CN102951921A - Preparation method of Y4Si3O12 whisker toughened Y2SiO5 composite coating - Google Patents
Preparation method of Y4Si3O12 whisker toughened Y2SiO5 composite coating Download PDFInfo
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- CN102951921A CN102951921A CN2012104581739A CN201210458173A CN102951921A CN 102951921 A CN102951921 A CN 102951921A CN 2012104581739 A CN2012104581739 A CN 2012104581739A CN 201210458173 A CN201210458173 A CN 201210458173A CN 102951921 A CN102951921 A CN 102951921A
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- 238000000576 coating method Methods 0.000 title claims abstract description 45
- 239000011248 coating agent Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 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 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 238000012986 modification Methods 0.000 claims abstract description 8
- 230000004048 modification Effects 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 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 47
- 239000000843 powder Substances 0.000 claims description 41
- 239000011159 matrix material Substances 0.000 claims description 34
- 229910052799 carbon Inorganic materials 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 30
- 150000001722 carbon compounds Chemical class 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000013078 crystal Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- 239000010439 graphite Substances 0.000 claims description 20
- 239000000725 suspension Substances 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 16
- 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
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 10
- 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
- 229960000935 dehydrated alcohol Drugs 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
- 229910052740 iodine Inorganic materials 0.000 claims description 10
- 239000011630 iodine Substances 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- 206010013786 Dry skin Diseases 0.000 claims description 5
- 229910003923 SiC 4 Inorganic materials 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 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
- 238000012856 packing Methods 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
- 238000001073 sample cooling Methods 0.000 claims description 5
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 5
- 238000001652 electrophoretic deposition Methods 0.000 abstract description 2
- 239000002103 nanocoating Substances 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 230000003628 erosive effect Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 description 17
- 230000003647 oxidation Effects 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 6
- 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 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
- 230000003064 anti-oxidating effect Effects 0.000 description 2
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 2
- 239000002737 fuel gas Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 230000003026 anti-oxygenic effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000013459 approach Methods 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
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of an Y4Si3O12 whisker toughened Y2SiO5 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 Y2SiO5 composite coating by using a hydrothermal electrophoretic deposition method. According to the Y4Si3O12 whisker toughened Y2SiO5 composite coating, the time for stable work of the Y4Si3O12 whisker toughened Y2SiO5 composite coating in a high-temperature gas erosion atmosphere is effectively prolonged; and according to the preparation process, the compactness of the coating, the cohesion of a nanocoating and the binding force of internal and external coatings are greatly improved, and subsequent treatment is avoided.
Description
Technical field
The invention belongs to the 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
12Crystal whisker toughened Y
2SiO
5The preparation method of 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, anti-ablation, high strength, high-modulus, particularly 2200 ℃ of inert atmosphere with interior condition under its strength and modulus with the excellent properties that temperature raises and increases, it is had broad application prospects at aerospace field.Yet the C/C matrix material will be oxidized at the aerobic environment that surpasses 450 ℃, and the 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 takes full advantage of its performance.
Improve the C/C compound material antioxygenic property and mainly contain two kinds of approach: a kind of is the matrix modification technology; A kind of is the top coat technology.Studies show that, the matrix modification technology is only applicable to low-temperature zone to the oxidation protection of C/C material.Coating technology then 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 other compound coating take SiC as transition layer, such as SiC-B4C/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 the Fast ion flow Scouring Condition, the high-temperature oxidation resistant ceramic coating of carbon/carbon compound material high-speed fuel gas wash away easily come off under the environment 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
12Crystal whisker toughened Y
2SiO
5The preparation method of compound coating, prepared Y
4Si
3O
12Crystal whisker toughened Y
2SiO
5Compound coating is fine and close, force of cohesion is good and high-temperature oxidation resistance is excellent, can prolong in combustion gas to wash away under the dynamic environment protection against oxidation time to the C/C matrix material.
