CN102924108B - Method for preparing Y2Si2O7 whisker-toughened mullite composite coating - Google Patents

Method for preparing Y2Si2O7 whisker-toughened mullite composite coating Download PDF

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CN102924108B
CN102924108B CN201210458776.9A CN201210458776A CN102924108B CN 102924108 B CN102924108 B CN 102924108B CN 201210458776 A CN201210458776 A CN 201210458776A CN 102924108 B CN102924108 B CN 102924108B
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黄剑锋
杨柳青
曹丽云
王雅琴
费杰
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Yang Jieru
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a method for preparing a Y2Si2O7 whisker-toughened mullite composite coating. The method comprises the following steps: preparing a SiC porous internal coating on the matrix surface of a C/C composite material through an embedding method, preparing Y2Si2O7 whiskers, and then performing surface modification to the Y2Si2O7 whiskers with a composite surface active agent to obtain a mixed liquor; and performing ultrasonic electrophoretic selective assembly deposition to the C/C composite material prepared with the SiC porous internal coating and the mixed liquor to obtain a Y2Si2O7 whisker pinning layer, and finally preparing the Y2Si2O7 whisker-toughened mullite composite coating through a hydrothermal electrophoretic deposition method. Compared with other coatings, the prepared Y2Si2O7 whisker-toughened mullite composite coating can effectively increase the oxidation-resistance temperature, can realize the anti-oxidation protection of 400 hours for the C/C composite material under the condition of dynamic brush of high temperature (1700 DEG C) gas, and the oxidation loss rate is lower than 0.77 percent.

Description

A kind of Y 2si 2o 7the preparation method of crystal whisker toughened mullite compound coating
Technical field
The invention belongs to C/C technical field of composite materials, relate to a kind of preparation method of C/C matrix material high-temperature oxidation resistant coating, be specifically related to a kind of Y 2si 2o 7the preparation method of crystal whisker toughened mullite compound coating.
Background technology
Carbon/carbon (C/C) matrix material has the excellent properties such as thermal expansivity is low, density is low, high temperature resistant, resistance to ablation, high strength, high-modulus, particularly 2200 ℃ of inert atmosphere with interior condition under its strength and modulus excellent properties of raising and increase with temperature, it is had broad application prospects at aerospace field.Yet C/C matrix material will be oxidized at the aerobic environment that surpasses 450 ℃, oxidation quality loss causes its strength degradation, has limited its practical application.Therefore, solving C/C matrix material high-temp antioxidizing problem is the key that makes full use of its performance.
Improve C/C compound material antioxygenic property and mainly contain two kinds of approach: a kind of is matrix modification technology; A kind of is top coat technology.Research shows, matrix modification technology is only applicable to the oxidation protection of low-temperature zone to C/C material.Coating technology can solve the high temperature oxidation problem of C/C material.
The more C/C matrix material high-temperature oxidation resistant coating of research has SiC[Y.L.Zhang at present, H.J.Li, Q.G.Fu.A C/SiC gradient oxidation protective coating for carbon/carboncomposites.Surf.Coaf.Techol., 2006,201:3491-3495.], CrSi 2[Fu Qian-Gang, LiHe-Jun, Shi Xiao-Hong.A SiC whisker-toughened SiC-CrSi 2oxidation protectivecoating for carbon/carbon composites, April.Surf.Sci., 2007,253:3757-3760.], Si-Mo[Zhi-Qiao Yan, Xiang Xiong, Peng Xiao, Feng Chen, Hong-Bo Zhang, Bai-Yun Huang.A multilayer coating of dense SiC alternated with porous Si-Mofor the oxidation protection of carbon/carbon composites, Carbon, 2008,46 (1): 149-153.], Si-MoSi 2[Yu-Lei Zhang, He-Jun Li, Xi-Yuan Yao.Oxidation protectionof C/SiC coated carbon/carbon composites with Si-Mo coating at hightemperature, Corros.Sci., 