CN101818302A - Mo-containing bulk nanocrystalline Fe3Al material and preparation method thereof - Google Patents
Mo-containing bulk nanocrystalline Fe3Al material and preparation method thereof Download PDFInfo
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- CN101818302A CN101818302A CN200910117703A CN200910117703A CN101818302A CN 101818302 A CN101818302 A CN 101818302A CN 200910117703 A CN200910117703 A CN 200910117703A CN 200910117703 A CN200910117703 A CN 200910117703A CN 101818302 A CN101818302 A CN 101818302A
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Abstract
The invention relates to a Mo-containing bulk nanocrystalline Fe3Al material and a preparation method thereof. The Mo-containing bulk nanocrystalline Fe3Al material comprises the following components of by weight percent: 11 to 14% of Al, 68 to 85% of Fe and 2 to 15% of Mo. The preparation method comprises the following steps of: preparing a powdered material according to the components, placing the powdered material in a planetary ball mill for mixing for 16 hours, then placing the mixed reaction material to a copper mould provided with a copper substrate to be pressed by a press machine at the pressure of 60 MPa, placing an ignition agent on the surface, reacting the reaction material in a thermit reaction vessel, blowing the reaction vessel for exhausting the air therein by argon at the room temperature, exhausting the air again when the temperature of the vessel raises to 180 DEG C, and then introducing the argon with the pressure of 7 MPa, and continuously raising the temperature of the vessel. When the temperature in the vessel reaches about 260 DEG C, the ignition agent starts reaction and releases a large amount of heat, thereby triggering the reaction among the reaction materials. The gain size of the obtained material is 15 to 35 nanometers.
Description
Technical field
The present invention relates to the bulk nano-crystalline material technology of preparing.
Background technology
Improve the room temperature fragility of Fe-Al series intermetallic compound, improve its intensity, it is an important research direction, it has been generally acknowledged that alloying is to improve one of brittle effective means of Fe-Al series intermetallic compound room temperature, the interpolation of alloying element also can effectively improve the temperature-room type plasticity of intermetallic compound, middle hot strength and creep resistance.For further improving Fe
3The intensity of Al is improved plasticity, to Fe
3Al carries out alloying, and wherein alloy element can be divided into two classes: a class is the element of solid solution effect, and another kind of is not have or the element of solid solution seldom.Mo improves Fe
3Al alloy high-temp intensity is effective elements the most, simultaneously, adds Mo and will make Fe
3The grain refining of Al alloy is separated out particle and is distributed in mutually in the matrix, improves the hot strength of alloy effectively.
The nanometer of grain-size also is expected to solve its ubiquitous room temperature fragility problem.Along with nearly decades nano material technology constantly full-fledged, the various countries investigator is considering to utilize nano material technology further to solve the problems such as room temperature fragility of intermetallic compound.But traditional heat pressing process from nano particle exists technology of preparing complexity, cost height, quality of materials not high (for example having a large amount of cavities the material), particle nano-scale to be difficult to shortcomings such as maintenance.And the gross distortion method that grow up recent years is difficult to obtain the material of grain-size less than 100nm, and is confined to metallic substance substantially.Therefore, also do not have so far a kind of obtain the block nanometer structured material easy, cost is low and the technology of scalable suitability for industrialized production, this problem seriously hampers the Research And Engineering of nanocrystalline material and uses.
Thermite reaction fusing preparation bulk nano-crystalline material method is a kind of relatively more novel, with low cost and the potentiality of amplification suitability for industrialized production are arranged, the principle of this technology is: at the synthetic required intermetallic compound of aluminothermy chemical reaction that passes through under the low outside temperature between the oxide compounds such as aluminium powder body and iron, nickel, intermetallic compound is melted under the instantaneous high calorie effect that reaction discharges self simultaneously, have the common melting technology superheating temperature (about 1000 ℃) that is beyond one's reach, make melt at first be crossed thermal purification.By the control material purity, under protective atmosphere, react, melt in situ is deposited on the cooling ground, keep the melt purity.Thereby melt has bigger condensate depression in process of setting, guarantees to have little critical nucleus when crystallization begins, high nucleation rate and low atomic diffusion speed.Simultaneously melt is solidified under the higher speed of cooling effect that is in than the high heat conduction egative film of low ambient temperature, melt nucleus growth time in crystallisation process is restricted, the nucleus size is finally hindered at nano-scale in the material thereby solidify when finishing, and obtains the intermetallic compound bulk nano-crystalline material.
