CN102951920B - Preparation method of Y4Si3O12 whisker toughened mullite composite coating - Google Patents
Preparation method of Y4Si3O12 whisker toughened mullite composite coating Download PDFInfo
- Publication number
- CN102951920B CN102951920B CN201210458003.0A CN201210458003A CN102951920B CN 102951920 B CN102951920 B CN 102951920B CN 201210458003 A CN201210458003 A CN 201210458003A CN 102951920 B CN102951920 B CN 102951920B
- Authority
- CN
- China
- Prior art keywords
- whisker
- carbon
- powder
- deposition
- sic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000576 coating method Methods 0.000 title claims abstract description 47
- 239000011248 coating agent Substances 0.000 title claims abstract description 44
- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000000151 deposition Methods 0.000 claims abstract description 66
- 230000008021 deposition Effects 0.000 claims abstract description 51
- 238000001962 electrophoresis Methods 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000012986 modification Methods 0.000 claims abstract description 8
- 230000004048 modification Effects 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 53
- 229910052799 carbon Inorganic materials 0.000 claims description 43
- 239000000843 powder Substances 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 34
- 239000011159 matrix material Substances 0.000 claims description 33
- 150000001722 carbon compounds Chemical class 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000013078 crystal Substances 0.000 claims description 22
- 239000010439 graphite Substances 0.000 claims description 20
- -1 mullite compound Chemical class 0.000 claims description 20
- 239000000725 suspension Substances 0.000 claims description 20
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 15
- 239000011863 silicon-based powder Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 241000209456 Plumbago Species 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 7
- 229910052740 iodine Inorganic materials 0.000 claims description 7
- 239000011630 iodine Substances 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 5
- 230000005855 radiation Effects 0.000 claims description 5
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 20
- 230000003647 oxidation Effects 0.000 abstract description 18
- 230000003064 anti-oxidating effect Effects 0.000 abstract description 4
- 238000001652 electrophoretic deposition Methods 0.000 abstract description 2
- 230000003628 erosive effect Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 230000004580 weight loss Effects 0.000 abstract 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 33
- 238000005516 engineering process Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 229910019974 CrSi Inorganic materials 0.000 description 4
- 150000001721 carbon Chemical class 0.000 description 4
- 229910016006 MoSi Inorganic materials 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000002737 fuel gas Substances 0.000 description 3
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 3
- 239000011253 protective coating Substances 0.000 description 3
- 229910007991 Si-N Inorganic materials 0.000 description 2
- 229910006295 Si—Mo Inorganic materials 0.000 description 2
- 229910006294 Si—N Inorganic materials 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000009991 scouring Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 206010037660 Pyrexia Diseases 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- IUHFWCGCSVTMPG-UHFFFAOYSA-N [C].[C] Chemical class [C].[C] IUHFWCGCSVTMPG-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002103 nanocoating Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of an Y4Si3O12 whisker toughened mullite composite coating. The preparation method comprises the following steps of: preparing a SiC porous internal coating on the surface of a C/C composite material substrate by using an embedding method; preparing Y4Si3O12 whisker and performing surface modification on the Y4Si3O12 whisker by using composite surfactant to obtain mixed solution; performing ultrasonic electrophoresis selective assembly and deposition by using the C/C composite material prepared with the SiC porous internal coating on the surface and the mixed solution to obtain a Y4Si3O12 whisker pinning layer; and finally preparing the Y4Si3O12 whisker toughened mullite composite coating by using a hydrothermal electrophoretic deposition method. Compared with other coatings, the Y4Si3O12 whisker toughened mullite composite coating has the advantages that the anti-oxidation temperature can be effectively improved, anti-oxidation protection of 450 hours for the C/C composite material can be achieved under the high-temperature gas dynamic erosion condition of 1,500 DEG C, and the oxidation weight loss ratio is less than 0.62 percent.