2011,53:2075-2079.], Mo-Si-N[Z.H.Lai, J.C.Zhu, J.H.Jeon.Phase constitutions of Mo-Si-N anti-oxidation multi-layer coatings onC/C composites by fused slurry.Mater.Sci.Eng.A, 2009,499:267-270.] and Si-Mo-SiO 2[Z.Q.Yan, X.Xiong, P.Xiao, et al.Si-Mo-SiO 2oxidation protectivecoatings prepared by slurry painting for C/C-SiC composites.Surf.Coaf.Techol., 2008,202:4734-4740.] etc., Huang Jianfeng etc. have also studied take other compound coating that SiC is transition layer, as SiC-B 4c/SiC/SiO 2[Jun Li, Ruiying Luo, Chen Lin.Oxidation resistance of agradient self-healing coating for cabon/carbon composites, Carbon, 2007,45:2471-2478], SiC/Y 2siO 5[Argirusis Chr., Damjanovic T., Borchardt G..Yttriumsilicate coating system for oxidation protection of C/C-Si-SiC composites:Electrophoretic deposition and oxygen self-diffusion measurements, Journal of theEuropean Ceramic Society, 2007,27 (2-3): 1303-1306.] and SiC/MoSi 2-CrSi 2-Si[Li-He-Jun, Feng Tao, Fu Qian-Gang.Oxidation and erosionresistance of MoSi 2-CrSi 2-Si/SiC coated C/C composites in static and aerodynamicoxidation environment, Carbon, 2012,48:1636-1642.] etc.Yet above-mentioned coating does not also reach the 1600-2500 ℃ of application request under Fast ion flow Scouring Condition, the high-temperature oxidation resistant ceramic coating of carbon/carbon compound material high-speed fuel gas wash away under environment, easily come off and the oxidation protection time short.
Summary of the invention
The object of the present invention is to provide and a kind ofly can prepare densification, force of cohesion is good and high-temperature oxidation resistance is excellent Y 2si 2o 7the preparation method of crystal whisker toughened mullite compound coating.Y prepared by the present invention 2si 2o 7crystal whisker toughened mullite compound coating can extend in combustion gas and washes away the protection against oxidation time to C/C matrix material under dynamic environment.
For achieving the above object, the technical solution used in the present invention is:
Step 1: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) first, get commercially available analytically pure Si powder, C powder and WO 3powder, by Si powder: C powder: WO 3the mass ratio preparation embedding powder of powder=3 ~ 4:4 ~ 5:1.5 ~ 2.0, then puts into plumbago crucible by pretreated carbon/carbon compound material, and is imbedded in embedding powder;
2) secondly, plumbago crucible is put into vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of controlling vertical vacuum furnace is 30 ~ 50 ℃/min, furnace temperature is risen to 1700 ~ 1800 ℃ from room temperature, after insulation 0.5 ~ 1h, with stove naturally cooling, with dehydrated alcohol, will complete the carbon/carbon compound material ultrasonic cleaning 1.5 ~ 2h of embedding, ultrasonic power is 400 ~ 500W;
3) last, dry obtaining with the internally coated carbon/carbon compound material of SiC porous in the electric drying oven with forced convection of 70 ~ 80 ℃;
Step 2: adopt complexed surfactant to Y 2si 2o 7whisker carries out surface modification:
1) sodium lauryl sulphate is mixed with to the solution that concentration is 0.5 ~ 0.7mol/L, by Y 2si 2o 7whisker (is shown in patent " a kind of Y 2si 2o 7the preparation method of whisker " (number of patent application: 201210139468.X)) be immersed in solution, ultrasonic radiation 70 ~ 90min, ultrasonic power is 200 ~ 400W, then filters and isolate Y 2si 2o 7whisker;
2) by separating obtained Y 2si 2o 7whisker and Virahol are pressed Y 2si 2o 7whisker: Virahol=(8 ~ 12g): the ratio of (150 ~ 300ml) is mixed with suspension then adds iodine by (0.3 ~ 0.5) g/mL in suspension, stirs and obtains mixed solution;
Step 3: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y 2si 2o 7whisker pinning layer:
1) mixed solution step 2 being made is placed in ultrasonic electric deposition apparatus, prepared by the step 1 of take is negative electrode with the internally coated C/C matrix material of porous SiC, take graphite as anode, carry out galvanic deposit, it is 400 ~ 500W that ultrasonic power is controlled, deposition voltage is 50 ~ 60V, and deposition current is 0.2 ~ 0.3A, and depositing time is 13 ~ 20min;
