CN100577605C - High-temperature oxidation-resistant material and high-temperature anti-oxidation coating prepared thereby - Google Patents
High-temperature oxidation-resistant material and high-temperature anti-oxidation coating prepared thereby Download PDFInfo
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- CN100577605C CN100577605C CN200710165074A CN200710165074A CN100577605C CN 100577605 C CN100577605 C CN 100577605C CN 200710165074 A CN200710165074 A CN 200710165074A CN 200710165074 A CN200710165074 A CN 200710165074A CN 100577605 C CN100577605 C CN 100577605C
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Abstract
The invention relates to a heat-resistant refractory material frequently used in aerospace field, in particular to a heat-resistant anti-oxidant material and a heat-resistant anti-oxidant coating prepared by the material. the heat-resistant anti-oxidant material is made into powder and placed into the vessel, the ethanol or pure water with 3-7 times volume of the above powder is used as carrier, the potassium or sodium salt with 1.5-2.3 percent of the above powder mass is added for even mixing, additionally polyethylene glycol with 0.1-1.3 percent of the above powder mass is added for once more even mixing, and then the coating slurry is spread on the substrate, and sintered under the condition of temperature 1350 DEG C to 1650 DEG C and vacuum more than 10E-1 Pa, and finally kept warm for 5-30 minutes. The coating can be matched with the Nb-W alloy under high temperature environment for use, the invention has the performances of anti-oxidization and anti-flushing, and can widely be applied on the engine nozzles, turbine blades, combustion chamber and other high temperature structural parts.
Description
Technical field
The present invention relates to be usually used at present the high temperature resistant refractory material in the aerospace field, especially a kind of high-temperature oxidation-resistant material, and high-temperature oxidation resistant coating prepared therefrom.
Background technology
Along with the high speed development of aeronautical and space technology, high-efficiency engine, superelevation sonic flight device and many thermal structure spares all need the material that can have active strength, oxidation-resistance and workability under 1300 ℃～1800 ℃.People have developed the multiple superalloy based on refractory metal for this reason, niobium tungstenalloy series wherein, because its excellent high-temperature mechanical property and high-melting-point, properties of low density are that other high-temperature materials hardly match, thereby have obtained widespread use at aerospace field.
In actual use, nearly all superalloy all has at high temperature vigorous oxidation and makes material suffer " calamity unrest " destructive problem, has seriously limited the range of application of material.Greatly about being vigorous oxidation more than 350 ℃, the heating element of tungsten, molybdenum, tantalum usually is limited to because of high temperature oxidation use under the high vacuum condition as niobium and niobium-base alloy.
Along with the expansion of alloy Application Areas, the research of superalloy and coating thereof and application have also obtained fast development.Wherein C103 alloy and coating thereof are applicable to high temperature range below 1400 ℃, at home and abroad continued to have used two, 30 years, the 5BM ц of USSR (Union of Soviet Socialist Republics) development is a kind of aerospace high-temperature material that obviously is better than C103, can be used for 1600 ℃ of-1700 ℃ of high temperature after adding coating layer, it is reported, rhenium, iridium alloy can use 1800 ℃-2000 ℃, but its proportion is bigger, and price is too high.At present, aerospace high temperature niobium alloy such as C103 alloy, and United States Patent (USP) 5,942, niobium alloy that 055 and 5,721,061 grade is mentioned and coating thereof generally only are applicable to stable use the below 1400 ℃, not competent hot environment more than 1600 ℃ can not satisfy the engine that more high specific impulse and working efficiency require.
Summary of the invention
The purpose of this invention is to provide and in hot environment, to be used with the niobium tungstenalloy, have performances such as antioxidant anticorrosive, antiscour, and can be widely used in a kind of high-temperature oxidation-resistant material on engine nozzle, turbine blade, combustion chamber and other high-temperature structural components;
Another object of the present invention provides a kind of high-temperature oxidation resistant coating by above-mentioned high-temperature oxidation-resistant material preparation.