Description
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
4si
3o
12the 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 protection of 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 on C/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 paintingfor 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 coatingfor 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 a kind of Y
4si
3o
12the preparation method of crystal whisker toughened mullite compound coating.The prepared Y that compound coating is fine and close, force of cohesion is good and high-temperature oxidation resistance is excellent
4si
3o
12crystal whisker toughened mullite compound coating, can extend in combustion gas and wash 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 B
2o
3powder, by Si powder: C powder: B
2o
3powder=(3 ~ 5): (4 ~ 6): the mass ratio preparation embedding powder of (1.5 ~ 2.0), then pretreated carbon/carbon compound material is put into plumbago crucible, and 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
4si
3o
12whisker carries out surface modification:
1) Sodium dodecylbenzene sulfonate is mixed with to the solution that concentration is 0.5 ~ 0.7mol/L, by Y
4si
3o
12whisker (is shown in patent " a kind of Y
4si
3o
12the preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in solution, ultrasonic radiation 70 ~ 90min, ultrasonic power is 200 ~ 400W, then filters and isolate Y
4si
3o
12whisker;
2) by separating obtained Y
4si
3o
12whisker and Virahol are pressed Y
4si
3o
12whisker: 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
4si
3o
12whisker 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
4si
3o
12whisker embeds the Y of SiC hole
4si
3o
12whisker pinning layer;
Step 4: adopt water heat electrophoresis deposition legal system for Y
4si
3o
12crystal 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
4si
3o
12whisker embeds the Y of SiC hole
4si
3o
12the 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 ~ 260V carries out water heat electrophoresis deposition, after deposition 10 ~ 30min, stops energising, after sample is cooling, takes out, the baking oven that is placed in 100 ~ 120 ℃ is dry, obtains with Y
4si
3o
12the C/C matrix material sample of crystal whisker toughened mullite compound coating.
Described Si powder, C powder and B
2o
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 45 * 45 * 45 ~ 50 * 50 * 50mm
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
4si
3o
12, 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,
4si
3o
12thermal expansivity (4.3 * 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.Not only 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
4si
3o
12the 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. this novel Y
4si
3o
12crystal 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 450h under the dynamic Scouring Condition of high-temperature fuel gas of 1500 ℃, and oxidative mass loss is less than 0.62%.
Accompanying drawing explanation
Fig. 1 is the Y of embodiment 1 preparation
4si
3o
12the SEM photo on crystal whisker toughened mullite compound coating surface.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
Embodiment 1:
The pre-treatment of step 1:C/C matrix material:
1) get the 2D-carbon/carbon compound material that aircraft brake sheet is used, be processed into 50 * 50 * 50mm
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 times, clean ultrasonic time is 80min 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 B that commercially available analytically pure granularity is 40 ~ 50 μ m
2o
3powder, by Si powder: C powder: B
2o
3the mass ratio preparation embedding powder of powder=3:5:1.8, 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
4si
3o
12whisker carries out surface modification:
1) Sodium dodecylbenzene sulfonate is mixed with to the solution that concentration is 0.7mol/L, by Y
4si
3o
12whisker (is shown in patent " a kind of Y
4si
3o
12the preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in solution, ultrasonic radiation 90min, ultrasonic power is 200W, then filters and isolate Y
4si
3o
12whisker;
2) by separating obtained Y
4si
3o
12whisker and Virahol are pressed Y
4si
3o
12the 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
4si
3o
12whisker 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 0.1A, 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
4si
3o
12whisker embeds the Y of SiC hole
4si
3o
12whisker pinning layer;
Step 5: adopt water heat electrophoresis deposition legal system for Y
4si
3o
12crystal 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
4si
3o
12whisker embeds the Y of SiC hole
4si
3o
12the 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 200 ℃, adjusting deposition voltage is that 230V 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
4si
3o
12the C/C matrix material sample of crystal whisker toughened mullite compound coating.
Y as seen from Figure 1
4si
3o
12whisker is sprawled in the same way and is interspersed in mullite coating, and compound coating even compact, does not have crackle.
Embodiment 2:
The pre-treatment of step 1:C/C matrix material:
1) get the 2D-carbon/carbon compound material that aircraft brake sheet is used, be processed into 45 * 45 * 45mm
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 4 times, clean ultrasonic time is 50min at every turn, and ultrasonic power is 180W, 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 B that commercially available analytically pure granularity is 40 ~ 50 μ m
2o
3powder, by Si powder: C powder: B
2o
3the mass ratio preparation embedding powder of powder=4:6:2, 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
4si
3o
12whisker carries out surface modification:
1) Sodium dodecylbenzene sulfonate is mixed with to the solution that concentration is 0.5mol/L, by Y
4si
3o
12whisker (is shown in patent " a kind of Y
4si
3o
12the preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in solution, ultrasonic radiation 70min, ultrasonic power is 300W, then filters and isolate Y
4si
3o
12whisker;
2) by separating obtained Y
4si
3o
12whisker and Virahol are pressed Y
4si
3o
12the 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
4si
3o
12whisker 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
4si
3o
12whisker embeds the Y of SiC hole
4si
3o
12whisker pinning layer;
Step 5: adopt water heat electrophoresis deposition legal system for Y
4si
3o
12crystal 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
4si
3o
12whisker embeds the Y of SiC hole
4si
3o
12the 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 260V 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
4si
3o
12the C/C matrix material sample of crystal whisker toughened mullite compound coating.