2) after deposition finishes, the matrix material of negative electrode is taken off, use distilled water wash 3 ~ 5 times, at 80 ~ 120 ℃, be dried, with porous SiC, on internally coated carbon/carbon compound material, obtaining Y 2si 2o 7whisker embeds the Y of SiC hole 2si 2o 7whisker pinning layer;
Step 4: adopt water heat electrophoresis deposition legal system for Y 2si 2o 7crystal whisker toughened mullite compound coating:
1) get in the Virahol that 10 ~ 30g mullite powder is suspended in 100 ~ 300ml, magnetic agitation 10 ~ 30h, adds the iodine of 0.12 ~ 0.16g subsequently, and magnetic agitation 10 ~ 30h, is prepared into suspension;
2) with step 3, make with Y 2si 2o 7whisker embeds the Y of SiC hole 2si 2o 7the C/C matrix material of whisker pinning layer is as depositing base, fixedly depositing base is in negative electrode, anode is selected graphite cake, and suspension is poured in water heat electrophoresis deposition reactor, and controlling packing ratio is 60 ~ 70%, insulation after being heated to 160 ~ 200 ℃, adjusting deposition voltage is that 200 ~ 280V carries out water heat electrophoresis deposition, stops energising after depositing 10 ~ 30min, after sample is cooling, takes out, the baking oven that is placed in 100 ~ 120 ℃ is dry, obtains with Y 2si 2o 7the C/C matrix material sample of crystal whisker toughened mullite compound coating.
Described Si powder, C powder and WO 3the granularity of powder is 40 ~ 50 μ m.
The described C/C matrix material pre-treatment following steps of guaranteeing replacement:
1) get the 2D-carbon/carbon compound material that aircraft brake sheet is used, be processed into 30 * 30 * 30 ~ 35 * 35 * 35mm 3cubes, and the surface treatment to its chamfering of polishing, chamfering is 50 ~ 60 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 ~ 5 times, clean ultrasonic time is 50 ~ 80min at every turn, and ultrasonic power is 160 ~ 200W, finally dry in the electric drying oven with forced convection of 70 ~ 80 ℃.
The granularity of described mullite powder is 40 ~ 50 μ m.
Due to Y 2si 2o 7, mullite, SiC three have good materialization consistency, wettability and approaching thermal expansivity [C.Friedrich, R.Gadow, M.Speicher.Protective multilayercoatings for carbon-carbon composites, Surf.Coat.Technol., 2002,151-152:405-411.], therefore can fully sprawl each other packing defect.In addition Y, 2si 2o 7thermal expansivity (3.9 * 10 -6k -1) and SiC (4.5 * 10 -6k -1) comparatively approaching, can effectively prevent coating high-temp cracking and the problem coming off.Adopt the coated designs of crystal whisker toughened matrix material formula simultaneously, it can strengthen the bonding force between inside and outside coating, matrix and undercoat, effectively utilize composite principle, have complementary advantages, when improving antiscour shear stress, also can greatly improve antioxidant property.Therefore the present invention utilizes Y 2si 2o 7crystal whisker toughened mullite compound coating, has effectively extended its time of washing away steady operation in atmosphere at high-temperature fuel gas, and preparation technology is by the bonding force greatly improving between compactness, nano coating force of cohesion and the inside and outside coating of coating, has avoided subsequent disposal.
Beneficial effect:
1. the present invention adopts Y 2si 2o 7the coating structure design of the matrix material formula of crystal whisker toughened mullite utilizes composite principle, utilizes mullite and Y 2siO 5the advantage of whisker bi-material and strong point can also greatly improve its antioxidant property when improving compound coating antiscour shear stress.
2. technological operation of the present invention is controlled, temperature is low, preparation cycle is short, its organic advantage that combines the correlation techniques such as hydro-thermal, ultrasonic, electrophoresis and arc-over also simultaneously, can obtain densification, force of cohesion by force and interface in conjunction with good coating.