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) at first, gets commercially available analytically pure Si powder, C powder and B
2O
3Powder is pressed the Si powder: C powder: B
2O
3Powder=(3 ~ 5): (4 ~ 6): the mass ratio preparation embedding powder of (0.5 ~ 1.0), then pretreated carbon/carbon compound material is put into plumbago crucible, and it is imbedded in the embedding powder;
2) secondly, plumbago crucible is put into vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of control vertical vacuum furnace is 10 ~ 20 ℃/min, after furnace temperature risen to 1500 ~ 1600 ℃ from room temperature, with the stove naturally cooling, will finish the carbon/carbon compound material ultrasonic cleaning 0.5 ~ 1h of embedding with dehydrated alcohol behind insulation 2 ~ 3h, ultrasonic power is 200 ~ 300W;
3) last, drying obtains with the internally coated carbon/carbon compound material of SiC porous in 50 ~ 60 ℃ electric drying oven with forced convection;
Step 2: adopt complexed surfactant to Y
4Si
3O
12Whisker carries out surface modification:
1) sodium lauryl sulphate is mixed with the solution that concentration is 0.3 ~ 0.5mol/L, with Y
4Si
3O
12Whisker (is seen patent " a kind of Y
4Si
3O
12The preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in the solution, and ultrasonic radiation 30 ~ 50min, ultrasonic power are 400 ~ 600W, then filter and isolate Y
4Si
3O
12Whisker;
2) with separating obtained Y
4Si
3O
12Whisker and Virahol are pressed Y
4Si
3O
12Whisker: Virahol=(8 ~ 12g): (150 ~ 300ml) ratio is mixed with suspension, then adds iodine by (0.1 ~ 0.3) g/mL in suspension, stirs and obtains mixed solution;
Step 3: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y
4Si
3O
12The whisker pinning layer:
1) mixed solution that step 2 is made places the ultrasonic electric deposition apparatus, take step 1 preparation with the internally coated C/C matrix material of porous SiC as negative electrode, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled to be 200 ~ 300W, deposition voltage is 30 ~ 40V, and deposition current is 0.05 ~ 0.1A, and depositing time is 3 ~ 7min;
2) after deposition finishes, the matrix material of negative electrode is taken off, with distilled water wash 3 ~ 5 times, 80 ~ 120 ℃ of dryings, namely obtaining Y with the internally coated carbon/carbon compound material of porous SiC
4Si
3O
12Whisker embeds the Y of SiC hole
4Si
3O
12The whisker pinning layer;
Step 4: adopt the standby Y of water heat electrophoresis deposition legal system
4Si
3O
12Crystal whisker toughened Y
2SiO
5Compound coating:
1) gets 10 ~ 30g Y
2SiO
5Powder is suspended in the Virahol of 100 ~ 300ml, and magnetic agitation 10 ~ 30h adds the iodine of 0.02 ~ 0.06g 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 the water heat electrophoresis deposition reactor, and the control packing ratio is 40 ~ 50%, insulation after being heated to 80 ~ 120 ℃, adjusting deposition voltage is that 150 ~ 180V carries out water heat electrophoresis deposition, stops energising behind deposition 40 ~ 50min, takes out after the sample cooling, place 60 ~ 80 ℃ baking oven dry, obtain with Y
4Si
3O
12Crystal whisker toughened Y
2SiO
5The C/C matrix material sample of compound coating.
Described Si powder, C powder and B
2O
3The granularity of powder is 20 ~ 30 μ m.
The described C/C matrix material pre-treatment following steps of guaranteeing replacement:
1) gets the 2D-carbon/carbon compound material that the aircraft brake sheet is used, be processed into 35 * 35 * 35 ~ 40 * 40 * 40mm
3Cubes, and to the surface treatment of its chamfering of polishing, chamfering is 30 ~ 40 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 ~ 5 times, clean ultrasonic time is 10 ~ 30min at every turn, and ultrasonic power is 80 ~ 120W, dry in 50 ~ 60 ℃ electric drying oven with forced convection at last.
Described Y
2SiO
5The granularity of powder is 20 ~ 30 μ m.
