CN114163251A - Nano fiber toughened silicon carbide surface environment barrier ceramic coating and preparation method thereof - Google Patents
Nano fiber toughened silicon carbide surface environment barrier ceramic coating and preparation method thereof Download PDFInfo
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- CN114163251A CN114163251A CN202111520315.5A CN202111520315A CN114163251A CN 114163251 A CN114163251 A CN 114163251A CN 202111520315 A CN202111520315 A CN 202111520315A CN 114163251 A CN114163251 A CN 114163251A
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 91
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 54
- 230000004888 barrier function Effects 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 238000005524 ceramic coating Methods 0.000 title claims abstract description 38
- 238000000576 coating method Methods 0.000 claims abstract description 48
- 239000011248 coating agent Substances 0.000 claims abstract description 47
- 230000007613 environmental effect Effects 0.000 claims abstract description 37
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 63
- 239000002243 precursor Substances 0.000 claims description 56
- 229910002651 NO3 Inorganic materials 0.000 claims description 45
- 238000010438 heat treatment Methods 0.000 claims description 45
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 38
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 33
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 31
- 239000004202 carbamide Substances 0.000 claims description 31
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 26
- 238000010041 electrostatic spinning Methods 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 25
- 238000009841 combustion method Methods 0.000 claims description 17
- 238000005507 spraying Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000007750 plasma spraying Methods 0.000 claims description 13
- 238000000498 ball milling Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 8
- 229910052735 hafnium Inorganic materials 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 229910052765 Lutetium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- -1 rare earth nitrate Chemical class 0.000 claims description 2
- 238000003980 solgel method Methods 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 30
- 230000003647 oxidation Effects 0.000 abstract description 12
- 238000007254 oxidation reaction Methods 0.000 abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 abstract description 10
- 239000001301 oxygen Substances 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 9
- INIGCWGJTZDVRY-UHFFFAOYSA-N hafnium zirconium Chemical compound [Zr].[Hf] INIGCWGJTZDVRY-UHFFFAOYSA-N 0.000 abstract description 7
- 230000035876 healing Effects 0.000 abstract description 6
- 150000002910 rare earth metals Chemical class 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 150000003839 salts Chemical class 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract description 4
- KQHQLIAOAVMAOW-UHFFFAOYSA-N hafnium(4+) oxygen(2-) zirconium(4+) Chemical compound [O--].[O--].[O--].[O--].[Zr+4].[Hf+4] KQHQLIAOAVMAOW-UHFFFAOYSA-N 0.000 abstract description 3
- 229910003465 moissanite Inorganic materials 0.000 abstract description 3
- 239000006104 solid solution Substances 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 105
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 105
- 239000000243 solution Substances 0.000 description 95
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 20
- 238000002485 combustion reaction Methods 0.000 description 18
- 238000003756 stirring Methods 0.000 description 17
- 230000002378 acidificating effect Effects 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 12
- 238000002425 crystallisation Methods 0.000 description 12
- 239000002244 precipitate Substances 0.000 description 10
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 229910002609 Gd2Zr2O7 Inorganic materials 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 230000035699 permeability Effects 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- FLVFLHZPYDNHJE-UHFFFAOYSA-N chloro hypochlorite;hafnium Chemical compound [Hf].ClOCl FLVFLHZPYDNHJE-UHFFFAOYSA-N 0.000 description 3
- PDPJQWYGJJBYLF-UHFFFAOYSA-J hafnium tetrachloride Chemical compound Cl[Hf](Cl)(Cl)Cl PDPJQWYGJJBYLF-UHFFFAOYSA-J 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 229910007266 Si2O Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- WWFZRAYTGNKUQC-UHFFFAOYSA-H [Al+3].[Y+3].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O Chemical compound [Al+3].[Y+3].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O WWFZRAYTGNKUQC-UHFFFAOYSA-H 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- TZNXTUDMYCRCAP-UHFFFAOYSA-N hafnium(4+);tetranitrate Chemical compound [Hf+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O TZNXTUDMYCRCAP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- APRNQTOXCXOSHO-UHFFFAOYSA-N lutetium(3+);trinitrate Chemical compound [Lu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O APRNQTOXCXOSHO-UHFFFAOYSA-N 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a nano-fiber toughened silicon carbide surface environmental barrier ceramic coating and a preparation method thereof, belonging to the field of coating preparation.YAG is introduced to improve the thermal adaptability of rare earth zirconium (hafnium) acid salt and a matrix, and the coating can play a part of the function of microcrack healing in a long-time high-temperature thermal protection stage compared with a low-melting point coating; meanwhile, the oxidation product of SiC, zirconium hafnium oxide and YAG components form a high-temperature solid solution, so that cracks can be effectively healed, and oxygen permeation is prevented; in addition, the YAG nano-fiber is introduced and the composite coating containing the YAG coating has good chemical compatibility, so that a compact coating can be formed, the toughness of the composite coating is improved, and the high-temperature stability of the nano-fiber toughened composite coating is improved. The coating can play a role in effectively resisting oxygen and insulating heat, and the service life of SiC and the composite material is prolonged.