3. the Y that prepared by the present invention 2si 2o 7crystal whisker toughened mullite compound coating is compared with other coatings, can effectively improve oxidation resistance temperature, can obtain the protection against oxidation to C/C matrix material 400h under the dynamic Scouring Condition of high-temperature fuel gas of 1700 ℃, and oxidative mass loss is less than 0.77%.
Accompanying drawing explanation
Fig. 1 is the Y of embodiment 1 preparation 2si 2o 7y in crystal whisker toughened mullite compound coating 2si 2o 7the SEM photo of whisker pinning layer section.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is specifically described.
Embodiment 1:
Step 1:C/C matrix material pre-treatment bag:
1) get the 2D-carbon/carbon compound material that aircraft brake sheet is used, be processed into 30 * 30 * 30mm 3cubes, and the surface treatment to its chamfering of polishing, chamfering is 50 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 ~ 5 times, clean ultrasonic time is 50min at every turn, and ultrasonic power is 200W, last dry in the electric drying oven with forced convection of 70 ℃.
Step 2: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) first, get Si powder, C powder and the WO that commercially available analytically pure granularity is 40 ~ 50 μ m 3powder, by Si powder: C powder: WO 3the mass ratio preparation embedding powder of powder=4:4:1.8, then puts into plumbago crucible by pretreated carbon/carbon compound material, and is imbedded in embedding powder;
2) secondly, plumbago crucible is put into vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of controlling vertical vacuum furnace is 30 ℃/min, furnace temperature is risen to 1700 ℃ from room temperature, after insulation 1h, with stove naturally cooling, with dehydrated alcohol, will complete the carbon/carbon compound material ultrasonic cleaning 2h of embedding, ultrasonic power is 500W;
3) last, dry obtaining with the internally coated carbon/carbon compound material of SiC porous in the electric drying oven with forced convection of 80 ℃;
Step 3: adopt complexed surfactant to Y 2si 2o 7whisker carries out surface modification:
1) sodium lauryl sulphate is mixed with to the solution that concentration is 0.7mol/L, by Y 2si 2o 7whisker (is shown in patent " a kind of Y 2si 2o 7the preparation method of whisker " (number of patent application: 201210139468.X)) be immersed in solution, ultrasonic radiation 90min, ultrasonic power is 200W, then filters and isolate Y 2si 2o 7whisker;
2) by separating obtained Y 2si 2o 7whisker and Virahol are pressed Y 2si 2o 7the ratio of whisker: Virahol=8g:230ml is mixed with suspension, then in suspension, by 0.5g/mL, adds iodine, stirs and obtains mixed solution;
Step 4: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y 2si 2o 7whisker pinning layer:
1) mixed solution step 3 being made is placed in ultrasonic electric deposition apparatus, prepared by the step 2 of take is negative electrode with the internally coated C/C matrix material of porous SiC, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled as 500W, deposition voltage is 50V, and deposition current is 0.2A, and depositing time is 13min;
2) after deposition finishes, the matrix material of negative electrode is taken off, use distilled water wash 5 times, at 80 ℃, be dried, with porous SiC, on internally coated carbon/carbon compound material, obtaining Y 2si 2o 7whisker embeds the Y of SiC hole 2si 2o 7whisker pinning layer;
Step 5: adopt water heat electrophoresis deposition legal system for Y 2si 2o 7crystal whisker toughened mullite compound coating:
1) getting 10g granularity is that the mullite powder of 40 ~ 50 μ m is suspended in the Virahol of 200ml, and magnetic agitation 10h adds the iodine of 0.14g subsequently, and magnetic agitation 10h, is prepared into suspension;
2) with step 4, make with Y 2si 2o 7whisker embeds the Y of SiC hole 2si 2o 7the C/C matrix material of whisker pinning layer is as depositing base, fixedly depositing base is in negative electrode, anode is selected graphite cake, and suspension is poured in water heat electrophoresis deposition reactor, and controlling packing ratio is 70%, insulation after being heated to 160 ℃, adjusting deposition voltage is that 200V carries out water heat electrophoresis deposition, after deposition 30min, stops energising, after sample is cooling, takes out, the baking oven that is placed in 110 ℃ is dry, obtains with Y 2si 2o 7the C/C matrix material sample of crystal whisker toughened mullite compound coating.
