CN114351134B - Crack-resistant high-temperature corrosion-resistant gradient ceramic coating and preparation method thereof - Google Patents
Crack-resistant high-temperature corrosion-resistant gradient ceramic coating and preparation method thereof Download PDFInfo
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- 238000005524 ceramic coating Methods 0.000 title claims abstract description 46
- 238000005260 corrosion Methods 0.000 title claims description 18
- 230000007797 corrosion Effects 0.000 title claims description 16
- 238000002360 preparation method Methods 0.000 title claims description 11
- 239000000919 ceramic Substances 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000000576 coating method Methods 0.000 claims abstract description 24
- 239000011248 coating agent Substances 0.000 claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 239000010410 layer Substances 0.000 claims abstract description 15
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 14
- 239000002344 surface layer Substances 0.000 claims abstract description 14
- 230000037452 priming Effects 0.000 claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000110 selective laser sintering Methods 0.000 claims description 4
- 229940058020 2-amino-2-methyl-1-propanol Drugs 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000149 argon plasma sintering Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 239000011229 interlayer Substances 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract description 2
- 239000002184 metal Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000035939 shock Effects 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention disclosesThe composite ceramic coating is designed into a double-layer gradient structure, and Al with high length-diameter ratio is added into a ceramic priming layer and a ceramic surface layer 2 O 3 Whisker, during sintering, al with high length-diameter ratio 2 O 3 The whisker can play a role in toughening and simultaneously has high length-diameter ratio Al 2 O 3 Whisker addition, during sintering, high aspect ratio Al 2 O 3 Whisker growth, which is favorable for increasing the binding force of a coating interface (coating and a substrate surface and between two coatings) through high length-diameter ratio Al 2 O 3 The pinning effect of the whisker on the interface of the two coatings plays a role in interlayer crack prevention, reduces the interface effect and avoids the falling of the ceramic coating caused by interlayer stress concentration.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a crack-resistant high-temperature corrosion-resistant gradient ceramic coating and a preparation method thereof.
Background
With the development of technology, many industrial devices need a metal matrix to be in service in severe environments for a long time, such as high temperature, humidity, high pressure, acid and alkali environments, so that the service life of the metal material is greatly shortened, and the actual production requirements cannot be met. The ceramic coating has the advantages of good high temperature resistance, oxidation resistance, wear resistance, corrosion resistance and the like, and is widely paid attention to more and more scientific researchers and enterprises. Moreover, the ceramic coating is widely applied to various industrial fields such as construction, metallurgy, ships, chemical machinery, aerospace and the like, and has very broad market prospect.
By depositing and cladding a ceramic coating on the surface of the metal matrix, the metal matrix can be isolated from a high-temperature and high-corrosion environment due to the existence of the ceramic coating, so that the risk of oxidation corrosion of the metal matrix is greatly reduced, and devices (such as a superheater tube) introducing the ceramic coating can operate in the high-temperature and high-corrosion environment.
The metal-based ceramic coating refers to the generic term for a ceramic protective layer or surface film applied to a metal surface. However, the brittle nature of the ceramic material and the large difference in physical properties of the metal matrix result in a lower bond strength of the ceramic coating to the metal matrix. In addition, the ceramic coating has high brittleness, and can be subjected to the actions of compressive stress, impact load, fatigue cyclic stress and the like in a frictional wear environment, and once the stress in the coating exceeds the tensile limit of the coating material, the coating material is subjected to brittle fracture, so that cracks are generated, and the cracks in the coating are easily expanded to peel off the coating.
Disclosure of Invention
Aiming at the problems in the background technology, the invention provides a preparation method of a crack-resistant high-temperature corrosion-resistant gradient ceramic coating.
The technical scheme of the invention is as follows:
a preparation method of a crack-resistant high-temperature corrosion-resistant gradient ceramic coating comprises the following specific steps:
step S1, preparing Al with high length-diameter ratio 2 O 3 Whisker:
mixing water, polyethylene glycol and 2-amino-2-methyl-1-propanol, regulating pH value to 10-11, and mixing with Al 2 O 3 Mixing the whiskers, and ball-milling for 30-120 min under the conditions of ultrasonic and stirring; drying and sieving to obtain Al with high length-diameter ratio 2 O 3 Whiskers;
step S2, adding (30-50) wt% of SiC, (30-50) wt% of Si 3 N 4 (8-14) wt% Cr 2 O 3 (4-10) WC in weight percent is ceramic powder;
step S3, al with high aspect ratio 2 O 3 Whisker and ceramic powder are mixed to be used as a priming layer of the composite coating, wherein Al 2 O 3 The whisker content is 10-30%;
step S4, al with high aspect ratio 2 O 3 Whisker and flaky alumina particles are mixed with ceramic powder to form a ceramic surface layer, wherein Al 2 O 3 The whisker content is 5-10%, and the flaky alumina particle content is 4-8%;
wherein the flaky alumina particles are flaky alumina powder with particle morphology, the ratio of the plate width to the plate thickness of the flaky alumina particles is between 3 and 10, and the plate width of the flaky alumina particles is between 0.3 and 0.9 mu m;
and S5, finally, carrying out gradient sintering on the alloy substrate coated with the composite ceramic coating to obtain the composite ceramic coating.