Description
Technical Field
The invention belongs to the field of coating preparation, and relates to a nanofiber-toughened silicon carbide surface environmental barrier ceramic coating and a preparation method thereof.
Background
The SiC has excellent high-temperature stability and good mechanical property, is often used as an ultra-high temperature structure composite material, and can be applied to the thermal protection field of C/C composite materials. With the increasing deterioration of the service environment of hot end structural components, the development of a thermal barrier/environmental barrier coating system, the improvement of the service temperature and the service life of the thermal barrier/environmental barrier coating system become the key points of the future application of the SiC-based composite material. Rare (zirconium) hafnium-based composite oxide (A)2B2O7A ═ rare earth element, B ═ zr (hf)) has excellent properties such as high melting point, low thermal conductivity, and low oxygen permeability, and is widely used in the field of environmental heat barriers. The low expansion, low oxygen permeability and good high-temperature stability of YAG also have good prospect in the field of high-temperature thermal protection.
The document "SiC/SiC-YAG-SZ oxidation protective coatings for carbon/carbon composites. Yi Zeng, Xiang Xiong, Shun Guo, Wuzhuang Zhang. Corroson Science,2013,70: 68-73" mentions the oxidation of SiC in a high temperature environment and the reaction of YAG-SZ in the compositionBecome Y2Si2O、Y2SiO5, etc. which play the role of healing cracks and pinning to improve the thermal protection life of the coating, but the continuous erosion protection function of the outer coating is reduced under the long-term high-temperature oxidation. Document "Microstructure and thermal shock Performance of Y2Hf2O7coating deposited on SiC coated C/C composite, Shengyue Gu, Shouyang Zhang, Fei, Liu, Guingying Liang, Wei Li applied Surface science 2018,455:849-855. "indicates that the oxide coating with good microstructure can be prepared on the Surface of the SiC coating by supersonic plasma spraying, the preparation of the oxide coating improves the service life of SiC and composite materials, but the oxygen-resistant and heat-insulating effects of the coating are reduced because cracks appear on the Surface of the coating after long-time thermal protection, the SiC layer is oxidized, and then the failure of the composite materials is initiated.
In summary, SiC surface oxide coatings still suffer from insufficient thermal adaptation and coating healing capabilities. The development of a multifunctional coating system is a problem in the application of the expanded SiC-based composite material in an extreme environment.
Disclosure of Invention
The invention aims to overcome the defect that the SiC surface oxide coating in the prior art has insufficient healing capacity, and provides a nanofiber toughened silicon carbide surface environmental barrier ceramic coating and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the nano-fiber toughened silicon carbide surface environmental barrier ceramic coating is YAG-A2B2O7；
A is trivalent rare earth element, B is Zr or Hf;
the nano-fiber is YAG nano-fiber;
the silicon carbide is a SiC coating or a matrix.
Preferably, the nanofiber-toughened silicon carbide surface environmental barrier ceramic coating comprises, by mass, 0.5-10 parts of YAG nanofibers and 50-89.5 parts of A2B2O7And 10-40 parts of YAG powder.
Preferably, the trivalent rare earth element is any one of Y, La, Gd, Sm and Lu.
A preparation method of the nanofiber toughened silicon carbide surface environmental barrier ceramic coating comprises the following steps:
step 1) preparing YAG nano fibers by combining a sol-gel method with electrostatic spinning;
step 2) preparing YAG powder by a solution combustion method:
mixing aluminum nitrate, nitrate of A, urea and deionized water, and obtaining well-crystallized YAG powder by a solution combustion method and a heat treatment process;
step 3) solution combustion method for preparing A2B2O7Powder:
mixing the nitrate of A, the nitrate of B, urea and deionized water, and obtaining the nitrate A by a solution combustion method and a heat treatment process2B2O7Powder;
step 4) mixing YAG powder and A2B2O7Uniformly mixing the powder and YAG nano-fiber, granulating to obtain powder for spraying, and spraying the powder for spraying on the surface of silicon carbide to obtain a nano-fiber toughened silicon carbide surface environmental barrier ceramic coating;
a is trivalent rare earth element, B is Zr or Hf.
Preferably, the specific operation of step 1) is:
mixing the nitrate of the A, aluminum nitrate and deionized water to prepare a first precursor solution;
adding deionized water and polyvinyl alcohol into the first precursor solution to prepare an electrostatic spinning precursor solution;
and (3) carrying out electrostatic spinning and heat treatment on the electrostatic spinning precursor solution to obtain the YAG nano-fiber.
Preferably, in the step 2), the molar ratio of the trivalent rare earth element to the Al element is 3:5, the molar weight of the urea is 1.2-2.0 times of the total molar weight of the aluminum nitrate and the rare earth nitrate;
in the step 3), the molar ratio of the elements A to B is 1:1, the molar quantity of the urea is 1.2-2.0 times of the total molar quantity of the nitrate of A and the nitrate of B;
in the step 4), the YAG powder and A are counted by mass portion2B2O7The mixing amount of the powder and the YAG nano-fiber is as follows: 0.5 to 10 parts of YAG nano fiber and 50 to 89.5 parts of A2B2O7Powder and 10-40 parts of YAG powder.