The yttrium silicate of different crystal forms all has higher fusing point, Y
2SiO
5Fusing point be 1980 ℃, Y
4Si
3O
12Fusing point be 1950 ℃.Y
2SiO
5Not only have quite high fusing point, and oxygen permeability being extremely low under the high temperature of 1973K, only is 1 * 10
-10Kg/ (m
-s) [OguraY, Kondo M, Mormoto T, et al.Oxygen permeability of Y
2SiO
5[J] .Materials Transactions, 2001,42 (6): 1124-1130.].Y
2SiO
5Thermal expansivity be 6.9 * 10
-6K
-1, Y
4Si
3O
12Thermal expansivity be 4.3 * 10
-6K
-1, the thermal expansivity (4.5 * 10 of the two and SiC
-6K
-1) very approaching, Y
4Si
3O
12Can effectively prevent coating high-temp cracking and the problem that comes off as the external coating (EC) of being combined with the SiC undercoat, adopt simultaneously the coated designs of crystal whisker toughened matrix material formula, it can effectively utilize composite principle, have complementary advantages, when improving the antiscour shear stress, also can greatly improve antioxidant property.Y
4Si
3O
12Crystal whisker toughened Y
2SiO
5Compound coating has effectively prolonged it in the time that high-temperature fuel gas washes away steady operation in the atmosphere, and preparation technology will improve the bonding force between compactness, nano coating force of cohesion and the inside and outside coating of coating greatly, has avoided subsequent disposal.
Description of drawings
Fig. 1 is the Y of embodiment 1 preparation
4Si
3O
12Crystal whisker toughened Y
2SiO
5The SEM photo of compound coating section.
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing.
Embodiment 1:
The pre-treatment of step 1:C/C matrix material:
1) gets the 2D-carbon/carbon compound material that the aircraft brake sheet is used, be processed into 35 * 35 * 35mm
3Cubes, and to the surface treatment of its chamfering of polishing, chamfering is 30 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 4 times, clean ultrasonic time is 10min at every turn, and ultrasonic power is 80W, last dry in 50 ℃ electric drying oven with forced convection.
Step 2: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) at first, gets Si powder, C powder and the B that commercially available analytically pure granularity is 20 ~ 30 μ m
2O
3Powder is pressed the Si powder: C powder: B
2O
3Then the mass ratio preparation embedding powder of powder=3:5:0.5 is put into plumbago crucible with pretreated carbon/carbon compound material, and it is imbedded in the embedding powder;
2) secondly, plumbago crucible is put into vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of control vertical vacuum furnace is 10 ℃/min, after furnace temperature risen to 1500 ℃ from room temperature, with the stove naturally cooling, will finish the carbon/carbon compound material ultrasonic cleaning 0.5h of embedding with dehydrated alcohol behind the insulation 3h, ultrasonic power is 300W;
3) last, drying obtains with the internally coated carbon/carbon compound material of SiC porous in 50 ℃ electric drying oven with forced convection;
Step 3: adopt complexed surfactant to Y
4Si
3O
12Whisker carries out surface modification:
1) sodium lauryl sulphate is mixed with the solution that concentration is 0.3mol/L, with Y
4Si
3O
12Whisker (is seen patent " a kind of Y
4Si
3O
12The preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in the solution, and ultrasonic radiation 30min, ultrasonic power are 400W, then filter and isolate Y
4Si
3O
12Whisker;
2) with separating obtained Y
4Si
3O
12Whisker and Virahol are pressed Y
4Si
3O
12The ratio of whisker: Virahol=8g:260ml is mixed with suspension, then presses 0.1g/mL adding iodine in suspension, stirs and obtains mixed solution;
Step 4: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y
4Si
3O
12The whisker pinning layer:
1) mixed solution that step 3 is made places the ultrasonic electric deposition apparatus, take step 2 preparation with the internally coated C/C matrix material of porous SiC as negative electrode, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled to be 200W, deposition voltage is 30V, and deposition current is 0.05A, and depositing time is 3min;
2) after deposition finishes, the matrix material of negative electrode is taken off, with distilled water wash 3 times, 80 ℃ of dryings, namely obtaining Y with the internally coated carbon/carbon compound material of porous SiC
4Si
3O
12Whisker embeds the Y of SiC hole
4Si
3O
12The whisker pinning layer;
Step 5: adopt the standby Y of water heat electrophoresis deposition legal system
4Si
3O
12Crystal whisker toughened Y
2SiO
5Compound coating:
1) gets the Y that the 30g granularity is 20 ~ 30 μ m
2SiO
5Powder is suspended in the Virahol of 200ml, and magnetic agitation 10h adds the iodine of 0.06g 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 the water heat electrophoresis deposition reactor, and the control packing ratio is 40%, insulation after being heated to 80 ℃, adjusting deposition voltage is that 150V carries out water heat electrophoresis deposition, stops energising behind the deposition 40min, takes out after the sample cooling, place 60 ℃ baking oven dry, obtain with Y
4Si
3O
12Crystal whisker toughened Y
2SiO
5The C/C matrix material sample of compound coating.
