CN1865478A - Process for preparing high performance Fe3Al-base composite materials - Google Patents

Process for preparing high performance Fe3Al-base composite materials Download PDF

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Publication number
CN1865478A
CN1865478A CN 200610011512 CN200610011512A CN1865478A CN 1865478 A CN1865478 A CN 1865478A CN 200610011512 CN200610011512 CN 200610011512 CN 200610011512 A CN200610011512 A CN 200610011512A CN 1865478 A CN1865478 A CN 1865478A
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powder
sintering
ball mill
ball
alc
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贾成厂
何箐
孟杰
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

The invention discloses a high-property Fe2Al base composite material preparing method in the metal composition base material domain, which comprises the following steps: blending 80-70 at percent Fe and 20-30 at percent Al; milling in the high-energy ball grinder for 1-20 min; setting the ball grinding dielectric as organic liquid without water; loading the grinded powder in the mould to sinter in the discharge plasma sintering equipment; setting the sintering speed at 5-200 deg.c per min at 900-1100 deg.c for 1-10 min; pressing 1-100 Mpa pressure; cooling to indoor temperature. The bent strength of Fe3Al-Fe3AlC0.5 composite material can reach 2500 Mpa, whose relative density is more than 99.9 percent.

Description

A kind of preparation high performance Fe 3The method of Al based composites
Technical field
The invention belongs to the intermetallic compound based composite material preparing technical field, a kind of preparation high performance Fe particularly is provided 3The method of Al based composites.
Background technology
Fe 3The Al intermetallic compound has high strength, low cost, low density, good mechanical behavior under high temperature and cheap cost (not containing strategic element), simultaneously it has good anticorrosive, sulfidation corrosion and antioxidant property, therefore has application promise in clinical practice at high-temperature structural material and some special dimension.Abroad, because therefore its excellent performance is " stainless steel that the poor afford to use " by person.But because Fe 3The room temperature fragility of Al intermetallic compound and be difficult to processing characteristics, make it still not have a large amount of commercial applications, in recent years, the researchist has carried out a large amount of research to its alloying, technology of preparing and related compound material, in the hope of improving its room temperature fragility and being difficult to processing characteristics.The interpolation of C element can be at Fe 3Generate hard crisp phase Fe among the Al 3AlC 0.5, the generation of this cenotype can improve Fe 3The intensity of Al intermetallic compound, creep resistance, environment hydrogen embrittlement and workability.
This matrix material is with Fe 3Al is the matrix phase, and alloying element C is except can the gap strengthening and suppress the grain growth, simultaneously can also and the matrix effect generate Fe 3AlC 0.5As being the precipitation strength phase.Data shows: matrix mutually in C content within the specific limits the time, Fe 3The hardness of Al and intensity all rise with the rising of C content, the obvious refinement of the crystal grain of this alloy simultaneously, and hot workability is obviously improved.(see: Zhang Yonggang, Han Yafang, chief editors such as Chen Guoliang. the intermetallic compound structure material. National Defense Industry Press. Beijing, 2001,890.)
Prepare Fe at present 3The method of Al intermetallic compound mainly is fusion casting and powder metallurgic method, adopts that traditional fusion casting cost is low, efficient is high, but in the fusion-casting process Al very easily reaction forms hydrogen ion with steam, the as-cast structure crystal grain that obtains simultaneously is thick, component segregation, temperature-room type plasticity is low, and fragility is big; In addition, be easy to generate shrinkage cavity or shrinkage porosite, produce tiny crack, the performance of foundry goods is reduced.Simultaneously this method following process difficulty, cost are higher.The powder metallurgy process preparation mainly contains hot pressing, hot isostatic pressing, discharge plasma sintering and mechanical alloying etc., because powder metallurgic method has the preparation complicated shape, characteristics such as few cutting output in the course of processing, goods composition are even are so this respect has carried out more research.For Fe 3Al-Fe 3AlC 0.5Matrix material adopts above two kinds of methods all to need to solve Fe 3AlC 0.5Distribution and interface pollution problem, how to make Fe 3AlC 0.5Be evenly distributed on Fe after the generation 3Al crystal boundary and bonding interface are pollution-free to be the emphasis direction of research.
Mechanical alloying is a kind of high-energy ball-milling process, it is the element powders mechanically mixing according to a certain ratio that to desire alloying, running for a long time in equipment such as high energy ball mill, pass through abrading-ball, strong interaction between powder and the spherical tank, external energy is delivered in element powders or the intermetallic compound powder particle, powder is under the collision repeatedly of ball-milling medium, withstand shocks, shear, friction and compress the effect of multiple power, through extruding repeatedly, cold welding and pulverizing, the obvious like this contact area that increases reaction, shortened the diffusion length of atom, impel diffusion and solid state reaction take place between the heterogeneity, mixed powder is realized alloying on atom magnitude level, form alloy powder.(see: Wang Qingxue, open alliance. mechanical alloying---novel solid-state non-equilibrium processing technology. Chinese pottery .2002,38 (2): 36.)
