CN1386891A - Process for co-diffusing aluminium-rere-earth element in silicon titanocarbide material - Google Patents
Process for co-diffusing aluminium-rere-earth element in silicon titanocarbide material Download PDFInfo
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- CN1386891A CN1386891A CN 02109467 CN02109467A CN1386891A CN 1386891 A CN1386891 A CN 1386891A CN 02109467 CN02109467 CN 02109467 CN 02109467 A CN02109467 A CN 02109467A CN 1386891 A CN1386891 A CN 1386891A
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- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 26
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title description 2
- 229910052710 silicon Inorganic materials 0.000 title 1
- 239000010703 silicon Substances 0.000 title 1
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 22
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 21
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 13
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 11
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 21
- 238000001764 infiltration Methods 0.000 claims description 19
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- 238000009792 diffusion process Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052734 helium Inorganic materials 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 150000002910 rare earth metals Chemical class 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 3
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 3
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 3
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical group O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 2
- 229910009817 Ti3SiC2 Inorganic materials 0.000 abstract description 10
- 229910052593 corundum Inorganic materials 0.000 abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 239000002344 surface layer Substances 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 description 28
- 238000007254 oxidation reaction Methods 0.000 description 28
- 238000000576 coating method Methods 0.000 description 16
- 239000011248 coating agent Substances 0.000 description 14
- 239000010936 titanium Substances 0.000 description 10
- 230000008595 infiltration Effects 0.000 description 8
- ZWOQODLNWUDJFT-UHFFFAOYSA-N aluminum lanthanum Chemical compound [Al].[La] ZWOQODLNWUDJFT-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- RFEISCHXNDRNLV-UHFFFAOYSA-N aluminum yttrium Chemical compound [Al].[Y] RFEISCHXNDRNLV-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- 229910002244 LaAlO3 Inorganic materials 0.000 description 1
- 229910000943 NiAl Inorganic materials 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 238000005269 aluminizing Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000005475 siliconizing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
A process for co-diffusing Al-rare-earth element into Ti3SiC2 material is characterized by that its diffusing material is composed of Al powder, rare-earth oxide powder and sodium fluoride powder. It is prepared by embedding the Ti3SiC2 material in the diffusing powder at 1000-1200 deg.C for 2-8 hr. When it is oxidized in the air at 1000-1200 deg.C, a complete Al2O3 surface layer is formed. It can be used in high-temp corrosion environment.
Description
Technical Field
The invention relates to a surface engineering technology, in particular to a method for co-infiltrating titanium silicon carbide material aluminum-rare earth.
Background
Silicon titanium carbide (Ti)3SiC2) Is a structure/function integrated material with excellent performance, organically integrates the plasticity, the electric conduction, the heat conduction and the easy addition of metalThe ceramic material has the characteristics of high temperature resistance, thermal shock resistance, high strength and low specific gravity, and has wide application prospect when being used as a high-temperature structural material. Although the silicon titanium carbide material contains an oxidation resistance element Si, a titanium dioxide and a mixed oxide layer of the titanium dioxide and the silicon dioxide are mainly formed in the oxidation process, and the oxidation resistance is poor above 1000 ℃.
At present, for heat-resistant alloy materials, a thermal diffusion metal infiltration method is widely adopted to prepare a compound coating to improve the high-temperature oxidation resistance of the compound coating. For ceramic materials, this method is rarely used. The reason is that the ceramic material has good stability and is oxidation-resistant, and the ceramic material is usually used as an oxidation-resistant coating material of other metals; second, the infiltrant does not readily react with the ceramic to form a new compound layer. Due to Ti3SiC2The oxidation resistance is poor above 1000 ℃, and the application of a protective coating is necessary for realizing the practicability of the coating. At Ti3SiC2The work on the preparation of the oxidation resistant coatings reported only thermal Diffusion siliconizing(T.El-Ragy, M.W.Barsum, Diffusion kinetics of the carbonization and silicidation of Ti3SiC2J.appl.Phys., 83(1) (1998)112-&119), in particular, a test piece sandwiched by two single crystal silicon pieces and subjected to thermal diffusion at high temperature (1350 ℃ C.), high vacuum, and applied force, with a coating thickness of about 10 μm for 15 hours. The process has the following defects: the process is complex, the operation time is long, the power consumption is large, the cost is high, the coating thickness is not ideal enough, and the industrialization is not easy to realize. In addition, although aluminizing on superalloys is a relatively extensive protective technique, no mention is made of TiSiC2The Al infiltration or Al-RE co-infiltration is reported.
Disclosure of Invention
The invention aims to provide a titanium silicon carbide (Ti)3SiC2) The method for the co-infiltration of the material with the rare earth element (RE) has the advantages of simple process, strong practicability and low cost, and can effectively improve the high-temperature oxidation resistance of the titanium silicon carbide material.
