-120nm), the analytical pure aluminum nitrate of 0.2g and 4g phenolic resin dispersion in the analytical pure Virahol (quality is 1568g) of 2000ml, ultrasonic disperse 5h, obtains electrophoresis liquid;
Step 4, the C/C matrix material of porous surface step 2 prepared is placed in the electrophoresis chamber be connected with electrophoresis apparatus negative electrode and fixes, the electrophoresis liquid that in electrophoresis chamber prepared by implantation step 3, control operating voltage 70V, depositing time 30s, deposit rear taking-up, dried under 80 DEG C of conditions, obtain the C/C matrix material that surface deposition has SiC nanowire;
Step 5, chemical vapor deposition stove put into by the C/C matrix material containing SiC nanowire step 4 prepared, and with trichloromethyl silane (MTS) for presoma, adopts MTS-H
2-Ar sedimentary system prepares SiC coating, and wherein Ar gas is as diluent gas, H
2as reactant gases, MTS is placed in constant temperature waters by bubbling H
2bring in mixed gas tank and Ar and H
2enter together after mixing in Reaktionsofen and participate in reaction.Depositing operation is as follows: depositing temperature is 1300 DEG C, and deposition pressure is 2000Pa, and depositing time is 6h.Take out after cooling, obtain the C/C matrix material that surface preparation has the SiC coating of SiC nanowire.
The SiC coating that electrophoresis SiC nanowire prepared by the present embodiment is tough is in atmosphere in 1500 DEG C of oxidation experiments, and oxidation weight loss is 5.7%, compare not containing the SiC coating of SiC nanowire at the oxidation weight loss 20% of 1500 DEG C, antioxidant effect is remarkable.
Fig. 1 is the stereoscan photograph of C/C matrix material after low-level oxidation treat surface prepared by embodiment 3, can find out, C/C surface becomes more coarse, there is a large amount of gullies and pore structure, and the formation of this structure will be conducive to SiC nanowire deposition in electrophoresis process.
Fig. 2 is the stereoscan photograph of C/C matrix material after electrophoretic deposition SiC nanowire prepared by embodiment 3, and observe and find, SiC nanowire is covered in C/C surface, in random disordered arrangements.
Fig. 3 is that the C/C surface prepared by embodiment 3 contains the surface scan electromicroscopic photograph that SiC nanowire deposits SiC coating sample again, and visible SiC nanowire by particulate state SiC coating bridges together, illustrates that it plays tough effect to coating.
Fig. 4 is the profile scanning electromicroscopic photograph of the SiC nanowire highly malleablized SiC coating prepared by embodiment 3, and visible SiC coating has infiltrated C/C surface with lower area, interface without de-being stained with, without hole, illustrate coating and matrix set good.
Fig. 5 be prepared by embodiment 3 containing with not containing SiC nanowire SiC coating 1500 DEG C at oxidation weight loss curve, the visible coating rate of weight loss containing SiC nanowire is starkly lower than not containing the coating of SiC nanowire, illustrates that the coating antioxidant effect containing SiC nanowire is better; After 30 hours oxidation experiments, weightless less than 5%, confirm that antioxidant effect is remarkable.
Claims (1)
1. a preparation method for electrophoretic deposition nano wire highly malleablized SiC oxidation resistant coating, is characterized in that comprising the following steps:
Step one, C/C matrix material is used water and dehydrated alcohol ultrasonic cleaning 5-10min respectively, be placed in air and dry or oven for drying;
Step 2, under atmospheric pressure environment, with 5-7 DEG C/min heat-up rate, resistance furnace temperature is risen to 500-550 DEG C from room temperature, the C/C matrix material processed through step one is placed in resistance furnace flat-temperature zone, insulation 100-300min, powered-down subsequently, naturally cool to room temperature, obtain the porous C/C composite of surface modification;
Step 3, be the technical grade SiC nanowire of 0.025-0.127% by mass percent, the resol of mass percent to be the analytical pure aluminum nitrate of 0.01-0.013% and mass percent be 0.127-0.254% joins ultrasonic stirring 2-5h in the Virahol of surplus, obtained homodisperse electrophoresis liquid;
Step 4, the C/C matrix material of porous surface step 2 prepared are placed in the electrophoresis chamber be connected with electrophoresis apparatus negative electrode and fix, the electrophoresis liquid that in electrophoresis chamber prepared by implantation step three, control operating voltage 10-70V, depositing time 30-180s, deposit rear taking-up, dry under 30-80 DEG C of condition, obtain the C/C matrix material that surface deposition has SiC nanowire;
Chemical vapor deposition stove put into by step 5, the C/C matrix material containing SiC nanowire step 4 prepared, and take trichloromethyl silane as presoma, adopts MTS-H
2-Ar sedimentary system prepares SiC coating, and wherein Ar gas is as diluent gas, H
2as reactant gases, MTS is placed in constant temperature waters by bubbling H
2bring in mixed gas tank and Ar and H
2enter together after mixing in Reaktionsofen and participate in reaction.Depositing operation is as follows: depositing temperature is 1100-1300 DEG C, and deposition pressure is 2000-4000Pa, and depositing time is 6-8h.Take out after cooling, obtain the C/C matrix material that surface preparation has the SiC coating of SiC nanowire.
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CN111069726A (en) * | 2018-10-19 | 2020-04-28 | 天津大学 | Carbon-carbon composite material and metal brazing connection method based on electrophoretic deposition of SiC nanowires |
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CN111069726A (en) * | 2018-10-19 | 2020-04-28 | 天津大学 | Carbon-carbon composite material and metal brazing connection method based on electrophoretic deposition of SiC nanowires |
CN111069726B (en) * | 2018-10-19 | 2021-04-30 | 天津大学 | Carbon-carbon composite material and metal brazing connection method based on electrophoretic deposition of SiC nanowires |
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