The sintering process of powdered alloy mainly contains hot pressing, hot extrusion, hot isostatic pressing, discharge plasma sintering etc.Wherein discharge plasma sintering is a kind of Fast Sintering novel process.Moment, interrupted, high energy pulse electric current are fed and be equipped with on the mould of powder, between powder particle, can produce plasma discharge, cause the effects such as purification, activation, homogenizing of powder.This sintering method has following characteristics: (1) sintering temperature is low, and sintering time is short, can obtain tiny, uniform tissue, and can keep the state of nature of starting materials; (2) can obtain high compactedness material; (3), can be similar to material with complex such as gradient material and large-scale workpiece by sintering by control sintering component and technology.(Luo Xiyu. the latest developments of discharge plasma sintering material. powder metallurgy industry .2001,11 (6): 7.)
Summary of the invention
The object of the present invention is to provide a kind of preparation high performance Fe 3The method of Al based composites has solved composite material reinforcement body Fe 3AlC 0.5At Fe 3Al crystal boundary place's uniform distribution and with matrix Fe 3Interface between Al obtains comparatively excellent tissue and performance simultaneously in conjunction with problem such as pollution-free.
The present invention prepares Fe 3Al-Fe 3AlC 0.5The technology of matrix material is: with Fe powder, Al powder is raw material, and pure Fe powder, Al powder are pressed composition Fe (80~70), and Al (20~30) (at%) mixes, and ball milling 5~15min in high energy ball mill, ball-milling medium are anhydrous organic liquid.Powder behind the ball milling is put into mould, carries out sintering on the discharge plasma sintering machine.Be incubated 1~10min after being warming up to 900~1100 ℃ with the speed of 5~200 ℃/min in the sintering process, apply the pressure of 1~100MPa simultaneously, utilize water quench then to room temperature.Can avoid introducing too much elemental oxygen in the short period of time ma process, increase the reactive behavior of powder simultaneously by high-energy ball milling, in the sintering process, at high temperature, the C atom in the used graphite jig evenly is diffused in the sample, and Fe 3The Al reaction generates Fe 3AlC 0.5After sintering is finished, the Fe of disperse 3AlC 0.5Can be evenly distributed in Fe 3The crystal boundary place of Al, simultaneously, owing to be that the C element at high temperature reacts Fe with matrix 3Al and Fe 3AlC 0.5Pollution-free at the interface.Thereby prepare high performance Fe 3Al-Fe 3AlC 0.5Matrix material.
The present invention also can add B powder 0.01~0.5at%, Cr powder 0.5%~2at% in addition in Fe powder, Al powder raw material.
Anhydrous organic liquid of the present invention is dehydrated alcohol or sherwood oil.Described high energy ball mill is oscillatory type ball mill, planetary ball mill or stirring ball mill.
The invention has the advantages that:
1, can prepare strengthening phase Fe 3AlC 0.5Content is the Fe of 2%~5% (volume fraction), homogeneous microstructure 3Al-Fe 3AlC 0.5Matrix material.The room temperature flexural strength of matrix material reaches 2500MPa, and relative density is greater than 99.9%.Utilize high-energy ball milling technology, increased the reactive behavior of powder, utilize in the sintering process etc. the effect of exsomatizing make the C atom evenly diffusion and matrix react, be easy to prepare have high-performance, the Fe of even compact tissue 3Al-Fe 3AlC 0.5Matrix material.
2, the present invention has simple, the easy handling of preparation technology, characteristics such as material property height.
Embodiment
Embodiment 1: ball milling 5min powder is at 1050 ℃ of discharge plasma sinterings
Raw material: Fe powder (<74 μ m) 50.000g, Al powder (<74 μ m) 7.366g.
Behind above-mentioned raw materials powder thorough mixing, take by weighing the 10g mixed powder and pack in the stainless steel jar mill, add abrading-ball, ratio of grinding media to material is 10: 1, adds the 1ml dehydrated alcohol again, the start ball milling, behind the ball milling 5min, separated powder and abrading-ball, powder is air-dry.Powder behind the ball milling 5min places graphite jig, is incubated 5min after being warming up to 1050 ℃ of sintering temperatures with the speed of 100 ℃/min, applies the pressure of 50MPa simultaneously.Density of material is 6.60g/cm behind the sintering 3, Fe 3AlC 0.5Volume fraction be 2.37%.This composite hardness 410Hv0.05, flexural strength: 1600MPa.Under opticmicroscope and scanning electron microscope, all can be observed Fe 3AlC 0.5Be distributed in Fe 3Al crystal boundary place.
Embodiment 2: ball milling 15min powder is at 1000 ℃ of discharge plasma sinterings
Raw material: with embodiment 1.Behind the raw material powder thorough mixing, take by weighing the 10g mixed powder and pack in the stainless steel jar mill, add abrading-ball, ratio of grinding media to material is 10: 1, adds the 1ml sherwood oil again, grind afterwards separated powder and abrading-ball, powder is air-dry.Powder behind the ball milling 10min places graphite jig, is incubated 5min after being warming up to 1000 ℃ of sintering temperatures with the speed of 100 ℃/min, applies the pressure of 40MPa simultaneously.Density of material is 6.55g/cm behind the sintering 3, Fe 3AlC 0.5Volume fraction be 2.81%.This composite hardness 566Hv0.05, flexural strength: 1500MPa.
Embodiment 3: ball milling 10min powder is at 1050 ℃ of discharge plasma sinterings
Raw material: Fe powder (2~3 μ m) 50.000g, Al powder (<74 μ m) 7.421g, B powder (2~3 μ m) 0.106g.
Behind the raw material powder thorough mixing, take by weighing the 10g mixed powder and pack in the stainless steel jar mill, add abrading-ball, ratio of grinding media to material is 10: 1, adds the 1ml dehydrated alcohol again, grind separation dried powder afterwards.Powder behind the ball milling 120min places graphite jig, is incubated 5min after being warming up to 1050 ℃ of sintering temperatures with the speed of 100 ℃/min, applies the pressure of 50MPa simultaneously.Density of material is 6.51g/cm behind the sintering 3, Fe 3AlC 0.5Volume fraction be 3.01%, the average grain size of matrix is about 15 μ m.This composite hardness 623Hv0.05, flexural strength: 2140MPa.Can observe Fe from metallograph 3AlC 0.5Be distributed in Fe 3The crystal boundary place of Al matrix.