Y as seen from Figure 1 2si 2o 7whisker closely interts in the same way between SiC undercoat and mullite external coating, whisker smooth surface, and diameter of whiskers is about 1 ~ 3 μ m, and whisker length is about 10 ~ 15 μ m.
Embodiment 2:
Step 1:C/C matrix material pre-treatment bag:
1) get the 2D-carbon/carbon compound material that aircraft brake sheet is used, be processed into 33 * 33 * 33mm 3cubes, and the surface treatment to its chamfering of polishing, chamfering is 55 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 ~ 5 times, clean ultrasonic time is 65min at every turn, and ultrasonic power is 160W, last dry in the electric drying oven with forced convection of 75 ℃.
Step 2: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) first, get Si powder, C powder and the WO that commercially available analytically pure granularity is 40 ~ 50 μ m 3powder, by Si powder: C powder: WO 3the mass ratio preparation embedding powder of powder=3.5:5:2, then puts into plumbago crucible by pretreated carbon/carbon compound material, and is imbedded in embedding powder;
2) secondly, plumbago crucible is put into vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of controlling vertical vacuum furnace is 50 ℃/min, furnace temperature is risen to 1750 ℃ from room temperature, after insulation 0.5h, with stove naturally cooling, with dehydrated alcohol, will complete the carbon/carbon compound material ultrasonic cleaning 1.5h of embedding, ultrasonic power is 400W;
3) last, dry obtaining with the internally coated carbon/carbon compound material of SiC porous in the electric drying oven with forced convection of 75 ℃;
Step 3: adopt complexed surfactant to Y 2si 2o 7whisker carries out surface modification:
1) sodium lauryl sulphate is mixed with to the solution that concentration is 0.5mol/L, by Y 2si 2o 7whisker (is shown in patent " a kind of Y 2si 2o 7the preparation method of whisker " (number of patent application: 201210139468.X)) be immersed in solution, ultrasonic radiation 70min, ultrasonic power is 300W, then filters and isolate Y 2si 2o 7whisker;
2) by separating obtained Y 2si 2o 7whisker and Virahol are pressed Y 2si 2o 7the ratio of whisker: Virahol=10g:150ml is mixed with suspension, then in suspension, by 0.3g/mL, adds iodine, stirs and obtains mixed solution;
Step 4: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y 2si 2o 7whisker pinning layer:
1) mixed solution step 3 being made is placed in ultrasonic electric deposition apparatus, prepared by the step 2 of take is negative electrode with the internally coated C/C matrix material of porous SiC, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled as 400W, deposition voltage is 55V, and deposition current is 0.3A, and depositing time is 17min;
2) after deposition finishes, the matrix material of negative electrode is taken off, use distilled water wash 3 times, at 100 ℃, be dried, with porous SiC, on internally coated carbon/carbon compound material, obtaining Y 2si 2o 7whisker embeds the Y of SiC hole 2si 2o 7whisker pinning layer;
Step 5: adopt water heat electrophoresis deposition legal system for Y 2si 2o 7crystal whisker toughened mullite compound coating:
1) getting 20g granularity is that the mullite powder of 40 ~ 50 μ m is suspended in the Virahol of 100ml, and magnetic agitation 20h adds the iodine of 0.16g subsequently, and magnetic agitation 20h, is prepared into suspension;
2) with step 4, make with Y 2si 2o 7whisker embeds the Y of SiC hole 2si 2o 7the C/C matrix material of whisker pinning layer is as depositing base, fixedly depositing base is in negative electrode, anode is selected graphite cake, and suspension is poured in water heat electrophoresis deposition reactor, and controlling packing ratio is 65%, insulation after being heated to 180 ℃, adjusting deposition voltage is that 240V carries out water heat electrophoresis deposition, after deposition 20min, stops energising, after sample is cooling, takes out, the baking oven that is placed in 120 ℃ is dry, obtains with Y 2si 2o 7the C/C matrix material sample of crystal whisker toughened mullite compound coating.