The present invention designs different molybdenum content and has prepared three combination gold by thermite reaction, and material composition is (mass percent), Al:11-14%, Fe:68-85%, Mo:2-15%.Experimental raw is selected Powdered, molten alloy in the thermite reaction stove.
Summary of the invention
The bulk nano-crystalline Fe that the purpose of this invention is to provide a kind of Mo of containing
3Al material and preparation method thereof.
The present invention is the bulk nano-crystalline Fe that contains Mo
3Al material and preparation method thereof, by mass percentage, its composition is Al:11～14%, Fe:68～85%, Mo:2～15%.
Be ready to dusty material according to the above composition, putting into planetary ball mill mixed 16 hours, then the reaction mass that mixes is placed the copper mould of being furnished with the copper ground and use pressing machine compacting under the pressure of 60MPa, put detonator on its surface, in the thermite reaction container, react then, with argon purge reaction vessel eliminating air wherein, wait until exhaust once more when vessel temp rises to 180 ℃ under the room temperature, the argon gas that feeds 7MPa then continues the rising vessel temp.Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thus the reaction of initiation reaction storeroom, and the grain-size of gained material is 15～35 nanometers.
Performances more of the present invention such as following table:
Compression experiment carries out ultimate load 10t, pressure head speed 0.5mm/min on " microcomputer control polarity formula universal testing machine " that Shijin Group Co., Ltd., Jinan produces; Hardness is measured on HBRVU-187.5 type Bu Luoweishi optics sclerometer, and its test condition is that load 298N loads time length 15s; Grain-size is by the X diffraction experiment, and diffraction angle is the 5-100 degree, and the JEOL-2010 transmission electron microscope observing, the highest acceleration voltage 200kv, magnification 100k times, lattice resolution 0.194nm.The grain-size and the performance perameter of material are as shown in table 1.
Table 1 contains the Fe of Mo
3The grain-size of Al material and mechanical property
| Performance | Yield strength σ 0.2??(MPa) | Ultimate compression strength (MPa) | Vickers' hardness (HV) | Grain-size (nm) |
| Material of the present invention | ??500～1000 | ??1000～1500 | ??200～500 | ??15～35 |
These above-mentioned performance indexs are all carried out in strict accordance with national standard.
The invention has the beneficial effects as follows that at the block Fe-Al-Mo material that obtains nanocrystalline grain size, the cost of material preparation simultaneously is lower.
Embodiment:
Embodiment 1:
Be Al:30.1%, Fe according to prescription (quality percentage composition)
2O
3: 66.9%, Mo:3.0%, raw material is Powdered, take by weighing corresponding quality, the powder that weighs up was mixed in planetary ball mill 16 hours, then the reaction mass that mixes is placed the copper mould of being furnished with the copper ground and use pressing machine compacting under the pressure of 60MPa, put detonator on its surface, in the thermite reaction container, react then, use argon purge reaction vessel eliminating air wherein under the room temperature, exhaust once more when vessel temp rises to 180 ℃ by the time, the argon gas that feeds 7MPa then continues the rising vessel temp.Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thus the reaction of initiation reaction storeroom.Be reflected in a few times in second and finish, the product of generation cools to room temperature with the furnace and makes alloy under argon shield.The alloy ingredient that obtains is (mass percent), Al:13.1%, Fe:81.9%, Mo:5.0%.Performance data: hardness (HV): 329, yield strength: σ
0.2=590.3Mpa, ultimate compression strength: 1095.6Mpa, grain-size: 19nm.
Embodiment 2:
Be Al:29.2%, Fe according to prescription (quality percentage composition)
2O
3: 64.9%, Mo:5.9%, raw material is Powdered, take by weighing corresponding quality, the powder that weighs up was mixed in planetary ball mill 16 hours, put detonator on its surface, then the reaction mass that mixes is placed the copper mould of being furnished with the copper ground and use pressing machine compacting under the pressure of 60MPa, in the thermite reaction container, react, use argon purge reaction vessel eliminating air wherein under the room temperature, exhaust once more when vessel temp rises to 180 ℃ by the time, the argon gas that feeds 7MPa then continues the rising vessel temp.Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thus the reaction of initiation reaction storeroom.Be reflected in a few times in second and finish, the product of generation cools to room temperature with the furnace and makes alloy under argon shield.The alloy ingredient that obtains is (mass percent), Al:12.5%, Fe:77.5%, Mo:10.0%.Performance data: hardness (HV): 261.0, yield strength: σ
0.2=903.5Mpa, ultimate compression strength: 1385.2Mpa, grain-size: 31.5nm.