A kind of high-temperature oxidation-resistant material is characterized in that, component is:
MoSi2 is 2.5～9.5Wt%, and Mo is 2.5～10.0Wt%, and W is 1.0～4.0Wt%, and HfO2 is 0.1～1.5Wt%, and Y is 1.0～8.0Wt%;
Surplus is Si.
A kind of high-temperature oxidation-resistant material is characterized in that, comprises following component:
MoSi2 is 2.5～9.5Wt%, and Mo is 2.5～10.0Wt%, and W is 1.0～4.0Wt%, and HfO2 is 0.1～1.5Wt%, and Y is 1.0～8.0Wt%;
And at least a in the following component
Fe is 1.5～4.0Wt%, and Al is 2.0～8.0Wt%, and Ta is 3.0～9.0Wt%, and Ti is 0.1～3.0Wt%, and S is 0.1～5.0Wt%, and B is 0.1～2.5Wt%;
Surplus is Si.
Further, high-temperature oxidation-resistant material is characterized in that, component is:
MoSi2 is 6.5Wt%, and Mo is 6.0Wt%, and W is 3.8Wt%, and HfO2 is 1.5Wt%, and Y is 6.0Wt%;
Fe is 3.5Wt%, and Al is 4Wt%, and Ta is 4.5Wt%, and Ti is 1Wt%, and S is 0.9Wt%, and B is 1.7Wt%;
Surplus is Si.
A kind of high-temperature oxidation-resistant material is characterized in that, component is:
Al is 2.0～8.0Wt%, and MoSi2 is 2.5～9.5Wt%, and Ni is 0.1～5.8Wt%, and Mo is 2.5～10.0Wt%, and Ta is 3.0～9.0Wt%, and Cr is 1.0～10.0Wt%, and Zr is 4.0～15.0Wt%;
Surplus is Si.
A kind of high-temperature oxidation-resistant material is characterized in that, comprises following component:
Al is 2.0～8.0Wt%, and MoSi2 is 2.5～9.5Wt%, and Ni is 0.1～5.8Wt%, and Mo is 2.5～10.0Wt%, and Ta is 3.0～9.0Wt%, and Cr is 1.0～10.0Wt%, and Zr is 4.0～15.0Wt%;
And at least a in the following component
Fe is 1.5～4.0Wt%, and W is 1.0～4.0Wt%, and HfO2 is 0.1～1.5Wt%, and Ti is 0.1～3.0Wt%, and B is 0.1～2.5Wt%, and Y is 1.0～8.0Wt%, and V is 1.0～2.5Wt%;
Surplus is Si.
Further, high-temperature oxidation-resistant material is characterized in that, component is:
Al is 6.0Wt%, and MoSi2 is 8.0Wt%, and Ni is 5Wt%, and Mo is 8.0Wt%, and Ta is 3.4Wt%, and Cr is 8.5Wt%, and Zr is 7.5Wt%;
Fe is 1.5Wt%, and W is 3.0Wt%, and HfO2 is 1.2Wt%, and Ti is 0.5Wt%, and B is 2.0Wt%, and Y is 2.4Wt%, and V is 2.2Wt%;
Surplus is Si.
A kind of high-temperature oxidation resistant coating is characterized in that, can be prepared by following method:
To make granularity be 300 to 500 purpose powder and put into container to get aforementioned any one high-temperature oxidation-resistant material, use aforementioned powder volume 3-7 ethanol or pure water doubly to make carrier, add uniform mixing behind the sylvite of aforementioned powder quality 1.5～2.3% or the sodium salt, other adds behind the polyoxyethylene glycol of aforementioned powder quality 0.1～0.3% uniform mixing once more, make the coating slip, then this coating slip is coated on the base material, 1350 ℃～1650 ℃ of temperature, vacuum tightness is greater than fusing under 1.0 * 10-1Pa condition, be incubated 5-30 minute, can form high-temperature oxidation resistant coating.
Wherein sylvite or sodium salt are Repone K, sodium chloride, Potassium monofluoride or Sodium Fluoride.
Wherein base material is a niobium tungstenalloy base material.