Embodiment 3:
Step 1:C/C matrix material pre-treatment bag:
1) get the 2D-carbon/carbon compound material that aircraft brake sheet is used, be processed into 35 * 35 * 35mm 3cubes, and the surface treatment to its chamfering of polishing, chamfering is 60 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 ~ 5 times, clean ultrasonic time is 80min at every turn, and ultrasonic power is 180W, last dry in the electric drying oven with forced convection of 80 ℃.
Step 2: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) first, get Si powder, C powder and the WO that commercially available analytically pure granularity is 40 ~ 50 μ m 3powder, by Si powder: C powder: WO 3the mass ratio preparation embedding powder of powder=3:4.5:1.5, then puts into plumbago crucible by pretreated carbon/carbon compound material, and is imbedded in embedding powder;
2) secondly, plumbago crucible is put into vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of controlling vertical vacuum furnace is 40 ℃/min, furnace temperature is risen to 1800 ℃ from room temperature, after insulation 1h, with stove naturally cooling, with dehydrated alcohol, will complete the carbon/carbon compound material ultrasonic cleaning 2h of embedding, ultrasonic power is 450W;
3) last, dry obtaining with the internally coated carbon/carbon compound material of SiC porous in the electric drying oven with forced convection of 70 ℃;
Step 3: adopt complexed surfactant to Y 2si 2o 7whisker carries out surface modification:
1) sodium lauryl sulphate is mixed with to the solution that concentration is 0.6mol/L, by Y 2si 2o 7whisker (is shown in patent " a kind of Y 2si 2o 7the preparation method of whisker " (number of patent application: 201210139468.X)) be immersed in solution, ultrasonic radiation 80min, ultrasonic power is 400W, then filters and isolate Y 2si 2o 7whisker;
2) by separating obtained Y 2si 2o 7whisker and Virahol are pressed Y 2si 2o 7the ratio of whisker: Virahol=12g:300ml is mixed with suspension, then in suspension, by 0.4g/mL, adds iodine, stirs and obtains mixed solution;
Step 4: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y 2si 2o 7whisker pinning layer:
1) mixed solution step 3 being made is placed in ultrasonic electric deposition apparatus, prepared by the step 2 of take is negative electrode with the internally coated C/C matrix material of porous SiC, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled as 450W, deposition voltage is 60V, and deposition current is 0.2A, and depositing time is 20min;
2) after deposition finishes, the matrix material of negative electrode is taken off, use distilled water wash 4 times, at 120 ℃, be dried, with porous SiC, on internally coated carbon/carbon compound material, obtaining Y 2si 2o 7whisker embeds the Y of SiC hole 2si 2o 7whisker pinning layer;
Step 5: adopt water heat electrophoresis deposition legal system for Y 2si 2o 7crystal whisker toughened mullite compound coating:
1) getting 30g granularity is that the mullite powder of 40 ~ 50 μ m is suspended in the Virahol of 300ml, and magnetic agitation 30h adds the iodine of 0.12g subsequently, and magnetic agitation 30h, is prepared into suspension;
2) with step 4, make with Y 2si 2o 7whisker embeds the Y of SiC hole 2si 2o 7the C/C matrix material of whisker pinning layer is as depositing base, fixedly depositing base is in negative electrode, anode is selected graphite cake, and suspension is poured in water heat electrophoresis deposition reactor, and controlling packing ratio is 60%, insulation after being heated to 200 ℃, adjusting deposition voltage is that 280V carries out water heat electrophoresis deposition, after deposition 10min, stops energising, after sample is cooling, takes out, the baking oven that is placed in 100 ℃ is dry, obtains with Y 2si 2o 7the C/C matrix material sample of crystal whisker toughened mullite compound coating.