In order to achieve the purpose, the technical scheme of the invention is as follows: putting a titanium silicon carbide material in a solid powder mixture which is fully filled with aluminum powder, rare earth oxide powder and sodium fluoride, vacuumizing the system to 1-10 Pa, heating to 1000-1200 ℃ at a heating rate of 20-40 ℃/min under the protection of inert gas, keeping the temperature for 2-8 hours, and cooling to room temperature along with the furnace to obtain an aluminum-rich and rare earth-rich diffusion layer;
the purity of the aluminum powder (Al) is more than or equal to 99.00 percent, and the granularityis less than or equal to 0.4 mm; the purity of the rare earth oxide powder is more than or equal to 99.00 percent, and the particle size is less than or equal to 0.4 mm; sodium fluoride (NaF) was analytically pure; the components in the solid powder mixture comprise, by weight, 5-30 parts of aluminum powder, 65-90 parts of rare earth oxide and 0.5-5 parts of sodium fluoride; the inert gas in the aluminum-rare earth co-infiltration process is argon, and the purity is more than or equal to 99.99 percent; or helium with purity more than or equal to 99.99 percent; the rare earth oxide is La2O3、Y2O3、Gd2O3、Nd2O3Or CeO2。
The invention provides an aluminum-rare earth co-infiltration process for a titanium silicon carbide material, which has the following principle: firstly, adding a considerable amount of aluminum on the surface of the material, and endowing the material with oxidation resistance due to the main formation of aluminum oxide during oxidation; and secondly, when the rare earth is co-infiltrated with the rare earth element, the high activity of the rare earth is utilized to promote the infiltration of aluminum and improve the microstructure of the infiltrated layer on the one hand, and the high activity is favorable for reducing the oxidation rate of the infiltrated layer and improving the anti-stripping performance of the oxide film on the surface of the infiltrated layer on the other hand.
The invention has the following advantages:
1. after the aluminum-rare earth co-cementation heat treatment is adopted, the Ti content can be remarkably reduced3SiC2High temperature oxidation rate of the material. For example, Ti after constant temperature oxidation at 1100 ℃ in air for 20 hours3SiC2The oxidation weight of the catalyst is increased to 17mg/cm2While the oxidation weight gain of the coating is only 2.2mg/cm2The reduction is nearly 8 times; the oxidation parabolic linear constants of the two are respectively 4.43 multiplied by 10-7kg2m-4s-1And 1.58X 10-9kg2m-4s-1And 2 orders of magnitude reduction. The cyclic oxidation experiment at 1100 ℃ proves the anti-stripping performance of the oxide film on the surface of the coatingIt also has the improvement. The surface oxide film is mainly composed of intact Al2O3Layer composition with small amounts of discontinuous TiO on the outer surface2。
2. Has sufficient permeating layer thickness and protection life. The thickness of the infiltration layer in the process range of the invention can reach millimeter magnitude (the thickness of the conventional thermal diffusion coating is in micrometer magnitude), namely, the matrix contains enough aluminum, so that complete Al on the inner surface for a long time in the oxidation process can be ensured2O3The layer grows stably, and the service life of the permeable layer playing a protective role is long. In particular, the amount of rare earth incorporated reaches a measurable level, which is difficult to achieve with conventional metallic materials.
3. The operation is simple, and the industrialization is easy. The invention adopts the mixture of solid silicon powder and other additives to embed the sample of the titanium silicon carbide material, obtains the infiltration layer with high aluminum content through high-temperature thermal diffusion, and compared with other surface treatment technologies (such as physical vapor deposition coating, chemical vapor deposition coating, ion implantation elements and the like) in the prior art, the invention has the advantages of simple raw materials and operation process, shortened operation time, reducedpower consumption, low requirements on equipment and control precision, low whole cost and possibility of realizing industrialization.
4. The application range is wide. The invention can be used for processing smooth surfaces and actual workpieces with complex surfaces, has strong practicability and can ensure that Ti can be used3SiC2The material is applied to various high-temperature corrosive environments.
Drawings
FIG. 1 shows Ti of the present invention3SiC2The scanning electron micrograph of the section after the aluminum-lanthanum co-infiltration shows that the white bright spot area in the figure is La after analysis and verification3Al。
FIG. 2 shows Ti of the present invention3SiC2X-ray diffraction spectrum of the surface after the aluminum-lanthanum co-infiltration treatment.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Example 1
In the present invention, the composition of the solid powder mixture used for the aluminum-rare earth co-cementation is:
the purity of the aluminum powder (Al) is more than or equal to 99.00 percent, and the granularity is less than or equal to 0.4 mm;
the purity of the rare earth oxide powder is more than or equal to 99.00 percent, and the particle size is less than or equal to 0.4 mm;
sodium fluoride (NaF) was analytically pure.