Wherein coat-thickness is controlled at the 50-140 micron.
The coating of the high-temperature oxidation-resistant material preparation of technical solution of the present invention has following feature:
(1), coating has the good high-temperature oxidation-resistance: the life-span under high temperature (1600 ℃, 1700 ℃, 1800 ℃) is static is longer, and main test event is static, the thermal shock life-span in the air;
(2), coatingsurface is even, the coating microtexture: the coating of the present invention's development is formed (specifically seeing accompanying drawing 1) by four layers.Wherein 1 expression the first layer is so-called first blocking layer, is oxide compound; The 2 expression second layers i.e. second blocking layer are coated body, thus the layer growth oxide compound; 3 expressions are the 3rd blocking layer for the 3rd layer, are strengthening layer, are principal character and the gordian technique places that is different from general coating; 4 expressions are diffusion layer for the 4th layer, belong to internal diffusion stratotype coating.As these four layers of the blocking layer of oxygen, determined the quality and the life-span of coating usually.
(3), the coating main component is to contain different elementary composition intermetallic compounds such as Si, Y, this coating generates half vitreum at high-temperature oxidation resistant environment lower surface, plays the barrier function of oxygen.The oxide film formation speed is low, and has very strong defective self-healing ability.
(4), the niobium tungstenalloy after the coating not only has very strong high-temperature oxidation resistance and also keeps original excellent mechanical property simultaneously, and this niobium tungstenalloy afterwards coating performance is still good with the titanium alloy welding.
Description of drawings
Accompanying drawing 4 is the coatingsurface pattern of the embodiment of the invention 2.
Embodiment
According to coating system of the present invention and corresponding technology, prepared a kind of coating formula, count by weight percentage and contain the listed component of following table
Table 1 coating powder proportioning
To make granularity be 400 purpose powder and put into container will to go up the listed component of table, the dehydrated alcohol that adds 5 times of powder cumulative volumes is made carrier, add the sodium chloride that accounts for powder total mass 2.0% then, make its uniform mixing by stirring, other add account for powder total mass 0.2% polyoxyethylene glycol as binding agent, follow the coating powder to mix and grind, make the coating powder mix.The coating slip that configures is coated on the niobium tungstenalloy part, and coat-thickness is controlled at 100 microns, then 1500 ℃ of temperature, is incubated 30 minutes, and vacuum tightness is greater than 1 * 10
-1Fuse under the Pa condition, make coating prod at last.The coating prod that makes is carried out Performance Detection:
1) coatingsurface is observed and done metallurgical analysis, the coating after fusing presents the silver color of light, and surperficial metallurgical analysis shows that coated grains is even, is polynuclear plane, specifically sees accompanying drawing 2;
2) by the coating section is done probe analysis, this coating has tangible demixing phenomenon, specifically sees accompanying drawing 3;
3) coating life Performance Detection
In air, carry out 1700 ℃, 1800 ℃ of static continuously testeds, 1600 ℃-room temperature thermal shock performance test (when carrying out the thermal shock test, be warming up in 1600 ℃ and the temperature-fall period all be made as 18 seconds).
