CN102719713A - 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 - Google Patents
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 Download PDFInfo
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- CN102719713A CN102719713A CN2012102370377A CN201210237037A CN102719713A CN 102719713 A CN102719713 A CN 102719713A CN 2012102370377 A CN2012102370377 A CN 2012102370377A CN 201210237037 A CN201210237037 A CN 201210237037A CN 102719713 A CN102719713 A CN 102719713A
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Abstract
The invention relates to a high temperature oxidation-resistant material for low-density niobium alloy and a method for preparing a high temperature oxidation-resistant coating from the high temperature oxidation-resistant material. The high temperature oxidation-resistant material is characterized by comprising the following components in weight percentage: 10-15wt% of Si, 2-3wt% of Ti, 1-2wt% of Mo, 0.8-1.2wt% of HfO2, 0.7- 0.9wt% of W and the balance of Al. The high temperature oxidation-resistant coating prepared from the high temperature oxidation-resistant material effectively solves the problem of severe oxidation of low-density niobium alloy in an atmospheric environment above 800-degree C, especially about 1100-degree C, keeps high-temperature mechanical properties of the low-density niobium alloy to the maximum extent, expands the application range of low-density niobium alloy and prolongs the service life of low-density niobium alloy; moreover, the high temperature oxidation-resistant coating prepared from the high temperature oxidation-resistant material has good high temperature oxidation resistance, a uniform coating surface and a dense microstructure.
Description
Technical field
The present invention relates to a kind of low density niobic alloy high temperature antioxidation material and prepare the method for high-temperature oxidation resistant coating by it.
Background technology
Low density niobium alloy: be a kind of niobium-titanium-aluminium-chromium alloy, have hot strength, working plasticity and middle temperature antioxidant property preferably.This low density niobium alloy is after C-103 and Nb521, and the novel aerospace that began to develop in the national military project scientific research project in 2006 are used the niobium alloy material, and the present domestic C-103 density of using is 8.86g/cm
3, Nb521 density is 8.9g/cm
3, and niobium-titanium-aluminium-chromium alloy density is 5.759g/cm
3About, be a kind of typical low density niobium-base alloy.Because of this alloy does not still have the trade mark at present, so claim the low density niobium alloy.
The low density niobium alloy is a kind of niobium-titanium-aluminium-chromium alloy, has good hot strength, working plasticity and low temperature antioxidant property, and the use temperature scope is 1100～1300 ℃.The project verification development in domestic 2006 of this alloy; Obtained certain achievement at present; Niobium-titanium-aluminium-chromium alloy is mainly used in the big area of rail control engine than jet pipe extension, about 1100 ℃ of working temperatures, and density is little, cost is low; Have good weldableness with other niobium-base alloy and titanium series alloy, and the advantage of early warning process is arranged when destroying.
The low density niobium-base alloy is good ultrahigh-temperature structured material, but in atmosphere, more than 800 ℃ vigorous oxidation can take place, and very fast l100 ℃ of following oxidation, this has seriously restricted the application of this alloy; Various countries have carried out a large amount of research to the anti-oxidation method of niobium-base alloy, and the result shows that the main path of the high-temperature oxidation resistance that improves niobium alloy has alloying protection and top coat protection.Alloying is a cost with loss intensity and processing characteristics normally, and it is very little to the mechanical property influence of alloy to add coating, and can significantly improve oxidation-resistance, tests the practicable approach that proves.
In actual use, be to solve the rapid problem of oxidation of low density niobium alloy under the high temperature, need a kind of high-temperature oxidation resistant coating that matches with it of development, for the real use of low density niobium alloy lays the foundation.The low density niobium alloy contains a large amount of light metal elements; The composition of this and other niobium alloy has very big difference; No matter traditional ORC is hot expansibility or all can't satisfies request for utilization with the bonding properties of base material, therefore must carry out the ORC development supporting with low density niobium alloy surface.