Preferably, in step 2) and step 3),
the mixing conditions were: heating for 0.5-2h at the temperature of 40-80 ℃;
the reaction conditions of the solution combustion method are as follows: the temperature is 250-800 ℃, and the time is 0.3-2 h;
the reaction conditions of the heat treatment process are as follows: the temperature is 1000-1200 ℃, and the time is 1-2 h.
Preferably, in step 4), the granulation process includes drying and then ball milling, and the drying conditions are as follows: the temperature is 120 ℃, and the time is 2-4 h; and (4) sieving after ball milling, and taking powder in a 180-300-mesh sieve.
Preferably, in the first precursor solution, the molar ratio of the nitrate of a to the aluminum nitrate is 3:5, the mass ratio of the total nitrate to the deionized water is (10-60): 100, respectively;
in the electrostatic spinning precursor solution, the mass fraction of polyvinyl alcohol is 4-15%;
the reaction conditions when preparing the first precursor solution are as follows: the temperature is 6-100 ℃, and the time is 2-4 h;
the reaction conditions for preparing the electrostatic spinning precursor solution are as follows: the temperature is 80-100 ℃, and the time is 2-4 h;
the conditions of the heat treatment process are as follows: the temperature is 800-1200 ℃, and the time is 2-8 h.
Preferably, the spraying adopts a supersonic plasma spraying method;
the technological parameters of the supersonic plasma spraying are as follows: the power is 25-60 KW, the Ar flow is 32-68L/min, the powder feeding amount is 6-40 g/min, and the spraying distance is 70-110 mm.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a nano-fiber toughened silicon carbide surface environmental barrier ceramic coating, wherein rare earth zirconium (hafnium) acid salt has low thermal conductivity and low oxygen permeability, and has excellent high-temperature stability; YAG also has excellent thermophysical properties and is a candidate for an environmental barrier coating; the YAG is introduced to improve the thermal adaptability of the rare earth zirconium (hafnium) acid salt and the matrix, and compared with a low-melting point rare earth zirconium (hafnium) acid salt, the high-melting point yttrium aluminum phosphate can play a part of microcrack healing role in a long-time high-temperature thermal protection stage; meanwhile, the oxidation product of SiC, zirconium hafnium oxide and YAG components form a high-temperature solid solution, so that cracks can be effectively healed, and oxygen permeation is prevented; in addition, the YAG nano-fiber is introduced and the composite coating containing the YAG coating has good chemical compatibility, so that a compact coating can be formed, the toughness of the composite coating is improved, and the high-temperature stability of the nano-fiber toughened composite coating is improved. The coating can play a role in effectively resisting oxygen and insulating heat, and the service life of SiC and the composite material is prolonged.
According to the preparation method of the nanofiber toughened silicon carbide surface environment barrier ceramic coating provided by the invention, the YAG nanofibers with controllable morphology are obtained by adopting an electrostatic spinning method, the composite oxide powder with good composition is obtained by adopting a combustion method, the mixed materials are screened and granulated to avoid transition waste of the materials, and the nanofiber toughened ceramic composite coating with good microstructure is prepared by adopting a plasma spraying method.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention;
FIG. 2 is an XRD pattern of YAG nanofibers prepared in example 1;
FIG. 3 is an EDS diagram of the YAG precursor prepared in example 1;
FIG. 4 shows YAG nanofiber toughened YAG-Y prepared in example 12Zr2O7Surface topography map of the coating.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
example 1
The preparation process of the nanofiber toughened silicon carbide surface environmental barrier ceramic coating is shown in fig. 1:
1) yttrium nitrate and aluminum nitrate are used as YAG precursors, the yttrium nitrate and the aluminum nitrate are prepared into precursor solution according to the molar ratio of Y to Al being 3:5, and a proper amount of deionized water and polyvinyl alcohol (PVA) are added into the precursor solution to prepare electrostatic spinning precursor solution with 10% of PVA mass fraction;
2) and (3) preparing the electrostatic spinning fiber from the precursor solution under the conditions of voltage of 25kv, curing distance of 10cm, certain humidity and rotating speed. And carrying out heat treatment at 1200 ℃ for 2h to obtain the YAG nano fiber with good crystallization.
YAG and Y prepared by combustion method2Zr2O7The method comprises the following specific steps:
1)Y2Zr2O7preparing a precursor: dissolving zirconium nitrate in deionized water, then adding yttrium nitrate and urea into the solution, heating and stirring the solution until the solution is clear, adjusting the pH value of the solution to be acidic 3, and adding nitrate into the solution according to the molar ratio of Y to Zr of 1:1, carrying out ingredient calculation, and introducing urea which is a combustion agent according to 1.4 times of the mol of the required nitrate;
YAG precursor preparation: dissolving aluminum nitrate in deionized water, then adding yttrium nitrate and urea into the solution, heating and stirring the solution until the solution is clear, adjusting the pH value of the solution to be acidic 3, and adding nitrate according to the molar ratio of Y to Al of 3:5, the proportion calculation is carried out, and the urea is introduced into the combustion agent according to 1.4 times of the mol of the required nitrate.