Claims (4)

1. a Y 2si 2o 7the preparation method of crystal whisker toughened mullite compound coating, is characterized in that:
Step 1: adopt entrapping method to prepare SiC porous undercoat in carbon/carbon composite material base surface
1) first, get commercially available analytically pure Si powder, C powder and WO 3powder, by Si powder: C powder: WO 3the mass ratio preparation embedding powder of powder=3～4:4～5:1.5～2.0, then puts into plumbago crucible by pretreated carbon/carbon compound material, and is imbedded in embedding powder;
2) secondly, plumbago crucible is put into vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of controlling vertical vacuum furnace is 30～50 ℃/min, furnace temperature is risen to 1700～1800 ℃ from room temperature, after insulation 0.5～1h, with stove naturally cooling, with dehydrated alcohol, will complete the carbon/carbon compound material ultrasonic cleaning 1.5～2h of embedding, ultrasonic power is 400～500W;
3) last, dry obtaining with the internally coated carbon/carbon compound material of SiC porous in the electric drying oven with forced convection of 70～80 ℃;
Step 2: adopt complexed surfactant to Y 2si 2o 7whisker carries out surface modification:
1) sodium lauryl sulphate is mixed with to the solution that concentration is 0.5～0.7mol/L, by Y 2si 2o 7whisker is immersed in solution, ultrasonic radiation 70～90min, and ultrasonic power is 200～400W, then filters and isolate Y 2si 2o 7whisker;
2) by separating obtained Y 2si 2o 7whisker and Virahol are pressed Y 2si 2o 7whisker: Virahol=(8～12g): the ratio of (150～300mL) is mixed with suspension then adds iodine by (0.3～0.5) g/mL in suspension, stirs and obtains mixed solution;
Step 3: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y 2si 2o 7whisker pinning layer:
1) mixed solution step 2 being made is placed in ultrasonic electric deposition apparatus, prepared by the step 1 of take is negative electrode with the internally coated carbon/carbon compound material of porous SiC, take graphite as anode, carry out galvanic deposit, it is 400～500W that ultrasonic power is controlled, deposition voltage is 50～60V, and deposition current is 0.2～0.3A, and depositing time is 13～20min;
2) after deposition finishes, the matrix material of negative electrode is taken off, use distilled water wash 3～5 times, at 80～120 ℃, be dried, with porous SiC, on internally coated carbon/carbon compound material, obtaining Y 2si 2o 7whisker embeds the Y of SiC hole 2si 2o 7whisker pinning layer;
Step 4: adopt water heat electrophoresis deposition legal system for Y 2si 2o 7crystal whisker toughened mullite compound coating:
1) get in the Virahol that 10～30g mullite powder is suspended in 100～300mL, magnetic agitation 10～30h, adds the iodine of 0.12～0.16g subsequently, and magnetic agitation 10～30h, is prepared into suspension;
2) with step 3, make with Y 2si 2o 7whisker embeds the Y of SiC hole 2si 2o 7the carbon/carbon compound material of whisker pinning layer is as depositing base, fixedly depositing base is in negative electrode, anode is selected graphite cake, and suspension is poured in water heat electrophoresis deposition reactor, and controlling packing ratio is 60～70%, insulation after being heated to 160～200 ℃, adjusting deposition voltage is that 200～280V carries out water heat electrophoresis deposition, stops energising after depositing 10～30min, after sample is cooling, takes out, the baking oven that is placed in 100～120 ℃ is dry, obtains with Y 2si 2o 7the carbon/carbon compound material sample of crystal whisker toughened mullite compound coating.
2. Y according to claim 1 2si 2o 7the preparation method of crystal whisker toughened mullite compound coating, is characterized in that: described Si powder, C powder and WO 3the granularity of powder is 40～50 μ m.
3. Y according to claim 1 2si 2o 7the preparation method of crystal whisker toughened mullite compound coating, is characterized in that: described carbon/carbon compound material pre-treatment comprises the following steps:
1) get the 2D-carbon/carbon compound material that aircraft brake sheet is used, be processed into 30 * 30 * 30～35 * 35 * 35mm 3cubes, and the surface treatment to its chamfering of polishing, chamfering is 50～60 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3～5 times, clean ultrasonic time is 50～80min at every turn, and ultrasonic power is 160～200W, last dry in the electric drying oven with forced convection of 70～80 ℃.
4. Y according to claim 1 2si 2o 7the preparation method of crystal whisker toughened mullite compound coating, is characterized in that: the granularity of described mullite powder is 40～50 μ m.
CN201210458776.9A 2012-11-14 2012-11-14 Method for preparing Y2Si2O7 whisker-toughened mullite composite coating Active CN102924108B (en)

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