Specific performance sees the following form 2
Table 2 coating performance life tests
4) room-temperature mechanical property of base material and base material-coating, welding property are relatively
The room-temperature mechanical property of table 3 base material/base material-coating
| Test parameter (room temperature) | б b (Mpa) | б 0.2 (Mpa) | E (Gpa) | δ (％) | Hardness HV/5kg (M attitude) |
| The base material mechanical property | 512.2～525 | 385～430 | 90～117 | 21～25 | 168～187 |
| The substrate coating performance | 461～495 | 320～380 | 92～108 | 20～30.2 | 168～174 |
| The base material welding property | 460～490 | 350～420 | 96～114 | 21～26.3 | 179～186 |
| The welding coating performance | 455～487 | 324～418.4 | 89.4～97 | 24～31.4 | 186～197 |
5) mechanical behavior under high temperature of base material and base material-coating, welding property are relatively
Table 4 base material and base material-coating high-temp mechanical property
| 1600 ℃ of test parameters | Бb (Mpa) | б0.2 (Mpa) | E (Gpa) | δ (％) |
| The base material mechanical property | 112～115 | 97～103 | 70～75.1 | 35～45 |
| The base material welding property | 103～121 | 97～115.3 | 72～74.6 | 20.9～24 |
| The welding coating performance | 76.5～77.9 | 74.2～87 | 70～73 | 31.1～33.9 |
By the coating powder is optimized scope, count by weight percentage, see the following form:
Table 5 coating powder proportioning
To make granularity be 400 purpose powder and put into container will to go up the listed component of table, the pure water that adds 5 times of powder cumulative volumes is made carrier, add the Repone K that accounts for powder gross weight 2.0% then, make its uniform mixing by stirring, other add account for powder gross weight 0.2% polyoxyethylene glycol as binding agent, follow the coating powder to mix and grind, make the coating powder mix and abundant alloying.The coating slip that configures is coated on the niobium tungstenalloy part, and coat-thickness is controlled at 100 microns, then 1500 ℃ of temperature, is incubated 30 minutes, and vacuum tightness is greater than 1 * 10
-1Fuse under the Pa condition, make coating prod at last.The coating prod that makes is carried out Performance Detection:
1) coatingsurface is observed and done scanning electron microscope, the coating after fusing presents uniform grey, and scanning electron microscope is done on the surface, specifically sees accompanying drawing 4;
2) the anti-oxidant life tests of coating
By the anti-oxidant life performance of example two coatings is detected, 1700 ℃ of static propertiess of its high temperature are better than embodiment one coating performance.
The table 6 12# coating formula test life-span
Take off the matrix material of row component
MoSi
2Be 2.5Wt%, Mo is 2.5Wt%, and W is 1.0Wt%, HfO
2Be 0.1Wt%, Y is 1.0Wt%, and surplus is Si.
To make granularity be 300 purpose powder and put into container with above-mentioned matrix material, use the dehydrated alcohol of 3 times of aforementioned powder volume to make carrier, add uniform mixing behind the Repone K of aforementioned powder quality 1.5%, other adds the polyoxyethylene glycol of aforementioned powder quality 0.1%, make the coating slip, then this coating slip is coated on the niobium tungstenalloy base material, coat-thickness is controlled at 50 microns, 135 ℃ of temperature, vacuum tightness is greater than 1.0 * 10
-1Fuse under the Pa condition, be incubated 5 minutes, can form high-temperature oxidation resistant coating.
Take off the matrix material of row component
MoSi
2Be 9.5Wt%, Mo is 10.0Wt%, and W is 4.0Wt%, HfO
2Be 1.5Wt%, Y is 8.0Wt%, and surplus is Si.
To make granularity be 500 purpose powder and put into container with above-mentioned matrix material, use the pure water of 7 times of aforementioned powder volume to make carrier, add uniform mixing behind the sodium chloride of aforementioned powder quality 2.3%, other adds the polyoxyethylene glycol of aforementioned powder quality 0.3%, make the coating slip, then this coating slip is coated on the niobium tungstenalloy base material, coat-thickness is controlled at 140 microns, 1650 ℃ of temperature, vacuum tightness is greater than 1.0 * 10
-1Fuse under the Pa condition, be incubated 30 minutes, can form high-temperature oxidation resistant coating.
Embodiment 5
Take off the matrix material of row component
MoSi
2Be 5.5Wt%, Mo is 7.0Wt%, and W is 2.5Wt%, HfO
2Be 1.2Wt%, Y is 5.0Wt%, and surplus is Si.
To make granularity be 400 purpose powder and put into container with above-mentioned matrix material, use the pure water of 5 times of aforementioned powder volume to make carrier, add uniform mixing behind the Potassium monofluoride of aforementioned powder quality 1.9%, other adds the polyoxyethylene glycol of aforementioned powder quality 0.2%, make the coating slip, then this coating slip is coated on the niobium tungstenalloy base material, coat-thickness is controlled at 80 microns, 1500 ℃ of temperature, vacuum tightness is greater than 1.0 * 10
-1Fuse under the Pa condition, be incubated 20 minutes, can form high-temperature oxidation resistant coating.