2) Combustion reaction and heat treatment: placing the prepared solution in a muffle furnace preheated to 500 ℃ for reaction to obtain a fluffy product, and then carrying out heat treatment on the obtained substance in a high-temperature oxidation furnace at 1200 ℃ for 2h to respectively obtain YAG and Y with good crystallization2Zr2O7Ceramic powder.
1) YAG nano fiber in 3 wt%, YAG powder in 20 wt%, Y2Zr2O7According to the mass fraction of 77 wt.%, carrying out planetary ball millingMixing in the machine for 4 hr, taking out, and drying.
2) Preparing 3-7% of PVA solution, taking a proper amount of the PVA solution, a certain amount of nano-fiber and mixed powder, mixing and granulating, drying in an oven, ball-milling again, sieving with a 180-300-mesh sieve, and taking out the powder for later use.
3) Preparing YAG nanofiber toughened YAG-Y on the surface of the SiC substrate by adopting a supersonic plasma method2Zr2O7An environmental barrier ceramic coating.
The technological parameters of the supersonic plasma spraying method are as follows: the power is 35KW, the Ar flow is 50L/min, the powder feeding amount is 14g/min, and the spraying distance is 100 mm.
The prepared YAG nano-fiber toughens YAG-Y2Zr2O7The composite coating has less surface microcrack and better thermophysical compatibility.
Example 2
1) yttrium nitrate and aluminum nitrate are used as YAG precursors, and the ratio of yttrium nitrate to aluminum nitrate is as follows: al is 3:5, preparing a precursor solution, and adding a proper amount of deionized water and polyvinyl alcohol (PVA) to the precursor solution to prepare an electrostatic spinning precursor solution with the PVA mass fraction of 10%;
2) and (3) preparing the electrostatic spinning fiber from the precursor solution under the conditions of voltage of 25kv, curing distance of 12cm, certain humidity and rotating speed. And carrying out heat treatment at 1200 ℃ for 2h to obtain the YAG nano fiber with good crystallization.
YAG and Lu prepared by combustion method2Zr2O7The method comprises the following specific steps:
1)Lu2Zr2O7preparing a precursor: dissolving zirconium nitrate in deionized water, then adding lutetium nitrate and urea into the solution, heating and stirring the solution until the solution is clear, adjusting the pH value of the solution to be acidic 3, and adding nitrate into the solution according to the molar ratio of Lu to Zr of 1:1, carrying out ingredient calculation, and introducing urea which is a combustion agent according to 1.4 times of the mol of the required nitrate;
YAG precursor preparation: dissolving aluminum nitrate in deionized water, then adding yttrium nitrate and urea into the solution, heating and stirring the solution until the solution is clear, adjusting the pH value of the solution to be acidic 3, and adding nitrate according to the molar ratio of Y to Al of 3:5, the proportion calculation is carried out, and the urea is introduced into the combustion agent according to 1.4 times of the mol of the required nitrate.
2) Combustion reaction and heat treatment: placing the prepared solution in a muffle furnace preheated to 500 ℃ for reaction to obtain a fluffy product, and then carrying out heat treatment on the obtained substance in a high-temperature oxidation furnace at 1200 ℃ for 2h to respectively obtain YAG and Lu with good crystallization2Zr2O7Ceramic powder.
1) YAG nano fiber 8 wt%, YAG powder 26 wt%, Lu powder2Zr2O7And (3) fully mixing the components in 66 wt.% by mass in a planetary ball mill for 4 hours, and taking out and drying the mixture for later use.
2) Preparing 3-7% of PVA solution, taking a proper amount of the PVA solution, a certain amount of nano-fiber and mixed powder, mixing and granulating, drying in an oven, ball-milling again, sieving with a 180-300-mesh sieve, and taking out the powder for later use.
3) Preparing YAG nano-fiber toughened YAG-Lu on the surface of the SiC substrate by adopting a supersonic plasma method2Zr2O7An environmental barrier ceramic coating.
The technological parameters of the supersonic plasma spraying method are as follows: the power is 40KW, the Ar flow is 55L/min, the powder feeding amount is 26g/min, and the spraying distance is 100 mm.
The prepared YAG nano-fiber is toughened YAG-Lu2Zr2O7The composite coating has less surface microcrack and better thermophysical compatibility.
Example 3
1) yttrium nitrate and aluminum nitrate are used as YAG precursors, a precursor solution is prepared by the yttrium nitrate and the aluminum nitrate according to the molar ratio of Y to Al being 3:5, and a proper amount of deionized water and polyvinyl alcohol (PVA) are added to prepare an electrostatic spinning precursor solution;
2) and (3) preparing the electrostatic spinning fiber from the precursor solution under the conditions of voltage of 25kv, curing distance of 12cm, certain humidity and rotating speed. And carrying out heat treatment at 1200 ℃ for 2h to obtain the YAG nano fiber with good crystallization.