Further, the conditions of ultrasonic and stirring in step S1 are: the time is 30-60 min; the rotating speed in the ball milling treatment process is 50-70 rpm, and the diameter of the grinding ball is 3-5 mm.
Further, in step S2, the particle size of the ceramic powder is 20 to 60 μm, wherein 80% or more of the ceramic powder has a particle size.
Further, the thickness of the coating of the priming layer is 0.08-0.2 mm, and the thickness of the ceramic surface layer is 0.1-0.8 mm.
Further, the preparation of the coating in the steps S3 and S4 adopts a laser sintering process, and the method concretely comprises the following steps:
the selective laser sintering process is adopted, and the sintering conditions are as follows: the laser power is 200-1200W, the scanning speed is 160-300 mm/s, the scanning interval is 0.2-0.8 mm, and a priming layer and a ceramic surface layer are sequentially formed on the surface of the alloy substrate.
Further, the gradient sintering process in step S5 is as follows: gradient sintering is carried out in the sintering atmosphere of inert gas, and the conditions of the sintering process are as follows: heat preservation is carried out for 1h at the temperature of 250-420 ℃, then the temperature is raised at the speed of 5-10 ℃/min, heat preservation is carried out for 0.5-1 h at the temperature of 620-850 ℃, the temperature is continuously raised, high-temperature sintering is carried out for 0.5-1 h at the temperature of 1020-1060 ℃, and finally, the composite ceramic coating is formed on the surface of the alloy substrate.
The invention also aims to provide the crack-resistant high-temperature corrosion-resistant composite ceramic coating prepared by the preparation method.
Further, the thickness of the composite ceramic coating is 0.2-1.2mm.
The beneficial effects of the invention are as follows:
(1) The composite ceramic coating is designed into a double-layer gradient structure, and Al with high length-diameter ratio is added into the ceramic priming layer and the ceramic surface layer 2 O 3 Whisker, during sintering, al with high length-diameter ratio 2 O 3 The whisker can play a role in toughening and simultaneously has high length-diameter ratio Al 2 O 3 Whisker addition, during sintering, high aspect ratio Al 2 O 3 Whisker growth, which is favorable for increasing the binding force of a coating interface (coating and a substrate surface and between two coatings) through high length-diameter ratio Al 2 O 3 The pinning effect of the whisker on the interface of the two coatings plays a role in interlayer crack prevention, reduces the interface effect and avoids the falling of the ceramic coating caused by interlayer stress concentration.
(2) In the present invention, the ceramicFlaky Al with specific toughening effect is added into the surface layer 2 O 3 Particle, embedded flake Al during gradient sintering process 2 O 3 The particles help to inhibit the growth of crystal particles in the ceramic powder, so that the ceramic crystal particles in the coating are finer, the tissue structure is more uniform, the stress concentration and the generation of microscopic cracks are reduced, the microcrack expansion resistance of the surface layer of the coating can be improved, the formation of a high-density ceramic surface layer is facilitated, and the high-temperature resistance, corrosion resistance and oxidation resistance of the ceramic coating are improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments.
