CN101525716B - Iron aluminide intermetallic compound-titanium diboride composite material and preparation method thereof - Google Patents
Iron aluminide intermetallic compound-titanium diboride composite material and preparation method thereof Download PDFInfo
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- CN101525716B CN101525716B CN2009101166041A CN200910116604A CN101525716B CN 101525716 B CN101525716 B CN 101525716B CN 2009101166041 A CN2009101166041 A CN 2009101166041A CN 200910116604 A CN200910116604 A CN 200910116604A CN 101525716 B CN101525716 B CN 101525716B
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Abstract
The invention provides an iron aluminide intermetallic compound-titanium diboride composite material and a preparation method thereof. The material consists of 85%-95% of iron aluminide intermetallic compound and 5%-15% of titanium diboride in atom percent. The iron aluminide intermetallic compound-titanium diboride composite material is made by a mechanical alloying combined with a hot-pressing sintering method, which can avoid high-temperature melting and solidification procedure of normal metallurgical process, realize alloying at room temperature, and can reduce composition segregation and enhance influence of uneven phase distribution on performance, and process conditions are relatively simple and economic; and even dispersed phase can be introduced while obtaining fine nano-crystal structure, and the yield is high.
Description
Technical field
The present invention relates to iron aluminide intermetallic compound-titanium diboride composite material and preparation method thereof, particularly relate to a kind of method of utilizing the prepared by mechanical alloy iron aluminide intermetallic compound-titanium diboride composite material.
Background technology
Iron-aluminum based metal compound is owing to intensity height, anti-oxidant and anti-sulphur corrosion excellent property, and its toughness is higher than common stupalith, is the novel material that has the important application potentiality in aeronautical material and the high-temperature structural material field.Yet the same with other intermetallic compound, the two large problems that intensity sharply descended when fragility under its room temperature environment and temperature surpassed 600 ℃ has hindered its practical application.Many for this reason investigators attempt to solve moulding and application problem by crystal grain thinning and composite toughening.In Fe-Al intermetallic compound base body, add discrete wild phase (as staple fibre, whisker and particle etc.), by regulating stress distribution in the matrix material, stop crack propagation and giving full play to the effect of wild phase, can make the Fe-Al intermetallic compound based composite material have good comprehensive performances.Wherein, as toughener, the homodisperse of its raw material is all simple and easy to do than staple fibre and metal whisker composite with sintering densification with particle.Therefore, proper although particulate highly malleablized effect not as whisker and fiber, is selected as particle type, particle diameter and content, still have certain malleableize effect, can bring the improvement of hot strength, high temperature creep property simultaneously.
Traditional FeAl inter-metallic compound material preparation method is smelting process and fusion casting.Because the fusing point height of FeAl inter-metallic compound material is relatively more difficult with smelting method for preparing, and material is easy to generate component segregation in the melting.The low district, poor processability of moulding of temperature during the intermetallic compound that makes with fusion casting exists.
Because FeAl intermetallic compound fusing point is very high, has hindered traditional ingot metallurgy moulding, wild phase is significantly reduction of stability in the compound between melt metal, causes the wild phase dissolving, and the composition of matrix material changes; Simultaneously, the melt viscosity that contains wild phase is higher, and is mobile low, therefore adopts liquid condition shaping technology to be prepared and is subjected to certain limitation.
Summary of the invention
The present invention is for avoiding above-mentioned existing in prior technology weak point, the iron aluminide intermetallic compound-titanium diboride composite material that provide a kind of relative density height, has higher bending strength, hardness and fracture toughness property, being to be matrix with the intermetallic Fe-Al compound material, serves as to strengthen body with the titanium diboride ceramic particle;
The present invention provides the preparation method of iron aluminide intermetallic compound-titanium diboride composite material simultaneously.
Technical solution problem of the present invention adopts following technical scheme:
Iron aluminide intermetallic compound-titanium diboride composite material of the present invention is characterized in constituting by atomic percent: intermetallic Fe-Al compound 85%～95%, TiB2 5%～15%.