YAG and La prepared by combustion method2Hf2O7The method comprises the following specific steps:
1)La2Hf2O7preparing a precursor: hafnium tetrachloride (HfCl)4) Dissolving the precipitate in deionized water, adding excessive ammonia water, fully stirring to obtain white flocculent precipitate, centrifuging and repeatedly washing to obtain precipitate without chloride ions, then placing a beaker containing the white precipitate in a magnetic stirring water bath kettle, adding excessive nitric acid, heating and stirring until the beaker presents a transparent liquid, then adding lanthanum nitrate and urea into the solution, heating and stirring until the solution is clear, adjusting the pH value of the solution to be acidic 1, and adding the nitrate according to the molar ratio of La to Hf of 1:1, carrying out ingredient calculation, and introducing urea which is a combustion agent according to 1.4 times of the mol of the required nitrate;
YAG precursor preparation: dissolving aluminum nitrate in deionized water, then adding yttrium nitrate and urea into the solution, heating and stirring the solution until the solution is clear, adjusting the pH value of the solution to be acidic 3, and adding nitrate according to the molar ratio of Y to Al of 3:5, the proportion calculation is carried out, and the urea is introduced into the combustion agent according to 1.4 times of the mol of the required nitrate.
2) Combustion reaction and heat treatment: placing the prepared solution in a muffle furnace preheated to 500 ℃ for reaction to obtain a fluffy product, and then carrying out heat treatment on the obtained substance in a high-temperature oxidation furnace at 1200 ℃ for 2h to respectively obtain YAG and La with good crystallization2Hf2O7Ceramic powder.
1) YAG nano fiber 10 wt% and YAG powder 3 wt%5wt.％，La2Hf2O7And fully mixing the components for 4 hours in a planetary ball mill according to the mass fraction of 55 wt%, taking out and drying for later use.
2) Preparing 3-7% of PVA solution, taking a proper amount of the PVA solution, a certain amount of nano-fiber and mixed powder, mixing and granulating, drying in an oven, ball-milling again, sieving with a 180-300-mesh sieve, and taking out the powder for later use.
3) Preparing YAG nano-fiber toughened YAG-La on the surface of the SiC substrate by adopting a supersonic plasma method2Hf2O7An environmental barrier ceramic coating.
The technological parameters of the supersonic plasma spraying method are as follows: the power is 45KW, the Ar flow is 50L/min, the powder feeding amount is 30g/min, and the spraying distance is 100 mm.
The prepared YAG nano-fiber toughening YAG-La2Hf2O7The composite coating has less surface microcrack and better thermophysical compatibility.
Example 4
1) yttrium nitrate and aluminum nitrate are used as YAG precursors, and the ratio of yttrium nitrate to aluminum nitrate is as follows: preparing a precursor solution with Al of 3:5, and adding a proper amount of deionized water and polyvinyl alcohol (PVA) to prepare an electrostatic spinning precursor solution with the PVA mass fraction of 12%;
2) and (3) preparing the electrostatic spinning fiber from the precursor solution under the conditions of voltage of 25kv, curing distance of 12cm, certain humidity and rotating speed. And carrying out heat treatment at 1200 ℃ for 2h to obtain the YAG nano fiber with good crystallization.
YAG and Y prepared by combustion method2Zr2O7The method comprises the following specific steps:
1)Y2Zr2O7preparing a precursor: dissolving zirconium nitrate in deionized water, adding yttrium nitrate and urea into the solution, heating while stirring until the solution is clear, adjusting the pH value of the solution to be acidic 1, and carrying out batching on the nitrate according to the molar ratio of Y to Zr of 1:1Calculating that urea is introduced by 2 times of the mol of nitrate required by a combustion agent;
YAG precursor preparation: dissolving aluminum nitrate in deionized water, then adding yttrium nitrate and urea into the solution, heating and stirring the solution until the solution is clear, adjusting the pH value of the solution to be acidic 3, carrying out batching calculation on nitrate according to the molar ratio of Y to Al of 3:5, and introducing the urea which is a combustion agent according to 2 times of the mole of the required nitrate.
2) Combustion reaction and heat treatment: placing the prepared solution in a muffle furnace preheated to 500 ℃ for reaction to obtain a fluffy product, and then carrying out heat treatment on the obtained substance in a high-temperature oxidation furnace at 1200 ℃ for 2h to respectively obtain YAG and Y with good crystallization2Zr2O7Ceramic powder.
1) YAG nano fiber in 4 wt%, YAG powder in 38 wt%, Y2Zr2O7And (3) fully mixing the components for 4 hours in a planetary ball mill according to the mass fraction of 68 wt%, taking out and drying for later use.