Claims (4)

1, a kind ofly prepares Fe with powder metallurgical technique 3Al-Fe 3AlC 0.5The method of matrix material, it is characterized in that: with pure Fe powder and Al powder is raw material, pure Fe powder, Al powder are pressed composition Fe:80~70at%, Al:20~30at% mixes, ball milling 5~15min in high energy ball mill, ball-milling medium is anhydrous organic liquid, and the powder behind the ball milling is put into mould and carry out sintering on the discharge plasma sintering machine; Be incubated 1~10min after being warming up to 900~1100 ℃ with the speed of 5~200 ℃/min in the sintering process, the 1~100MPa that exerts pressure simultaneously is cooled to room temperature then.
2, method according to claim 1 is characterized in that: add the B powder of 0.01~0.5at%, the Cr powder of 0.5%~2at% in raw material in addition.
3, method according to claim 1 is characterized in that: described anhydrous organic liquid is dehydrated alcohol or sherwood oil.
4, method according to claim 1 is characterized in that: described high energy ball mill is oscillatory type ball mill, planetary ball mill or stirring ball mill.
CN 200610011512 2006-03-17 2006-03-17 Process for preparing high performance Fe3Al-base composite materials Pending CN1865478A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101994060A (en) * 2010-12-10 2011-03-30 合肥工业大学 Ferrum-aluminium-chromium (Fe-Al-Cr) intermetallic compound powder metallurgy material and preparation method thereof
CN103990804A (en) * 2014-05-16 2014-08-20 江苏大学 Method for recycling steel scraps
CN107488816A (en) * 2017-08-29 2017-12-19 南洋泵业(青岛)有限公司 A kind of high-toughness high-strength composite and preparation method thereof
CN113249604A (en) * 2021-06-25 2021-08-13 北京科技大学 High purity intermetallic compound Nb3Al block and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101994060A (en) * 2010-12-10 2011-03-30 合肥工业大学 Ferrum-aluminium-chromium (Fe-Al-Cr) intermetallic compound powder metallurgy material and preparation method thereof
CN101994060B (en) * 2010-12-10 2012-09-26 合肥工业大学 Ferrum-aluminium-chromium (Fe-Al-Cr) intermetallic compound powder metallurgy material and preparation method thereof
CN103990804A (en) * 2014-05-16 2014-08-20 江苏大学 Method for recycling steel scraps
CN103990804B (en) * 2014-05-16 2016-08-24 江苏大学 A kind of method recycling steel cuttings
CN107488816A (en) * 2017-08-29 2017-12-19 南洋泵业(青岛)有限公司 A kind of high-toughness high-strength composite and preparation method thereof
CN113249604A (en) * 2021-06-25 2021-08-13 北京科技大学 High purity intermetallic compound Nb3Al block and preparation method thereof

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