The proportion (weight percentage) of the solid powder mixture used for the aluminum-rare earth co-cementation is as follows:
5-30% of aluminum powder; 65-90% of rare earth oxide powder; 0.5-5% of sodium fluoride.
Embedding a sample of a silicon titanium carbide body material by using a solid powder mixture consisting of aluminum powder, rare earth oxide powder and sodium fluoride in a corundum charging bucket, and then placing the corundum charging bucket in a system capable of being vacuumized and filled with argon. Firstly, vacuumizing the system to 1-10 Pa, then filling argon (99.99% Ar) or helium (99.99% He), heating to 1000-1200 ℃ at the heating rate of 20-40 ℃/min, keeping the temperature for 2-8 hours, and then cooling to room temperature along with the furnace, thus completing the whole process of the aluminum-rare earth co-infiltration. After the titanium silicon carbide material is subjected to aluminum-rare earth co-infiltration, the RE-enriched material with the thickness reaching millimeter level can be obtained3Al dispersed particles and Al substituted matrix Ti3SiC2Ti formed of Si in (1)3AlC2The porous layer of (3).
The specific data in this embodiment are: ti3SiC2Sample size 10 × 5 × 2 mm; the infiltration material comprises the following components in percentage by weight: 20% aluminum powder, 79% lanthanum oxide (La)2O3) Powder, 1% sodium fluoride, total weight 25 Og; the system was evacuated to 10Pa, then argon (99.99% Ar) was introduced, the heating temperature: 1100 ℃, temperature rise rate: 20 ℃/min, heat preservation time: for 4 hours.
The aluminum-lanthanum co-cementation reaction comprises the following steps:
aluminum reduces a part of lanthanum in lanthanum oxide at high temperature to form composite oxide LaAlO3(ii) a The reduced lanthanum and aluminum form La3Al permeates into the material through the crystal boundary and the gap of the matrix material and finally exists in a dispersion enrichment area; some aluminum is dissolved in the other region of the silicon titanium carbide by the reaction formula (3).
The surface of the sample after permeation is smooth and is grey white. The sample after the aluminum-lanthanum co-infiltration is made into a metallographic sample, a plurality of white areas (see figure 1) are dispersedly distributed on the sample under the observation of a scanning electron microscope, the white areas are enriched with aluminum and lanthanum as shown by energy spectrum analysis, and the infiltrated layer penetrates through the thickness of the whole sample as shown in figure 1. X-ray diffraction analysis confirmed that the white region contained La3The Al phase, the result of X-ray diffraction analysis is shown in FIG. 2.
The resulting aluminiumlanthanum co-infiltrated layer is different from the infiltrated layer obtained by thermal diffusion infiltration of metal over conventional metals, where a compound coating is obtained. For example: the Ni-based alloy is infiltrated with Al to obtain a NiAl coating (Pichoir R. in: Materials and Coatings to Resist High Temperature corporation, Holmes D R, Rahmel A. Ed. London; Applied Science Publishers Ltd., 1978), even if Ti3SiC2By up-doping Si, a silicide (TiSi) is also obtained2And SiC) coating.
Ti3SiC2After the material is subjected to aluminum-lanthanum co-permeation, the linear constant of a parabola subjected to constant-temperature oxidation in air at the temperature of 1000-1200 ℃ is reduced by 2-3 orders of magnitude. For example, Ti after constant temperature oxidation at 1100 ℃ in air for 20 hours3SiC2The oxidation weight of the catalyst is increased to 17mg/cm2While the oxidation weight gain of the coating is only 2.2mg/cm2The reduction is nearly 8 times; and the linear constants of the parabolas of the oxidation are respectively 4.43 multiplied by 10-7kg2m-4s-1And 1.58X 10-9kg2m-4s-1And 2 orders of magnitude reduction. Cyclic oxidation experiment at 1100 deg.C (empty after 1 hour of oxidation)One cycle of cooling for 15 minutes) demonstrated that the oxide film on the surface of the infiltrated layer did not flake off for as long as 300 cycles. The surface oxide film was analyzed to be composed mainly of intact Al2O3Layer composition with small amounts of discontinuous TiO on the outer surface2. Intact Al2O3The layer is formed by infiltrating layer to improve Ti3SiC2The main cause of oxidation resistance.
Example 2
The difference from the embodiment 1 is that: example Ti3SiC2Sample size was 10 × 5 × 2 mm; the infiltration material comprises the following components in percentage by weight: 25% aluminum powder, 74.5% yttrium oxide (Y)2O3) Powder, 0.5% sodium fluoride, the total weight is 150 g; embedding a sample of a silicon titanium carbide material by using a solid powder mixture consisting of aluminum powder, yttrium oxide powder and sodium fluoride in a corundum charging bucket, and then placing the corundum charging bucket in a system capable of vacuumizing and filling argon. Firstly, vacuumizing the system to 10Pa, then filling argon (99.99% Ar), heating to 1100 ℃, and heating at the speed: 30 ℃/min, keeping the temperature for 2 hours, and then cooling to the room temperature along with the furnace, thus completing the whole process of the aluminum-yttrium co-infiltration.