Y as seen from Figure 1
4Si
3O
12Whisker is at SiC undercoat and Y
2SiO
5Directed interspersed between external coating (EC), the compound coating even compact.
Embodiment 2:
The pre-treatment of step 1:C/C matrix material:
1) gets the 2D-carbon/carbon compound material that the aircraft brake sheet is used, be processed into 38 * 38 * 38mm
3Cubes, and to the surface treatment of its chamfering of polishing, chamfering is 35 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 times, clean ultrasonic time is 20min at every turn, and ultrasonic power is 100W, last dry in 55 ℃ electric drying oven with forced convection.
Step 2: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) at first, gets Si powder, C powder and the B that commercially available analytically pure granularity is 20 ~ 30 μ m
2O
3Powder is pressed the Si powder: C powder: B
2O
3Then the mass ratio preparation embedding powder of powder=4:4:0.8 is put into plumbago crucible with pretreated carbon/carbon compound material, and it is imbedded in the embedding powder;
2) secondly, plumbago crucible is put into vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of control vertical vacuum furnace is 15 ℃/min, after furnace temperature risen to 1600 ℃ from room temperature, with the stove naturally cooling, will finish the carbon/carbon compound material ultrasonic cleaning 1h of embedding with dehydrated alcohol behind the insulation 2h, ultrasonic power is 260W;
3) last, drying obtains with the internally coated carbon/carbon compound material of SiC porous in 55 ℃ electric drying oven with forced convection;
Step 3: adopt complexed surfactant to Y
4Si
3O
12Whisker carries out surface modification:
1) sodium lauryl sulphate is mixed with the solution that concentration is 0.4mol/L, with Y
4Si
3O
12Whisker (is seen patent " a kind of Y
4Si
3O
12The preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in the solution, and ultrasonic radiation 40min, ultrasonic power are 500W, then filter and isolate Y
4Si
3O
12Whisker;
2) with 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 presses 0.2g/mL adding iodine in suspension, stirs and obtains mixed solution;
Step 4: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y
4Si
3O
12The whisker pinning layer:
1) mixed solution that step 3 is made places the ultrasonic electric deposition apparatus, take step 2 preparation with the internally coated C/C matrix material of porous SiC as negative electrode, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled to be 260W, deposition voltage is 36V, and deposition current is 0.08A, and depositing time is 5min;
2) after deposition finishes, the matrix material of negative electrode is taken off, with distilled water wash 4 times, 80 ℃ of dryings, namely obtaining Y with the internally coated carbon/carbon compound material of porous SiC
4Si
3O
12Whisker embeds the Y of SiC hole
4Si
3O
12The whisker pinning layer;
Step 5: adopt the standby Y of water heat electrophoresis deposition legal system
4Si
3O
12Crystal whisker toughened Y
2SiO
5Compound coating:
1) gets the Y that the 10g granularity is 20 ~ 30 μ m
2SiO
5Powder is suspended in the Virahol of 100ml, and magnetic agitation 20h adds the iodine of 0.02g 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 the water heat electrophoresis deposition reactor, and the control packing ratio is 45%, insulation after being heated to 100 ℃, adjusting deposition voltage is that 160V carries out water heat electrophoresis deposition, stops energising behind the deposition 45min, takes out after the sample cooling, place 70 ℃ baking oven dry, obtain with Y
4Si
3O
12Crystal whisker toughened Y
2SiO
5The C/C matrix material sample of compound coating.