Embodiment 6
Take off the matrix material of row component
Al is 2.0Wt%, MoSi
2Be 2.5Wt%, Ni is 0.1Wt%, and Mo is 2.5Wt%, and Ta is 3.0Wt%, and Cr is 1.0Wt%, and Zr is 4.0Wt%, and surplus is Si.
To make granularity be 300 purpose powder and put into container with above-mentioned matrix material, use the dehydrated alcohol of 3 times of aforementioned powder volume to make carrier, add uniform mixing behind the Repone K of aforementioned powder quality 1.5%, other adds the polyoxyethylene glycol of aforementioned powder quality 0.1%, make the coating slip, then this coating slip is coated on the niobium tungstenalloy base material, coat-thickness is controlled at 50 microns, 135 ℃ of temperature, vacuum tightness is greater than 1.0 * 10
-1Fuse under the Pa condition, be incubated 5 minutes, can form high-temperature oxidation resistant coating.
Embodiment 7
Take off the matrix material of row component
Al is 8.0Wt%, MoSi
2Be 9.5Wt%, Ni is 5.8Wt%, and Mo is 10.0Wt%, and Ta is 9.0Wt%, and Cr is 10.0Wt%, and Zr is 15.0Wt%, and surplus is Si.
To make granularity be 500 purpose powder and put into container with above-mentioned matrix material, use the pure water of 7 times of aforementioned powder volume to make carrier, add uniform mixing behind the sodium chloride of aforementioned powder quality 2.3%, other adds the polyoxyethylene glycol of aforementioned powder quality 0.3%, make the coating slip, then this coating slip is coated on the niobium tungstenalloy base material, coat-thickness is controlled at 140 microns, 1650 ℃ of temperature, vacuum tightness is greater than 1.0 * 10
-1Fuse under the Pa condition, be incubated 30 minutes, can form high-temperature oxidation resistant coating.
Embodiment 8
Take off the matrix material of row component
Al is 5.0Wt%, MoSi
2Be 6.5Wt%, Ni is 3.2Wt%, and Mo is 6.5Wt%, and Ta is 5.8Wt%, and Cr is 7.2Wt%, and Zr is 8.2Wt%, and surplus is Si.
To make granularity be 400 purpose powder and put into container with above-mentioned matrix material, use the pure water of 5 times of aforementioned powder volume to make carrier, add uniform mixing behind the Potassium monofluoride of aforementioned powder quality 1.9%, other adds the polyoxyethylene glycol of aforementioned powder quality 0.2%, make the coating slip, then this coating slip is coated on the niobium tungstenalloy base material, coat-thickness is controlled at 80 microns, 1500 ℃ of temperature, vacuum tightness is greater than 1.0 * 10
-1Fuse under the Pa condition, be incubated 20 minutes, can form high-temperature oxidation resistant coating.
In addition, the niobium tungstenalloy that uses among the above-mentioned whole embodiment of the present invention is the product of Dongfang Tantalum Industry Co., Ltd., Ningxia Hui autonomy Region.
Claims (7)
1, a kind of high-temperature oxidation-resistant material is characterized in that, component is:
Al is 2.0～8.0Wt%, MoSi
2Be 2.5～9.5Wt%, Ni is 0.1～5.8Wt%, and Mo is 2.5～10.0Wt%, and Ta is 3.0～9.0Wt%, and Cr is 1.0～10.0Wt%, and Zr is 4.0～15.0Wt%;
Surplus is Si.