2) Preparing 3-7% of PVA solution, taking a proper amount of the PVA solution, a certain amount of nano-fiber and mixed powder, mixing and granulating, drying in an oven, ball-milling again, sieving with a 180-300-mesh sieve, and taking out the powder for later use.
3) Preparing YAG nanofiber toughened YAG-Y on the surface of the SiC substrate by adopting a supersonic plasma method2Zr2O7An environmental barrier ceramic coating.
The technological parameters of the supersonic plasma spraying method are as follows: the power is 55KW, the Ar flow is 60L/min, the powder feeding amount is 40g/min, and the spraying distance is 100 mm.
The prepared YAG nano-fiber toughens YAG-Y2Zr2O7The composite coating has less surface microcrack and better thermophysical compatibility.
Example 5
1) yttrium nitrate and aluminum nitrate are adopted as YAG precursors, the yttrium nitrate and the aluminum nitrate are prepared into precursor solution according to the molar ratio of Y to Al being 3:5, and a proper amount of deionized water and polyvinyl alcohol are added to prepare electrostatic spinning precursor solution with the mass fraction of polyvinyl alcohol (PVA) being 8%;
2) and (3) preparing the electrostatic spinning fiber from the precursor solution under the conditions of voltage of 25kv, curing distance of 12cm, certain humidity and rotating speed. And carrying out heat treatment at 1200 ℃ for 2h to obtain the YAG nano fiber with good crystallization.
YAG and Gd prepared by combustion method2Zr2O7The method comprises the following specific steps:
1)Gd2Zr2O7preparing a precursor: dissolving zirconium nitrate in deionized water, then adding gadolinium nitrate and urea into the solution, heating and stirring the solution until the solution is clear, adjusting the pH value of the solution to be acidic 3, carrying out batching calculation on nitrate according to the molar ratio of Gd to Zr being 1:1, and introducing the urea as a combustion agent according to 1.6 times of the mole of the required nitrate;
YAG precursor preparation: dissolving aluminum nitrate in deionized water, then adding yttrium nitrate and urea into the solution, heating and stirring the solution until the solution is clear, adjusting the pH value of the solution to be acidic 3, carrying out batching calculation on nitrate according to the molar ratio of Y to Al of 3:5, and introducing the urea as a combustion agent according to 1.6 times of the mole of the required nitrate.
2) Combustion reaction and heat treatment: placing the prepared solution in a muffle furnace preheated to 450 ℃ for reaction to obtain a fluffy product, and then carrying out heat treatment on the obtained substance in a high-temperature oxidation furnace at 1200 ℃ for 2h to respectively obtain YAG and Gd with good crystallization2Zr2O7Ceramic powder.
1) YAG nano fiber in 7 wt%, YAG powder in 30 wt%, Gd2Zr2O7And (3) fully mixing the components in percentage by mass of 63 wt.% in a planetary ball mill for 4 hours, and taking out and drying the mixture for later use.
2) Preparing 3-7% of PVA solution, taking a proper amount of the PVA solution, a certain amount of nano-fiber and mixed powder, mixing and granulating, drying in an oven, ball-milling again, sieving with a 180-300-mesh sieve, and taking out the powder for later use.
3) Preparing YAG nano-fiber toughened YAG-Gd on the surface of the SiC substrate by adopting a supersonic plasma method2Zr2O7An environmental barrier ceramic coating.
The technological parameters of the supersonic plasma spraying method are as follows: the power is 50KW, the Ar flow is 60L/min, the powder feeding amount is 35g/min, and the spraying distance is 100 mm.
The prepared YAG nano-fiber toughens YAG-Gd2Zr2O7The composite coating has less surface microcrack and better thermophysical compatibility.
Example 6
1) yttrium nitrate and aluminum nitrate are adopted as YAG precursors, the yttrium nitrate and the aluminum nitrate are prepared into precursor solution according to the molar ratio of Y to Al being 3:5, and a proper amount of deionized water and polyvinyl alcohol are added to prepare electrostatic spinning precursor solution with the mass fraction of polyvinyl alcohol (PVA) being 8%;
2) and (3) preparing the electrostatic spinning fiber from the precursor solution under the conditions of voltage of 25kv, curing distance of 12cm, certain humidity and rotating speed. And carrying out heat treatment at 1200 ℃ for 2h to obtain the YAG nano fiber with good crystallization.
YAG and Sm prepared by combustion method2Hf2O7The method comprises the following specific steps:
1)Sm2Hf2O7preparing a precursor: hafnium oxychloride (HfOCl)2) Dissolving in deionized water, adding excessive ammonia water, stirring to obtain white flocculent precipitate, centrifuging, washing repeatedly to obtain precipitate without chloride ion, placing beaker containing white precipitate in magnetic stirring water bath, adding excessive nitric acid, heating while stirring until the beaker is transparent liquid, adjusting pH to acidic 1, adding nitrate according to the formulaSm and Hf are calculated according to the molar ratio of 1:1, and urea is introduced as a combustion agent according to 1.6 times of the mol of required nitrate;
YAG precursor preparation: dissolving aluminum nitrate in deionized water, then adding yttrium nitrate and urea into the solution, heating and stirring the solution until the solution is clear, adjusting the pH value of the solution to be acidic 3, carrying out batching calculation on nitrate according to the molar ratio of Y to Al of 3:5, and introducing the urea as a combustion agent according to 1.8 times of the mole of the required nitrate.