Embodiment 3:
The pre-treatment of step 1:C/C matrix material:
1) gets the 2D-carbon/carbon compound material that the aircraft brake sheet is used, be processed into 40 * 40 * 40mm
3Cubes, and to the surface treatment of its chamfering of polishing, chamfering is 40 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 5 times, clean ultrasonic time is 30min at every turn, and ultrasonic power is 120W, last dry in 60 ℃ electric drying oven with forced convection.
Step 2: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) at first, gets Si powder, C powder and the B that commercially available analytically pure granularity is 20 ~ 30 μ m
2O
3Powder is pressed the Si powder: C powder: B
2O
3Then the mass ratio preparation embedding powder of powder=5:6:1.0 is put into plumbago crucible with pretreated carbon/carbon compound material, and it is imbedded in the embedding powder;
2) secondly, plumbago crucible is put into vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of control vertical vacuum furnace is 20 ℃/min, after furnace temperature risen to 1550 ℃ from room temperature, with the stove naturally cooling, will finish the carbon/carbon compound material ultrasonic cleaning 1h of embedding with dehydrated alcohol behind the insulation 2.5h, ultrasonic power is 200W;
3) last, drying obtains with the internally coated carbon/carbon compound material of SiC porous in 60 ℃ electric drying oven with forced convection;
Step 3: adopt complexed surfactant to Y
4Si
3O
12Whisker carries out surface modification:
1) sodium lauryl sulphate is mixed with the solution that concentration is 0.5mol/L, with Y
4Si
3O
12Whisker (is seen patent " a kind of Y
4Si
3O
12The preparation method of whisker " (number of patent application: 201210140071.2)) be immersed in the solution, and ultrasonic radiation 50min, ultrasonic power are 600W, then filter and isolate Y
4Si
3O
12Whisker;
2) with 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 presses 0.3g/mL adding iodine in suspension, stirs and obtains mixed solution;
Step 4: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y
4Si
3O
12The whisker pinning layer:
1) mixed solution that step 3 is made places the ultrasonic electric deposition apparatus, take step 2 preparation with the internally coated C/C matrix material of porous SiC as negative electrode, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled to be 300W, deposition voltage is 40V, and deposition current is 0.1A, and depositing time is 7min;
2) after deposition finishes, the matrix material of negative electrode is taken off, with distilled water wash 5 times, 120 ℃ of dryings, namely obtaining Y with the internally coated carbon/carbon compound material of porous SiC
4Si
3O
12Whisker embeds the Y of SiC hole
4Si
3O
12The whisker pinning layer;
Step 5: adopt the standby Y of water heat electrophoresis deposition legal system
4Si
3O
12Crystal whisker toughened Y
2SiO
5Compound coating:
1) gets the Y that the 20g granularity is 20 ~ 30 μ m
2SiO
5Powder is suspended in the Virahol of 300ml, and magnetic agitation 30h adds the iodine of 0.04g 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 the water heat electrophoresis deposition reactor, and the control packing ratio is 50%, insulation after being heated to 120 ℃, adjusting deposition voltage is that 180V carries out water heat electrophoresis deposition, stops energising behind the deposition 50min, takes out after the sample cooling, place 80 ℃ baking oven dry, obtain with Y
4Si
3O
12Crystal whisker toughened Y
2SiO
5The C/C matrix material sample of compound coating.