2, a kind of high-temperature oxidation-resistant material is characterized in that, comprises following component:
Al is 2.0～8.0Wt%, MoSi
2Be 2.5～9.5Wt%, Ni is 0.1～5.8Wt%, and Mo is 2.5～10.0Wt%, and Ta is 3.0～9.0Wt%, and Cr is 1.0～10.0Wt%, and Zr is 4.0～15.0Wt%;
And at least a in the following component
Fe is 1.5～4.0Wt%, and W is 1.0～4.0Wt%, HfO
2Be 0.1～1.5Wt%, Ti is 0.1～3.0Wt%, and B is 0.1～2.5Wt%, and Y is 1.0～8.0Wt%, and V is 1.0～2.5Wt%;
Surplus is Si.
3, high-temperature oxidation-resistant material as claimed in claim 2 is characterized in that, component is:
Al is 6.0Wt%, MoSi
2Be 8.0Wt%, Ni is 5Wt%, and Mo is 8.0Wt%, and Ta is 3.4Wt%, and Cr is 8.5Wt%, and Zr is 7.5Wt%;
Fe is 1.5Wt%, and W is 3.0Wt%, HfO
2Be 1.2Wt%, Ti is 0.5Wt%, and B is 2.0Wt%, and Y is 2.4Wt%, and V is 2.2Wt%;
Surplus is Si.
4, a kind of high-temperature oxidation resistant coating is characterized in that, is prepared by following method:
The weighting profit requires in 1 to 3 any one high-temperature oxidation-resistant material to make granularity to be 300 to 500 purpose powder and to put into container, use aforementioned powder volume 3-7 ethanol or pure water doubly to make carrier, add uniform mixing behind the sylvite of aforementioned powder quality 1.5～2.3% or the sodium salt, other adds behind the polyoxyethylene glycol of aforementioned powder quality 0.1～0.3% uniform mixing once more, make the coating slip, then this coating slip is coated on the base material, 1350 ℃～1650 ℃ of temperature, vacuum tightness is greater than 1.0 * 10
-1Fuse under the Pa condition, be incubated 5-30 minute, can form high-temperature oxidation resistant coating.
5, high-temperature oxidation resistant coating as claimed in claim 4 is characterized in that:
Wherein sylvite or sodium salt are Repone K, sodium chloride, Potassium monofluoride or Sodium Fluoride.
6, high-temperature oxidation resistant coating as claimed in claim 4 is characterized in that:
Wherein base material is a niobium tungstenalloy base material.
7, high-temperature oxidation resistant coating as claimed in claim 4 is characterized in that:
Wherein coat-thickness is controlled at the 50-140 micron.
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| CN101962767B (en) * | 2010-10-26 | 2011-12-07 | 中国航天科技集团公司第五研究院第五一○研究所 | Electron beam cladding modification method for high-temperature preset coating |
| CN102061468B (en) * | 2011-01-24 | 2012-05-09 | 宁夏东方钽业股份有限公司 | High-temperature oxidation-resistant material and method for preparing high-temperature oxidation-resistant coating by using same |
| CN102719713B (en) * | 2012-07-10 | 2013-11-13 | 宁夏东方钽业股份有限公司 | High temperature oxidation-resistant material for low-density niobium alloy and method for preparing high temperature oxidation-resistant coating from high temperature oxidation-resistant material |
| CN104498941B (en) * | 2014-12-05 | 2017-06-20 | 宁夏东方钽业股份有限公司 | Molybdenum and molybdenum alloy high-temperature oxidation resistant coating and preparation method thereof |
| CN104561882B (en) * | 2015-01-30 | 2017-01-11 | 中国钢研科技集团有限公司 | High-temperature oxidation resistant coating on niobium alloy surface and preparation method of high-temperature oxidation resistant coating |
| CN104945023A (en) * | 2015-07-03 | 2015-09-30 | 苏州宏久航空防热材料科技有限公司 | High-temperature oxidation-resistant thermal-insulation composite ceramic coating |
| CN111872372B (en) * | 2020-08-04 | 2022-02-22 | 宁夏东方钽业股份有限公司 | Coating powder composition and method for preparing coating |
| CN113308689B (en) * | 2021-05-14 | 2022-07-05 | 宁夏东方钽业股份有限公司 | Niobium-tungsten alloy-Nb 6621 high-temperature oxidation-resistant coating material and preparation method thereof |
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