Low density niobium alloy material also has very big application value on aircraft engine, rocket ramjet and other heated component.See that from the material at high temperature performance low density niobium alloy is to be the material between the alloy between other high temperature niobium alloy and TiAl, the research and development of this material are for filling up the blank significant of domestic this field of materials.Therefore, for guaranteeing the successful use of this low density niobium alloy material, the high-temperature oxidation resistant coating that development matches with it is vital.
The low density niobium alloy is a kind of good functional structure material, is 60-80Mpa 1000 ℃ of tensile strength, and is carrying anti-oxidant function in the atmosphere below 800 ℃.Equally more than 800 ℃ be easy to oxidation with other tantalum, niobium, molybdenum, tungsten high temperature refractory; And the ultimate-use temperature of this alloy designs is at 900-1300 ℃; Thereby for of the application of Rapid Realization alloy at space industry; Must carry out oxidation protection to alloy surface and handle, wherein the surface preparation high-temperature oxidation resistant coating is the main path of low density niobic alloy high temperature antioxidation protection.
Summary of the invention
One of the object of the invention provides a kind of low density niobic alloy high temperature antioxidation material, and this material can be used in the coating that preparation has the good high-temperature oxidation-resistance;
Two of the object of the invention provides the method for the above-mentioned material prepn high-temperature oxidation resistant coating of a kind of usefulness, not only has very strong high-temperature oxidation resistance through the low density niobium alloy after the coating and has still kept its original excellent mechanical property simultaneously.
A kind of low density niobic alloy high temperature antioxidation material, its special feature is that component is by weight: Si is 10～15Wt%, and Ti is 2～3Wt%, and Mo is 1～2Wt%, HfO
2Be 0.8～1.2Wt%, W is 0.7～0.9Wt%, and surplus is Al.
A kind of low density niobic alloy high temperature antioxidation material, its special feature is that component is by weight: Si is 10～15Wt%, and Ti is 2～3Wt%, and Mo is 1～2Wt%, HfO
2Be 0.8～1.2Wt%, W is 0.7～0.9Wt%; And at least a in the following component: B is 0.5～2.5Wt%, and Ge is 1.5～2.5Wt%, and S is 0.25～0.45Wt%, and Fe is 1.2～4.0%, and Nb is 1.2～2.5Wt%; Surplus is Al.
Further, component is by weight: Si is 13Wt%, and Ti is 2.5Wt%, and Mo is 1.5Wt%, HfO
2Be 1Wt%, W is 0.8Wt%; And at least a in the following component: B is 1.5Wt%, and Ge is 2Wt%, and S is 0.30Wt%, and Fe is 3%, and Nb is 2Wt%; Surplus is Al.
A kind of method of low density niobic alloy high temperature antioxidation material prepn high-temperature oxidation resistant coating; Its special feature is, comprises the steps: that to require in 1 to 3 any described high-temperature oxidation-resistant material to process granularity be 350 to 550 purpose powder to the weighting profit and put into container, uses the ethanol or the pure water of 3～5 times of aforementioned powder volume to make carrier; Add uniform mixing behind sylvite or the sodium salt of aforementioned powder quality 1.5～3.5% again; Other adds behind the polyoxyethylene glycol of aforementioned powder quality 0.15～0.35% uniform mixing once more, makes the coating slip, then this slip is coated on the base material; 1200 ℃～1350 ℃ of temperature, vacuum is greater than 1.0 * 10
-1Fuse under the Pa condition, 10～30 minutes time, can form high-temperature oxidation resistant coating.
Wherein sylvite or sodium salt are sodium-chlor, Repone K, Potassium monofluoride or Sodium Fluoride.
Wherein base material is a low density niobium alloy base material.
Coat-thickness is controlled at 60～130 microns after wherein fusing moulding.