2) Combustion reaction and heat treatment: placing the prepared solution in a muffle furnace preheated to 450 ℃ for reaction to obtain a fluffy product, and then carrying out heat treatment on the obtained substance in a high-temperature oxidation furnace at 1200 ℃ for 2h to respectively obtain YAG (yttrium aluminum garnet), Sm (yttrium aluminum garnet) with good crystallization2Hf2O7Ceramic powder.
1) YAG nano fiber 9 wt%, YAG powder 35 wt%, Sm2Hf2O7And (3) fully mixing the components for 4 hours in a planetary ball mill according to the mass fraction of 56 wt%, taking out and drying for later use.
2) Preparing 3-7% of PVA solution, taking a proper amount of the PVA solution, a certain amount of nano-fiber and mixed powder, mixing and granulating, drying in an oven, ball-milling again, sieving with a 180-300-mesh sieve, and taking out the powder for later use.
3) Preparing YAG nano-fiber toughened YAG-Sm on the surface of the SiC substrate by adopting a supersonic plasma method2Hf2O7An environmental barrier ceramic coating.
The technological parameters of the supersonic plasma spraying method are as follows: the power is 55KW, the Ar flow is 60L/min, the powder feeding amount is 30g/min, and the spraying distance is 100 mm.
The prepared YAG nano fiber toughening YAG-Sm2Hf2O7The composite coating has less surface microcrack and better thermophysical compatibility.
The YAG nanofibers prepared in example 1 were characterized by an XRD pattern as shown in FIG. 2, from which it can be seen that: the prepared material has good X-ray diffraction information and good crystal characteristics.
The EDS results of the YAG precursor are shown in fig. 3, and it can be seen that: the prepared powder element proportion is compounded with the YAG element proportion.
YAG-Y2Zr2O7The SEM results of the coating are shown in fig. 4, which shows that: the prepared composite coating has compact surface, no obvious cracks and good microstructure characteristics.
The nitrate of zirconium is analytically pure zirconium nitrate; the nitrate of hafnium is analytically pure hafnium tetrachloride or hafnium oxychloride (HfOCl)2) Nitric acid and deionized water; the preparation operation of the hafnium nitrate in the step 2) comprises the following steps: dissolving hafnium tetrachloride or hafnium oxychloride in deionized water, adding excessive ammonia water, stirring thoroughly to obtain white flocculent precipitate, centrifuging, washing repeatedly to obtain white precipitate, placing beaker containing white precipitate in magnetic stirring water bath, adding nitric acid, heating while stirring until the beaker is transparent liquid, heating at 40-80 deg.C for 0.5-2 hr, and centrifuging (10000r, 5 min).
In conclusion, the invention provides a nanofiber toughened silicon carbide surface environmental barrier ceramic coating and a preparation method thereof. YAG nano-fiber is used as a reinforcing phase, YAG and rare earth zirconium (hafnium) composite oxide (A2Zr (Hf)2O7) is used as a spraying raw material, and a supersonic plasma spraying method is adopted to prepare the nano-fiber toughened ceramic composite coating with a good microstructure. The main benefits are: the low thermal conductivity of rare earth zirconium (hafnium) acid salt and the low expansion and low oxygen permeability of YAG improve the thermal adaptability of the composite coating and the matrix; the low-melting-point YAG component can play a role in healing microcracks in a high-temperature thermal protection stage; meanwhile, the oxidation product of SiC, zirconium hafnium oxide and YAG components form a solid solution, so that cracks can be effectively healed, and oxygen can be prevented from permeating; in addition, the introduction of the nano-fiber has good chemical compatibility with the composite coating, and the toughness of the coating is enhanced, so that the high-temperature stability of the nano-fiber toughened composite coating is improved.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. The nanofiber-toughened silicon carbide surface environmental barrier ceramic coating is characterized in that the nanofiber-toughened silicon carbide surface environmental barrier ceramic coating is YAG-A2B2O7；
A is trivalent rare earth element, B is Zr or Hf;
the nano-fiber is YAG nano-fiber;
the silicon carbide is a SiC coating or a matrix.
2. The nanofiber-toughened silicon carbide surface environment barrier ceramic coating as claimed in claim 1, wherein the nanofiber-toughened silicon carbide surface environment barrier ceramic coating comprises, by mass, 0.5-10 parts of YAG nanofibers and 50-89.5 parts of A2B2O7And 10-40 parts of YAG powder.
3. The nanofiber toughened silicon carbide surface environmental barrier ceramic coating according to claim 1, wherein the trivalent rare earth element is any one of Y, La, Gd, Sm and Lu.