Embodiment 3:
The pre-treatment of step 1:C/C matrix material:
1) get the 2D-carbon/carbon compound material that aircraft brake sheet is used, be processed into 48 * 48 * 48mm
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 5 times, clean ultrasonic time is 60min at every turn, and ultrasonic power is 160W, 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 B that commercially available analytically pure granularity is 40 ~ 50 μ m
2o
3powder, by Si powder: C powder: B
2o
3the mass ratio preparation embedding powder of powder=5:4:1.5, 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
4si
3o
12whisker carries out surface modification:
1) Sodium dodecylbenzene sulfonate is mixed with to the solution that concentration is 0.6mol/L, by Y
4si
3o
12whisker (is shown in patent " a kind of Y
4si
3o
12the preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in solution, ultrasonic radiation 80min, ultrasonic power is 400W, then filters and isolate Y
4si
3o
12whisker;
2) by separating obtained Y
4si
3o
12whisker and Virahol are pressed Y
4si
3o
12the 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
4si
3o
12whisker 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
4si
3o
12whisker embeds the Y of SiC hole
4si
3o
12whisker pinning layer;
Step 5: adopt water heat electrophoresis deposition legal system for Y
4si
3o
12crystal 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
4si
3o
12whisker embeds the Y of SiC hole
4si
3o
12the 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 160 ℃, adjusting deposition voltage is that 200V 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
4si
3o
12the C/C matrix material sample of crystal whisker toughened mullite compound coating.
Claims (4)
1. a Y
4si
3o
12the 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 B
2o
3powder, by Si powder: C powder: B
2o
3powder=(3～5): (4～6): the mass ratio preparation embedding powder of (1.5～2.0), then pretreated carbon/carbon compound material is put into plumbago crucible, and 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
4si
3o
12whisker carries out surface modification:
1) Sodium dodecylbenzene sulfonate is mixed with to the solution that concentration is 0.5～0.7mol/L, by Y
4si
3o
12whisker is immersed in solution, ultrasonic radiation 70～90min, and ultrasonic power is 200～400W, then filters and isolate Y
4si
3o
12whisker;
2) by separating obtained Y
4si
3o
12whisker and Virahol are pressed Y
4si
3o
12whisker: 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
4si
3o
12whisker 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
4si
3o
12whisker embeds the Y of SiC hole
4si
3o
12whisker pinning layer;
Step 4: adopt water heat electrophoresis deposition legal system for Y
4si
3o
12crystal 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
4si
3o
12whisker embeds the Y of SiC hole
4si
3o
12the 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 200～260V carries out water heat electrophoresis deposition, after deposition 10～30min, stops energising, after sample is cooling, takes out, the baking oven that is placed in 100～120 ℃ is dry, obtains with Y
4si
3o
12the carbon/carbon compound material sample of crystal whisker toughened mullite compound coating.
2. Y according to claim 1
4si
3o
12the preparation method of crystal whisker toughened mullite compound coating, is characterized in that: described Si powder, C powder and B
2o
3the granularity of powder is 40～50 μ m.