The invention provides a kind of low density niobic alloy high temperature antioxidation material and prepare the method for high-temperature oxidation resistant coating by it; Adopt the coating of this material prepn to efficiently solve the low density niobium alloy more than 800C; Especially 1100 ℃ of vigorous oxidation problems in the atmospheric environment up and down; And the composition of alloy can not change, and farthest keeps the mechanical behavior under high temperature of alloy, enlarges the low density niobium alloy scope of application simultaneously and prolongs its work-ing life.
Adopt the coating of high-temperature oxidation-resistant material preparation of the present invention to have following characteristic: (1) coating has the good high-temperature oxidation-resistance: the life-span under high temperature (1100 ℃, 1200 ℃, 1300 ℃) is static is longer, and main test event is static, the thermal shock life-span in the air.(2) coatingsurface is even, dense micro-structure; Through diffuseing to form transition layer, reached metallurgical binding between coating and the matrix; Under well-oxygenated environment, coatingsurface generates one deck glass coating protection matrix.(3) the coating staple is to contain different elementary composition intermetallic compounds such as Si, Al, and this coating generates half vitreum at high-temperature oxidation resistant environment lower surface, has stopped the erosion of oxygen, and has very strong defective self-healing ability.(4) the low density niobium alloy after the coating not only has very strong high-temperature oxidation resistance and still keeps its original excellent mechanical property simultaneously.
Embodiment
Embodiment 1:
High-temperature oxidation-resistant material, contain following component by weight percentage:
Nb:2Wt%, Si:13Wt%, B:1.5Wt%, Ge:2Wt%, Ti:2.5Wt%, S:0.30Wt%, Mo:1.5Wt%, HfO
2: 1Wt%, Fe:3%W:0.8Wt%, surplus is Al.
To process granularity be 450 purpose powder and put into container with above-mentioned listed component; Use the absolute ethyl alcohol of 4 times of aforementioned powder volume to make carrier; Add uniform mixing behind the sodium-chlor of aforementioned powder quality 2.5% again; Other add account for aforementioned powder total mass 0.25% polyoxyethylene glycol as sticker, mix with the coating powder and to adopt ball mill to grind to make slip in 5 hours.The coating slip is coated on the low density niobium alloy base material, and coat-thickness is controlled at 100 microns, and 1300 ℃ of temperature, vacuum is greater than 1 * 10 then
-1Fuse under the Pa condition, be incubated 25 minutes, make coating prod at last.The performance of the coating prod that makes is detected:
1, coatingsurface is observed and done metallurgical analysis, the coating after fusing presents silver gray, and surperficial metallurgical analysis shows that coated grains is even, compact structure.
2, through the coating section is done probe analysis, this coating structure is evenly distributed and at alloy surface pervious course is arranged, and forms metallurgical binding between the alloy.
3, coating life Performance Detection:
In air, carry out 1100 ℃, 1200 ℃, 1300 ℃ static continuously testeds, 1100 ℃-room temperature, the test of 1200 ℃-room temperature thermal shock performance.Concrete performance sees the following form 1.
Table 1 coating performance life tests
Embodiment 2:
Take off the matrix material of row component:
Si is 13Wt%, and Ti is 2.5Wt%, and Mo is 1.5Wt%, HfO
2Be 1Wt%, W is 0.8Wt%, and surplus is Al.
Above-mentioned matrix material is processed granularity 400 purpose powder and put into container, use the absolute ethyl alcohol of 3.5 times of aforementioned powder volume to make carrier, add uniform mixing behind the Repone K of aforementioned powder quality 3.0%; Other adds behind the polyoxyethylene glycol of aforementioned powder quality 0.3% uniform mixing once more; Adopt ball mill grinding to make the coating slip in 4 hours, then this coating slip is coated on the low density niobium alloy base material, coat-thickness is controlled at 80 microns; 1350 ℃ of temperature, vacuum is greater than 1 * 10
-1Fuse under the Pa condition, be incubated 15 minutes, can form high-temperature oxidation resistant coating.