Example 1
Preparation of crack-resistant high-temperature corrosion-resistant gradient ceramic coating:
step S1, preparing Al with high length-diameter ratio 2 O 3 Whisker:
(1)Al 2 O 3 the total adding amount of the whisker is configured according to 25vol% of the solid content of the slurry, polyethylene glycol accounting for 2% of the powder mass and 2-amino-2-methyl-1-propanol accounting for 0.15% of the powder mass are added into deionized water, the pH value of the solution is regulated to 10-11, the solution is stirred and mixed for 20min, and Al is slowly added under the action of ultrasonic and paddle synergistic stirring 2 O 3 The whisker is continuously stirred for 30min under ultrasonic synergy, and the obtained Al is obtained 2 O 3 Placing whisker slurry into a ball milling tank, using a 5mm zirconia grinding ball, and slowly ball-milling for 2 hours by using a roller ball mill at a rotating speed of 70 rpm;
ball-milling Al 2 O 3 Taking out whisker slurry, drying the slurry by using a rotary evaporation device, and sieving the slurry with a 100-mesh sieve to obtain Al with high length-diameter ratio 2 O 3 Whisker powder;
(2) 45wt% SiC, 35wt% Si 3 N 4 12wt% Cr 2 O 3 8wt% of WC is ceramic powder; more than 80% of the ceramic powder has a particle size of 20-60 mu m;
(3) Adopts selective laser sintering process and uses Al with high length-diameter ratio 2 O 3 The whisker is mixed with ceramic powder to form a priming layer on the surface of the base material, and the sintering conditions are as follows: the laser power is 1200W, the scanning speed is 260mm/s, and the scanning interval is 0.6mm;
wherein Al is 2 O 3 The whisker content is 10-30%; the thickness of the coating of the priming layer is 0.2mm;
(4) Adopts selective laser sintering process and uses Al with high length-diameter ratio 2 O 3 Whisker, flaky alumina particles and ceramic powder are mixed to form a ceramic surface layer on the surface of a priming layer, and sintering conditions are as follows: the laser power is 1200W, the scanning speed is 260mm/s, and the scanning interval is 0.6mm;
wherein Al is 2 O 3 The whisker content is 5-10%, and the flaky alumina particle content is 4-8%; the thickness of the ceramic surface layer is 0.6mm;
wherein the flaky alumina particles are flaky alumina powder with particle morphology, the ratio of the plate width to the plate thickness of the flaky alumina particles is between 3 and 10, and the plate width of the flaky alumina particles is between 0.3 and 0.9 mu m;
(5) And finally, carrying out gradient sintering on the alloy base material of the cladding composite ceramic coating, wherein the gradient sintering process is as follows: gradient sintering is carried out in the sintering atmosphere of inert gas, and the conditions of the sintering process are as follows: heat preservation is carried out for 1h at 320 ℃, then the temperature is raised at the speed of 8 ℃/min, heat preservation is carried out for 0.5h at 750 ℃, the temperature is continuously raised, high-temperature sintering is carried out for 0.5h at 1040 ℃, and finally the composite ceramic coating is formed on the surface of the alloy substrate.
Example 2
A plurality of groups of ceramic coatings are prepared according to the method of the example 1, the components and the proportion of the ceramic powder are kept unchanged, and Al with high length-diameter ratio in the priming layer and the ceramic surface layer is changed 2 O 3 The contents of the whisker and the flaky alumina particles are shown in Table 1. Comparative example 1 ceramic coating prepared directly from ceramic powder, comparative example 2 was prepared with a composition containing 25% al 2 O 3 Whisker and ceramic powder of 6% flaky alumina particlesThe ceramic coating is prepared.
TABLE 1 component content
And (3) testing: performance testing
Thermal shock test: performing thermal shock test at 1400 ℃ for 10 times on the ceramic coatings in examples 1-3 and comparative examples 1 and 2, and observing the falling-off condition and the oxidation resistance improvement rate of the coatings;
oxidative weight gain test: the ceramic coatings of examples 1 to 3 and comparative examples 1 and 2 were applied to the metal surface, the weight was measured, and the ceramic coatings were placed under the environments of 1100 ℃ and 1150 ℃ to measure the weight, and finally the weight gain was obtained;
thermal conductivity testing: and detecting by adopting a thermal conductivity tester. The test results are shown in Table 2.