4. A preparation method of the nanofiber toughened silicon carbide surface environmental barrier ceramic coating according to any one of claims 1 to 3, characterized by comprising the following steps:
step 1) preparing YAG nano fibers by combining a sol-gel method with electrostatic spinning;
step 2) preparing YAG powder by a solution combustion method:
mixing aluminum nitrate, nitrate of A, urea and deionized water, and obtaining well-crystallized YAG powder by a solution combustion method and a heat treatment process;
step 3) solution combustion method for preparing A2B2O7Powder:
mixing the nitrate of A and the nitrate of BMixing urea and deionized water, and performing solution combustion method and heat treatment process to obtain A2B2O7Powder;
step 4) mixing YAG powder and A2B2O7Uniformly mixing the powder and YAG nano-fiber, granulating to obtain powder for spraying, and spraying the powder for spraying on the surface of silicon carbide to obtain a nano-fiber toughened silicon carbide surface environmental barrier ceramic coating;
a is trivalent rare earth element, B is Zr or Hf.
5. The preparation method of the nanofiber toughened silicon carbide surface environmental barrier ceramic coating according to claim 4, wherein the specific operation of the step 1) is as follows:
mixing the nitrate of the A, aluminum nitrate and deionized water to prepare a first precursor solution;
adding deionized water and polyvinyl alcohol into the first precursor solution to prepare an electrostatic spinning precursor solution;
and (3) carrying out electrostatic spinning and heat treatment on the electrostatic spinning precursor solution to obtain the YAG nano-fiber.
6. The method for preparing the nanofiber toughened silicon carbide surface environmental barrier ceramic coating according to claim 4,
in the step 2), the molar ratio of the trivalent rare earth element to the Al element is 3:5, the molar weight of the urea is 1.2-2.0 times of the total molar weight of the aluminum nitrate and the rare earth nitrate;
in the step 3), the molar ratio of the elements A to B is 1:1, the molar quantity of the urea is 1.2-2.0 times of the total molar quantity of the nitrate of A and the nitrate of B;
in the step 4), the YAG powder and A are counted by mass portion2B2O7The mixing amount of the powder and the YAG nano-fiber is as follows: 0.5 to 10 parts of YAG nano fiber and 50 to 89.5 parts of A2B2O7Powder and 10-40 parts of YAG powder.
7. The method for preparing the nanofiber toughened silicon carbide surface environmental barrier ceramic coating according to claim 4, wherein in the step 2) and the step 3),
the mixing conditions were: heating for 0.5-2h at the temperature of 40-80 ℃;
the reaction conditions of the solution combustion method are as follows: the temperature is 250-800 ℃, and the time is 0.3-2 h;
the reaction conditions of the heat treatment process are as follows: the temperature is 1000-1200 ℃, and the time is 1-2 h.
8. The method for preparing the nanofiber toughened silicon carbide surface environmental barrier ceramic coating according to claim 4, wherein in the step 4), the granulation process comprises drying and then ball milling, and the drying conditions are as follows: the temperature is 120 ℃, and the time is 2-4 h; and (4) sieving after ball milling, and taking powder in a 180-300-mesh sieve.
9. The method for preparing the nanofiber toughened silicon carbide surface environmental barrier ceramic coating according to claim 5,
in the first precursor solution, the molar ratio of the nitrate of A to the aluminum nitrate is 3:5, the mass ratio of the total nitrate to the deionized water is (10-60): 100, respectively;
in the electrostatic spinning precursor solution, the mass fraction of polyvinyl alcohol is 4-15%;
the reaction conditions when preparing the first precursor solution are as follows: the temperature is 6-100 ℃, and the time is 2-4 h;
the reaction conditions for preparing the electrostatic spinning precursor solution are as follows: the temperature is 80-100 ℃, and the time is 2-4 h;
the conditions of the heat treatment process are as follows: the temperature is 800-1200 ℃, and the time is 2-8 h.
10. The method for preparing the nanofiber toughened silicon carbide surface environmental barrier ceramic coating according to claim 4, wherein the spraying adopts a supersonic plasma spraying method;
the technological parameters of the supersonic plasma spraying are as follows: the power is 25-60 KW, the Ar flow is 32-68L/min, the powder feeding amount is 6-40 g/min, and the spraying distance is 70-110 mm.
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| CN106631173A (en) * | 2017-01-16 | 2017-05-10 | 西北工业大学 | C/C composite material SiC-Y2Hf2O7 compound coating and preparation method thereof |
| US10604454B1 (en) * | 2016-06-16 | 2020-03-31 | United States Of America As Represented By The Administrator Of National Aeronautics And Space Administration | Advanced high temperature environmental barrier coating for SiC/SiC ceramic matrix composites |
| CN112851330A (en) * | 2021-01-23 | 2021-05-28 | 西安交通大学 | Method for preparing whisker toughening composite coating by liquid phase method spraying process |
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| US10604454B1 (en) * | 2016-06-16 | 2020-03-31 | United States Of America As Represented By The Administrator Of National Aeronautics And Space Administration | Advanced high temperature environmental barrier coating for SiC/SiC ceramic matrix composites |
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