Embodiment 3:
Take off the matrix material of row component:
B is 0.5Wt%, and Si is 10Wt%, and Ti is 2Wt%, and Ge is 1.5Wt%, and Mo is 1Wt%, HfO
2Be 0.8Wt%, W is 0.7Wt%, and S is 0.25Wt%, and surplus is Al.
Above-mentioned matrix material is processed granularity 350 purpose powder and put into container, use the absolute ethyl alcohol of 3 times of aforementioned powder volume to make carrier, add uniform mixing behind the sodium-chlor of aforementioned powder quality 1.5%; Other adds behind the polyoxyethylene glycol of aforementioned powder quality 0.15% uniform mixing once more; Adopt ball mill grinding to make the coating slip in 3 hours, then this coating slip is coated on the low density niobium alloy base material, coat-thickness is controlled at 60 microns; 1200 ℃ of temperature, vacuum is greater than 1 * 10
-1Fuse under the Pa condition, be incubated 10 minutes, can form high-temperature oxidation resistant coating.
Embodiment 4:
Take off the matrix material of row component:
Nb is 2.5Wt%, and Si is 15Wt%, and B is 2.5Wt%, and Ti is 3Wt%, and Fe is 4.0%, and Mo is 2Wt%, HfO
2Be 1.2Wt%, W is 0.9Wt%, and surplus is Al.
Above-mentioned matrix material is processed granularity 550 purpose powder and put into container, 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 3.5%; Other adds behind the polyoxyethylene glycol of aforementioned powder quality 0.35% uniform mixing once more; Adopt ball mill grinding to make the coating slip in 6 hours, then this coating slip is coated on the low density niobium alloy base material, coat-thickness is controlled at 130 microns; 1350 ℃ of temperature, vacuum is greater than 1 * 10
-1Fuse under the Pa condition, be incubated 30 minutes, can form high-temperature oxidation resistant coating.
Claims (7)
1. low density niobic alloy high temperature antioxidation material, it is characterized in that component is by weight: Si is 10～15Wt%, and Ti is 2～3Wt%, and Mo is 1～2Wt%, HfO
2Be 0.8～1.2Wt%, W is 0.7～0.9Wt%, and surplus is Al.
2. low density niobic alloy high temperature antioxidation material, it is characterized in that component is by weight: Si is 10～15Wt%, and Ti is 2～3Wt%, and Mo is 1～2Wt%, HfO
2Be 0.8～1.2Wt%, W is 0.7～0.9Wt%; And at least a in the following component: B is 0.5～2.5Wt%, and Ge is 1.5～2.5Wt%, and S is 0.25～0.45Wt%, and Fe is 1.2～4.0%, and Nb is 1.2～2.5Wt%; Surplus is Al.
3. a kind of low density niobic alloy high temperature antioxidation material as claimed in claim 2, it is characterized in that component is by weight: Si is 13Wt%, and Ti is 2.5Wt%, and Mo is 1.5Wt%, HfO
2Be 1Wt%, W is 0.8Wt%; And at least a in the following component: B is 1.5Wt%, and Ge is 2Wt%, and S is 0.30Wt%, and Fe is 3%, and Nb is 2Wt%; Surplus is Al.
4. the method for a low density niobic alloy high temperature antioxidation material prepn high-temperature oxidation resistant coating; It is characterized in that, comprise the steps: that to require in 1 to 3 any described high-temperature oxidation-resistant material to process granularity be 350 to 550 purpose powder to the weighting profit and put into container, uses the ethanol or the pure water of 3～5 times of aforementioned powder volume to make carrier; Add uniform mixing behind sylvite or the sodium salt of aforementioned powder quality 1.5～3.5% again; Other adds behind the polyoxyethylene glycol of aforementioned powder quality 0.15～0.35% uniform mixing once more, makes the coating slip, then this slip is coated on the base material; 1200 ℃～1350 ℃ of temperature, vacuum is greater than 1.0 * 10
-1Fuse under the Pa condition, 10～30 minutes time, can form high-temperature oxidation resistant coating.