The surface of the sample after permeation is smooth and is grey white. The observation of a scanning electron microscope and the analysis of X-ray diffraction show that the aluminum-yttrium co-permeation layer is obtained by the process. The Y-rich layer is dispersed in the infiltrated layer3Al phase, and Al solid-dissolved in the matrix. The thickness of the infiltrated layer reaches 2 mm. The oxidation experiment in the air at 1200 ℃ shows that the Ti after the aluminum-yttrium co-penetration3SiC2Complete and continuous Al is formed on the surface2O3The parabolic velocity constant decreases by 3 orders of magnitude.
The inert gas is also helium, and the purity is more than or equal to 99.99 percent; the rare earth oxide is also Gd2O3、Nd2O3Or CeO2。
Claims (5)
1. A method for co-infiltrating titanium silicon carbide material aluminum-rare earth is characterized by comprising the following steps: the titanium silicon carbide material is placed in a solid powder mixture which is fully filled with aluminum powder, rare earth oxide powder and sodium fluoride, heated to 1000-1200 ℃ at the heating rate of 20-40 ℃/min under the protection of inert gas, kept for 2-8 hours and cooled to room temperature along with a furnace, and the aluminum-rich and rare earth-rich diffusion layer is obtained.
2. The method of claim 1, wherein: the purity of the aluminum powder is more than or equal to 99.00 percent, and the granularity is less than or equal to 0.4 mm; the purity of the rare earth oxide powder is more than or equal to 99.00 percent, and the particle size is less than or equal to 0.4 mm; sodium fluoride was analytically pure.
3. The method of claim 1, wherein: the solid powder mixture comprises, by weight, 5-30 parts of aluminum powder, 65-90 parts of rare earth oxide and 0.5-5 parts of sodium fluoride.
4. The method of claim 1, wherein: the inert gas used in the aluminum-rare earth co-infiltration process is argon, and the purity is more than or equal to 99.99 percent; or helium with purity more than or equal to 99.99 percent.
5. The method of claim 1, wherein: the rare earth oxide is La2O3、Y2O3、Gd2O3、Nd2O3Or CeO2。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1321220C (en) * | 2003-11-17 | 2007-06-13 | 中国科学院金属研究所 | Method of forming boride coating layer on Ti3 SiC2 material surface |
| CN102992765A (en) * | 2012-11-09 | 2013-03-27 | 航天材料及工艺研究所 | Preparation method of tungsten-doped titanium-silicon-aluminum-carbon ceramic block body material |
| CN105948747A (en) * | 2016-05-18 | 2016-09-21 | 东北大学 | Method for preparing dense diffusion barrier of limiting current type oxygen sensor with co-permeation method |
| CN107858640A (en) * | 2017-11-21 | 2018-03-30 | 江苏大学 | A kind of method for improving calorized coating high temperature oxidation resistance |
| CN109400210A (en) * | 2018-11-30 | 2019-03-01 | 河北工业大学 | A kind of Ti3SiC2-Al2O3- SiC-Al composite material and preparation method |
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- 2002-04-12 CN CNB021094675A patent/CN1152152C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321220C (en) * | 2003-11-17 | 2007-06-13 | 中国科学院金属研究所 | Method of forming boride coating layer on Ti3 SiC2 material surface |
| CN102992765A (en) * | 2012-11-09 | 2013-03-27 | 航天材料及工艺研究所 | Preparation method of tungsten-doped titanium-silicon-aluminum-carbon ceramic block body material |
| CN102992765B (en) * | 2012-11-09 | 2014-03-05 | 航天材料及工艺研究所 | Preparation method of tungsten-doped titanium-silicon-aluminum-carbon ceramic block body material |
| CN105948747A (en) * | 2016-05-18 | 2016-09-21 | 东北大学 | Method for preparing dense diffusion barrier of limiting current type oxygen sensor with co-permeation method |
| CN107858640A (en) * | 2017-11-21 | 2018-03-30 | 江苏大学 | A kind of method for improving calorized coating high temperature oxidation resistance |
| CN109400210A (en) * | 2018-11-30 | 2019-03-01 | 河北工业大学 | A kind of Ti3SiC2-Al2O3- SiC-Al composite material and preparation method |
| CN109400210B (en) * | 2018-11-30 | 2021-07-06 | 河北工业大学 | Ti3SiC2-Al2O3-SiC-Al composite material and preparation method thereof |
| CN118290182A (en) * | 2024-04-03 | 2024-07-05 | 西安博德励勤复合材料科技有限公司 | Preparation method of fan blade |
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