TABLE 2 measurement of ceramic coating Properties
According to the data, the composite ceramic coating with the double-layer structure has good oxidation resistance, good high temperature resistance, no crack or falling after thermal shock test, good heat insulation performance and wide application prospect.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (7)
1. The preparation method of the crack-resistant high-temperature corrosion-resistant gradient ceramic coating is characterized by comprising the following specific steps:
step S1, preparing Al with high length-diameter ratio 2 O 3 Whisker：
Mixing water, polyethylene glycol and 2-amino-2-methyl-1-propanol, regulating pH value to 10-11, and mixing with Al 2 O 3 Mixing the whiskers, and ball-milling for 30-120 min under the conditions of ultrasonic and stirring; drying and sieving to obtain Al with high length-diameter ratio 2 O 3 Whiskers;
step S2, adding (30-50) wt% of SiC, (30-50) wt% of Si 3 N 4 (8-14) wt% Cr 2 O 3 (4-10) WC in weight percent is ceramic powder;
step S3, al with high aspect ratio 2 O 3 Whisker and ceramic powder are mixed to be used as a priming layer of the composite coating, wherein Al 2 O 3 The whisker content is 10-30%;
step S4, al with high aspect ratio 2 O 3 Whisker and flaky alumina particles are mixed with ceramic powder to form a ceramic surface layer, wherein Al 2 O 3 The whisker content is 5-10%, and the flaky alumina particle content is 4-8%;
wherein the flaky alumina particles are flaky alumina powder with particle morphology, the ratio of the plate width to the plate thickness of the flaky alumina particles is between 3 and 10, and the plate width of the flaky alumina particles is between 0.3 and 0.9 mu m;
step S5, finally, carrying out gradient sintering on the alloy substrate coated with the composite ceramic coating to obtain the composite ceramic coating;
the gradient sintering process in the step S5 is as follows: gradient sintering is carried out in the sintering atmosphere of inert gas, and the conditions of the sintering process are as follows: heat preservation is carried out for 1h at the temperature of 250-420 ℃, then the temperature is raised at the speed of 5-10 ℃/min, heat preservation is carried out for 0.5-1 h at the temperature of 620-850 ℃, the temperature is continuously raised, high-temperature sintering is carried out for 0.5-1 h at the temperature of 1020-1060 ℃, and finally, the composite ceramic coating is formed on the surface of the alloy substrate.
2. The method for preparing the crack-resistant high-temperature corrosion-resistant gradient ceramic coating according to claim 1, wherein the conditions of ultrasonic and stirring in the step S1 are as follows: the time is 30-60 min; the rotating speed in the ball milling treatment process is 50-70 rpm, and the diameter of the grinding ball is 3-5 mm.
3. The method for preparing the crack-resistant high-temperature corrosion-resistant gradient ceramic coating according to claim 1, wherein in the step S2, more than 80% of ceramic powder has a powder particle size of 20-60 μm.
4. The method for preparing the crack-resistant high-temperature corrosion-resistant gradient ceramic coating according to claim 1, wherein the thickness of the coating of the primer layer is 0.08-0.2 mm, and the thickness of the ceramic surface layer is 0.1-0.8 mm.
5. The preparation method of the crack-resistant high-temperature corrosion-resistant gradient ceramic coating as claimed in claim 1, wherein the coating preparation in the steps S3 and S4 adopts a laser sintering process, and is specifically as follows:
the selective laser sintering process is adopted, and the sintering conditions are as follows: the laser power is 200-1200W, the scanning speed is 160-300 mm/s, the scanning interval is 0.2-0.8 mm, and a priming layer and a ceramic surface layer are sequentially formed on the surface of the alloy substrate.
6. A gradient ceramic coating prepared by the method for preparing the crack-resistant high-temperature corrosion-resistant gradient ceramic coating according to any one of claims 1 to 5.
7. The gradient ceramic coating of claim 6, wherein the gradient ceramic coating has a thickness of 0.2mm to 1.2mm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0202504A2 (en) * | 1985-05-24 | 1986-11-26 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | Composite ceramic |
| JPH06157152A (en) * | 1992-11-16 | 1994-06-03 | Toshiba Corp | Fiber reinforced composite gradient material and it production |
| CN107056316A (en) * | 2017-06-20 | 2017-08-18 | 广东工业大学 | A kind of preparation method of high length-diameter ratio alumina whisker Strengthening and Toughening Ce TZP complex phase ceramics |
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2021
- 2021-11-23 CN CN202111393952.0A patent/CN114351134B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0202504A2 (en) * | 1985-05-24 | 1986-11-26 | Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. | Composite ceramic |
| US4767727A (en) * | 1985-05-24 | 1988-08-30 | Max-Planck-Gesellschaft Zur Foerderung Der Wissenschaften E.V. | Fibre-strengthened ceramic formed bodies |
| JPH06157152A (en) * | 1992-11-16 | 1994-06-03 | Toshiba Corp | Fiber reinforced composite gradient material and it production |
| CN107056316A (en) * | 2017-06-20 | 2017-08-18 | 广东工业大学 | A kind of preparation method of high length-diameter ratio alumina whisker Strengthening and Toughening Ce TZP complex phase ceramics |
Non-Patent Citations (1)
| Title |
|---|
| Al_2O_3晶须强化细晶氧化铝陶瓷的放电等离子烧结研究;梁媛媛;耐火与石灰(第03期);全文 * |
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