5. the method for a kind of low density niobic alloy high temperature antioxidation material prepn high-temperature oxidation resistant coating as claimed in claim 4 is characterized in that: wherein sylvite or sodium salt are sodium-chlor, Repone K, Potassium monofluoride or Sodium Fluoride.
6. the method for a kind of low density niobic alloy high temperature antioxidation material prepn high-temperature oxidation resistant coating as claimed in claim 4 is characterized in that: wherein base material is a low density niobium alloy base material.
7. the method for a kind of low density niobic alloy high temperature antioxidation material prepn high-temperature oxidation resistant coating as claimed in claim 4 is characterized in that: coat-thickness is controlled at 60～130 microns after wherein fusing moulding.
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| CN103949643A (en) * | 2014-05-16 | 2014-07-30 | 西安建筑科技大学 | Cladding method for preventing molybdenum and molybdenum alloy from being oxidized |
| CN103981383A (en) * | 2014-05-23 | 2014-08-13 | 西安瑞科新材料科技有限公司 | Method for preparing low-oxygen molybdenum and molybdenum alloy clad with Al4SiC4-HfC |
| CN105112915A (en) * | 2015-04-30 | 2015-12-02 | 宁夏东方钽业股份有限公司 | Oxidation-resistant material and method employing same for preparing tantalum-tungsten alloy anti-oxidation coating |
| CN105599382A (en) * | 2015-12-23 | 2016-05-25 | 常熟市东方特种金属材料厂 | Compound anti-oxidative special metal material |
| CN106242643A (en) * | 2016-07-28 | 2016-12-21 | 航天材料及工艺研究所 | A kind of resistance to 1,300 1500 DEG C of low density carbon watt surface oxidation-resistant coatings and preparation method thereof |
| CN111885847A (en) * | 2020-07-24 | 2020-11-03 | 苏州浪潮智能科技有限公司 | Manufacturing method of PCB, PCB and electronic equipment |
| CN114892163A (en) * | 2022-05-09 | 2022-08-12 | 宁夏东方钽业股份有限公司 | High-temperature antioxidant protective coating material, preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103949643A (en) * | 2014-05-16 | 2014-07-30 | 西安建筑科技大学 | Cladding method for preventing molybdenum and molybdenum alloy from being oxidized |
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| CN103981383A (en) * | 2014-05-23 | 2014-08-13 | 西安瑞科新材料科技有限公司 | Method for preparing low-oxygen molybdenum and molybdenum alloy clad with Al4SiC4-HfC |
| CN105112915A (en) * | 2015-04-30 | 2015-12-02 | 宁夏东方钽业股份有限公司 | Oxidation-resistant material and method employing same for preparing tantalum-tungsten alloy anti-oxidation coating |
| CN105599382A (en) * | 2015-12-23 | 2016-05-25 | 常熟市东方特种金属材料厂 | Compound anti-oxidative special metal material |
| CN106242643A (en) * | 2016-07-28 | 2016-12-21 | 航天材料及工艺研究所 | A kind of resistance to 1,300 1500 DEG C of low density carbon watt surface oxidation-resistant coatings and preparation method thereof |
| CN106242643B (en) * | 2016-07-28 | 2019-01-25 | 航天材料及工艺研究所 | A kind of resistance to 1300-1500 DEG C of low density carbon watt surface oxidation-resistant coating and preparation method thereof |
| CN111885847A (en) * | 2020-07-24 | 2020-11-03 | 苏州浪潮智能科技有限公司 | Manufacturing method of PCB, PCB and electronic equipment |
| CN114892163A (en) * | 2022-05-09 | 2022-08-12 | 宁夏东方钽业股份有限公司 | High-temperature antioxidant protective coating material, preparation method and application |
| CN114892163B (en) * | 2022-05-09 | 2023-11-21 | 宁夏东方钽业股份有限公司 | High-temperature antioxidant protective coating material, preparation method and application |
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