Claims (4)
1. Y
4Si
3O
12Crystal whisker toughened Y
2SiO
5The preparation method of compound coating is characterized in that:
Step 1: adopt entrapping method to prepare SiC porous undercoat in C/C composite material base surface
1) at first, gets commercially available analytically pure Si powder, C powder and B
2O
3Powder is pressed the Si powder: C powder: B
2O
3Powder=(3 ~ 5): (4 ~ 6): the mass ratio preparation embedding powder of (0.5 ~ 1.0), then pretreated carbon/carbon compound material is put into plumbago crucible, and it is imbedded in the embedding powder;
2) secondly, plumbago crucible is put into vertical vacuum furnace, pass into argon gas as shielding gas, the heat-up rate of control vertical vacuum furnace is 10 ~ 20 ℃/min, after furnace temperature risen to 1500 ~ 1600 ℃ from room temperature, with the stove naturally cooling, will finish the carbon/carbon compound material ultrasonic cleaning 0.5 ~ 1h of embedding with dehydrated alcohol behind insulation 2 ~ 3h, ultrasonic power is 200 ~ 300W;
3) last, drying obtains with the internally coated carbon/carbon compound material of SiC porous in 50 ~ 60 ℃ electric drying oven with forced convection;
Step 2: adopt complexed surfactant to Y
4Si
3O
12Whisker carries out surface modification:
1) sodium lauryl sulphate is mixed with the solution that concentration is 0.3 ~ 0.5mol/L, with Y
4Si
3O
12Whisker is immersed in the solution, and ultrasonic radiation 30 ~ 50min, ultrasonic power are 400 ~ 600W, then filter and isolate Y
4Si
3O
12Whisker;
2) with separating obtained Y
4Si
3O
12Whisker and Virahol are pressed Y
4Si
3O
12Whisker: Virahol=(8 ~ 12g): (150 ~ 300ml) ratio is mixed with suspension, then adds iodine by (0.1 ~ 0.3) g/mL in suspension, stirs and obtains mixed solution;
Step 3: adopt ultrasonic electrophoresis selectivity assembling deposition to obtain Y
4Si
3O
12The whisker pinning layer:
1) mixed solution that step 2 is made places the ultrasonic electric deposition apparatus, take step 1 preparation with the internally coated C/C matrix material of porous SiC as negative electrode, take graphite as anode, carry out galvanic deposit, ultrasonic power is controlled to be 200 ~ 300W, deposition voltage is 30 ~ 40V, and deposition current is 0.05 ~ 0.1A, and depositing time is 3 ~ 7min;
2) after deposition finishes, the matrix material of negative electrode is taken off, with distilled water wash 3 ~ 5 times, 80 ~ 120 ℃ of dryings, namely obtaining Y with the internally coated carbon/carbon compound material of porous SiC
4Si
3O
12Whisker embeds the Y of SiC hole
4Si
3O
12The whisker pinning layer;
Step 4: adopt the standby Y of water heat electrophoresis deposition legal system
4Si
3O
12Crystal whisker toughened Y
2SiO
5Compound coating:
1) gets 10 ~ 30g Y
2SiO
5Powder is suspended in the Virahol of 100 ~ 300ml, and magnetic agitation 10 ~ 30h adds the iodine of 0.02 ~ 0.06g 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 the water heat electrophoresis deposition reactor, and the control packing ratio is 40 ~ 50%, insulation after being heated to 80 ~ 120 ℃, adjusting deposition voltage is that 150 ~ 180V carries out water heat electrophoresis deposition, stops energising behind deposition 40 ~ 50min, takes out after the sample cooling, place 60 ~ 80 ℃ baking oven dry, obtain with Y
4Si
3O
12Crystal whisker toughened Y
2SiO
5The C/C matrix material sample of compound coating.
2. Y according to claim 1
4Si
3O
12Crystal whisker toughened Y
2SiO
5The preparation method of compound coating is characterized in that: described Si powder, C powder and B
2O
3The granularity of powder is 20 ~ 30 μ m.
3. Y according to claim 1
4Si
3O
12Crystal whisker toughened Y
2SiO
5The preparation method of compound coating is characterized in that: the described C/C matrix material pre-treatment following steps of guaranteeing replacement:
1) gets the 2D-carbon/carbon compound material that the aircraft brake sheet is used, be processed into 35 * 35 * 35 ~ 40 * 40 * 40mm
3Cubes, and to the surface treatment of its chamfering of polishing, chamfering is 30 ~ 40 °;
2) then use respectively each ultrasonic cleaning of deionized water and dehydrated alcohol 3 ~ 5 times, clean ultrasonic time is 10 ~ 30min at every turn, and ultrasonic power is 80 ~ 120W, dry in 50 ~ 60 ℃ electric drying oven with forced convection at last.
4. Y according to claim 1
4Si
3O
12Crystal whisker toughened Y
2SiO
5The preparation method of compound coating is characterized in that: described Y
2SiO
5The granularity of powder is 20 ~ 30 μ m.
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