Embodiment 3:
Be Al:28.2%, Fe according to prescription (quality percentage composition)
2O
3: 62.8%, Mo:9.0%, raw material is Powdered, take by weighing corresponding quality, the powder that weighs up was mixed in planetary ball mill 16 hours, put detonator on its surface, then the reaction mass that mixes is placed the copper mould of being furnished with the copper ground and use pressing machine compacting under the pressure of 60MPa, in the thermite reaction container, react, use argon purge reaction vessel eliminating air wherein under the room temperature, exhaust once more when vessel temp rises to 180 ℃ by the time, the argon gas that feeds 7MPa then continues the rising vessel temp.Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thus the reaction of initiation reaction storeroom.Be reflected in a few times in second and finish, the product of generation cools to room temperature with the furnace and makes alloy under argon shield.The alloy ingredient that obtains is (mass percent), Al:11.8%, Fe:73.2%, Mo:15.0%.Performance data: hardness (HV): 335.0, yield strength: σ
0.2=802.1Mpa, ultimate compression strength: 1148.0Mpa, grain-size: 17.3nm.
Embodiment 4:
Be Al:30.7%, Fe according to prescription (quality percentage composition)
2O
3: 68.2%, Mo:1.1%, raw material is Powdered, take by weighing corresponding quality, the powder that weighs up was mixed in planetary ball mill 16 hours, put detonator on its surface, then the reaction mass that mixes is placed the copper mould of being furnished with the copper ground and use pressing machine compacting under the pressure of 60MPa, in the thermite reaction container, react, use argon purge reaction vessel eliminating air wherein under the room temperature, exhaust once more when vessel temp rises to 180 ℃ by the time, the argon gas that feeds 7MPa then continues the rising vessel temp.Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thus the reaction of initiation reaction storeroom.Be reflected in a few times in second and finish, the product of generation cools to room temperature with the furnace and makes alloy under argon shield.The alloy ingredient that obtains is (mass percent), Al:13.6%, Fe:84.4%, Mo:2%.Performance data: hardness (HV): 416.0, yield strength: σ
0.2=771Mpa, ultimate compression strength: 1032.0Mpa, grain-size: 17.8nm.
Claims (2)
1. the bulk nano-crystalline Fe that contains Mo
3The Al material, by mass percentage, its composition is Al:11～14%, Fe:68～85%, Mo:2～15%.
2. the bulk nano-crystalline Fe that contains Mo
3The Al material preparation method, be ready to dusty material according to the described composition of claim 1, putting into planetary ball mill mixed 16 hours, then the reaction mass that mixes is placed the copper mould of being furnished with the copper ground and use pressing machine compacting under the pressure of 60MPa, put detonator on its surface, in the thermite reaction container, react then, use argon purge reaction vessel eliminating air wherein under the room temperature, exhaust once more when vessel temp rises to 180 ℃ by the time, the argon gas that feeds 7MPa then continues the rising vessel temp.Detonator begins to react and discharge a large amount of heat when temperature in the container reaches 260 ℃ of left and right sides, thus the reaction of initiation reaction storeroom, and the grain-size of gained material is 15～35 nanometers.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534279A (en) * | 2012-01-20 | 2012-07-04 | 北京科技大学 | In situ reaction hot-pressing method for manufacturing intermetallic compound T2 phase alloys |
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2009
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534279A (en) * | 2012-01-20 | 2012-07-04 | 北京科技大学 | In situ reaction hot-pressing method for manufacturing intermetallic compound T2 phase alloys |
| CN102534279B (en) * | 2012-01-20 | 2014-04-16 | 北京科技大学 | In situ reaction hot-pressing method for manufacturing intermetallic compound T2 phase alloys |
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Open date: 20100901 |