Iron aluminide intermetallic compound-titanium diboride composite material of the present invention, its characteristics also are:
By constituting of atomic percent: intermetallic Fe-Al compound 90%, TiB2 10%.
The atomic ratio of iron aluminium element is 1: 1 in the described intermetallic Fe-Al compound, and the atomic ratio of titanium boron is 1: 2 in the TiB2.
Iron aluminide intermetallic compound-titanium diboride composite material preparation method's of the present invention characteristics are to carry out as follows:
A, with Fe powder, Al powder, Ti powder and non-crystalline state B powder by 42.5～47.5%, 42.5～47.5%, 1.67～5% and 3.33～10% atomic percent batching, put into stainless steel jar mill, rotating speed low speed with 150 rev/mins on ball mill mixed powder 0.5 hour, made powder mixes even;
B, by weight percentage adds the process control agent that accounts for powder gross weight 1% in stainless steel jar mill, described process control agent is the easy volatile organic solvent;
C, under argon shield with mixed powder ball milling 40～50 hours, obtain the mechanical alloying composite powder;
D, the composite powder of described mechanical alloying is put into the electron tubes type low temperature oven, feed the mobile argon gas as protective atmosphere, be warming up to 350 ℃ with 5 ℃/minute speed, be incubated and cool to room temperature with the furnace after 0.5 hour, coming out of the stove obtains the composite powder of annealing;
E, the composite powder after will annealing place in the inertia graphite jig, put into the vacuum heating-press sintering stove, begin pressurization when being warming up to 450 ℃ with 10 ℃/minute speed, be incubated 0.5 hour, original pressure is 10MPa, still is heated to 1200 ℃ and pressure increased to 25MPa with 10 ℃/minute rate of heating then, is incubated 1 hour, cool to room temperature with the furnace, coming out of the stove obtains TiB
2/ FeAl matrix material.
Preparation method's of the present invention characteristics also are:
Among the described step a, the granularity of Fe powder, Al powder＜10 μ m, the granularity of Ti powder, non-crystalline state B powder＜45 μ m.
Process control agent among the step b is a normal heptane.
The rotating speed of ball mill is 700 rev/mins among the described step c, and ball material weight ratio is 10: 1.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the present invention is based on the premium properties of intermetallic Fe-Al compound and TiB2, utilize titanium diboride particle highly malleablized effect, and nano effect, make the matrix material relative density can reach more than 96%, have higher bending strength, hardness and fracture toughness property, realized wild phase and preparation condition are selected to optimize, improved the over-all properties of intermetallic Fe-Al compound.
2, the present invention adopts TiB
2Particle is as wild phase.TiB
2With the Fe-Al intermetallic compound good interface physics, chemical compatibility are arranged, select TiB
2As the wild phase of making the Fe-Al intermetallic compound based composite material is very suitable.
3, the present invention adopts mechanical alloying to prepare iron aluminide intermetallic compound-titanium diboride composite material in conjunction with hot-pressing sintering method, can avoid high temperature melting, the process of setting of common metallurgical method, at room temperature realize alloying, reduce component segregation and wild phase can not uniform distribution to Effect on Performance, the relative simple economy of processing condition; Can introduce even dispersed phase when obtaining meticulous nanocrystalline structure, and output is higher.
4, measure through performance test through the iron aluminide intermetallic compound-titanium diboride composite material of the inventive method preparation: its leading indicator is, bending strength is 1210MPa～1360MPa, and Vickers' hardness is 635～758 (HV10), and fracture toughness property is 5.78MPam
1/2～9.04MPam
1/2
5, iron aluminide intermetallic compound-titanium diboride composite material of the present invention has application potential in aeronautical material and high-temperature structural material field.
Below the invention will be further described by embodiment.