3. Y according to claim 1
4si
3o
12the 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 45 * 45 * 45～50 * 50 * 50mm
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
4si
3o
12the preparation method of crystal whisker toughened mullite compound coating, is characterized in that: the granularity of described mullite powder is 40～50 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210458003.0A CN102951920B (en) | 2012-11-14 | 2012-11-14 | Preparation method of Y4Si3O12 whisker toughened mullite composite coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210458003.0A CN102951920B (en) | 2012-11-14 | 2012-11-14 | Preparation method of Y4Si3O12 whisker toughened mullite composite coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102951920A CN102951920A (en) | 2013-03-06 |
| CN102951920B true CN102951920B (en) | 2014-04-16 |
Family
ID=47761375
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210458003.0A Active CN102951920B (en) | 2012-11-14 | 2012-11-14 | Preparation method of Y4Si3O12 whisker toughened mullite composite coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102951920B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114644531B (en) * | 2022-03-30 | 2022-11-29 | 陕西科技大学 | Method for preparing B2O3@ SiO2 core-shell-SiC coating on surface of C/C composite material and composite coating |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677174A (en) * | 2012-05-08 | 2012-09-19 | 陕西科技大学 | Preparation method of Y4Si3O12 crystal whiskers |
-
2012
- 2012-11-14 CN CN201210458003.0A patent/CN102951920B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102677174A (en) * | 2012-05-08 | 2012-09-19 | 陕西科技大学 | Preparation method of Y4Si3O12 crystal whiskers |
Non-Patent Citations (4)
| Title |
|---|
| Y2Si2O7晶须增强MoSi2复合涂层的制备及性能;王雅琴等;《复合材料学报》;20100430;第27卷(第2期);58-61 * |
| 王雅琴等.Y2Si2O7晶须增强MoSi2复合涂层的制备及性能.《复合材料学报》.2010,第27卷(第2期),58-61. |
| 硅酸钇高温抗氧化涂层的研究进展;邓飞等;《硅酸盐通报》;20070228;第26卷(第1期);101-105 * |
| 邓飞等.硅酸钇高温抗氧化涂层的研究进展.《硅酸盐通报》.2007,第26卷(第1期),101-105. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102951920A (en) | 2013-03-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102924108B (en) | Method for preparing Y2Si2O7 whisker-toughened mullite composite coating | |
| CN101514473B (en) | Method for preparing yttrium silicate coat by cathode rotation hydrothermal electrophoretic deposition | |
| CN108484190B (en) | Preparation method of carbon fiber reinforced multiphase carbide ceramic matrix composite | |
| CN106045550B (en) | The preparation method of SiC-ZrC gradient modifying carbon/carbon composite materials | |
| CN110357635A (en) | A method of improving carbon-based or ceramic matric composite surface oxidation-resistant coating bond strength | |
| CN101885623A (en) | Method for preparing carbon/carbon composite material mullite external coating by pulsed hydrothermal electrophoresis sedimentation method | |
| CN102674903B (en) | Preparation method of SiC/C-AlPO4-mullite antioxidation coating for C/C composite material | |
| CN106631161B (en) | A method of composite coating resistant to high temperature oxidation is prepared on carbon-based material surface | |
| CN102936145B (en) | Preparation method of Y2SiO5 whisker toughened mullite composite coating | |
| CN106083120A (en) | One prepares gradient-structure C/C MoSi2the method of SiC ceramic matrix composite material | |
| CN110304932A (en) | One kind having HfB2The preparation method of the Cf/SiC composite material at interface | |
| CN102936146B (en) | Preparation method of Y2Si2O7 whisker toughened Y2SiO5 composite coating | |
| CN102951920B (en) | Preparation method of Y4Si3O12 whisker toughened mullite composite coating | |
| CN105198500B (en) | A kind of laminar C/C MoSi2The preparation method of composite | |
| CN102951921B (en) | Preparation method of Y4Si3O12 whisker toughened Y2SiO5 composite coating | |
| CN101514474B (en) | Method for preparing Y2SiO5/MoSi2 composite coat by sonoelectrodeposition | |
| CN102942387B (en) | Preparation method of Y2Si2O7 crystal whisker toughening Y2Si2O7 composite coatings | |
| CN103044076B (en) | Method for preparing carbon/carbon composite yttrium silicate whisker reinforced mullite-C-AlPO4 complex external coating | |
| CN105669231A (en) | Preparation method of carbon fiber reinforced MoSi2-SiC ceramic matrix composite | |
| CN102936144B (en) | Method for preparing Y4Si3O12 crystal whisker toughening Y2Si2O7 composite coating | |
| CN102942379B (en) | Preparation method of Y4Si3O12 crystal whisker toughening Y4Si3O12 composite coatings | |
| CN115894085A (en) | Composite ceramic coating material and preparation method and application thereof | |
| CN106083209B (en) | A kind of preparation method of micro-structured configuration interlayer interface Mullite/ yttrium silicate composite coatings | |
| CN102924107B (en) | Method for preparing Y2SiO5 whisker toughened Y4Si3O12 composite coating | |
| CN104130021B (en) | The preparation method of the crystal whisker toughened mullite compound coating of a kind of carbon/carbon composite mullite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210531 Address after: 518000 No.6 Qinglong Road, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Pengbo Information Technology Co.,Ltd. Address before: No. 1, Weiyang District university garden, Xi'an, Shaanxi Province, Shaanxi Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY Effective date of registration: 20210531 Address after: 518000 no.2b, building 1, wanpan garden, Shahe, Nanshan District, Shenzhen City, Guangdong Province Patentee after: Wu Wenjie Address before: 518000 No.6 Qinglong Road, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee before: Shenzhen Pengbo Information Technology Co.,Ltd. |