Embodiment
Embodiment 1, prepares TiB according to the following steps
2/ FeAl matrix material:
1, raw material mixes powder
With granularity is that 10 μ m, massfraction are 99% Fe powder, granularity is that 10 μ m, massfraction are 98% Al powder, granularity is that 45 μ m, massfraction are that 99% Ti powder and granularity are that 45 μ m, massfraction are that 98% non-crystalline state B powder is a raw material, according to Fe: Al: Ti: B=47.5: 47.5: 1.67: 3.33 atomic ratio, it is 100 milliliters stainless steel jar mill that composite powder is put into internal volume, low speed mixes powder on GN-2 type high energy ball mill, raw material is mixed, and mixing the powder time is 0.5 hour.
2, mechanical alloying powder process
Concrete processing parameter is set to:
Ratio of grinding media to material: 10: 1;
Stacking factor: 0.5;
The ball milling time: 40 hours;
Drum's speed of rotation: 700 rev/mins;
Protective atmosphere: argon gas;
Process control agent: normal heptane (by weight percentage, for powder gross weight 1%).
According to above-mentioned processing parameter, composite powder is carried out mechanical alloying on GN-2 type high energy ball mill.
3, low-temperature annealing
To put into pottery through the composite powder of mechanical alloying and burn boat; then the burning boat is put into the electron tubes type High Temperature Furnaces Heating Apparatus and carry out the low-temperature annealing processing; feed the mobile argon gas as protective atmosphere; be warming up to 350 ℃ with 5 ℃/minute speed; be incubated 0.5 hour; cool to room temperature with the furnace, the annealing composite powder after the acquisition of coming out of the stove eliminates stress.
4, hot pressed sintering
Composite powder after the annealing is placed in the inertia graphite jig, put into the vacuum heating-press sintering stove, be warming up to 450 ℃ with 10 ℃/minute speed, be incubated 0.5 hour, begin pressurization (original pressure is 10MPa) simultaneously, still be heated to 1200 ℃ then, and pressure is increased to 25MPa, be incubated 1 hour with 10 ℃/minute rate of heating.Blank behind the sintering cools to room temperature with the furnace and comes out of the stove, and obtains TiB
2/ FeAl matrix material.
TiB by above prepared
2The specific performance of/FeAl matrix material is as follows, and is listed as first group of array in the table 1:
Bending strength (room temperature): 1360MPa;
Hardness (Vickers): 635HV10;
Fracture toughness property: 8.35MPam
1/2
Embodiment 2, prepare TiB according to the following steps
2/ FeAl matrix material:
1, raw material mixes powder
With granularity is that 10 μ m, massfraction are 99% Fe powder, granularity is that 10 μ m, massfraction are 98% Al powder, granularity is that 45 μ m, massfraction are that 99% Ti powder and granularity are that 45 μ m, massfraction are that 98% non-crystalline state B powder is a raw material, according to Fe: Al: Ti: B=45: 45: 3.33: 6.67 atomic ratio, it is 100 milliliters stainless steel jar mill that composite powder is put into internal volume, low speed mixes powder on GN-2 type high energy ball mill, raw material is mixed, and mixing the powder time is 0.5 hour.
2, mechanical alloying powder process
Concrete processing parameter is set to:
Ratio of grinding media to material: 10: 1;
Stacking factor: 0.5;
The ball milling time: 45 hours;
Drum's speed of rotation: 700 rev/mins;
Protective atmosphere: argon gas;
Process control agent: normal heptane (by weight percentage, for powder gross weight 1%).
According to above-mentioned processing parameter, composite powder is carried out mechanical alloying on GN-2 type high energy ball mill.
3, low-temperature annealing
To put into pottery through the composite powder of mechanical alloying and burn boat; then the burning boat is put into the electron tubes type High Temperature Furnaces Heating Apparatus and carry out the low-temperature annealing processing; feed the mobile high-purity argon gas as protective atmosphere; be warming up to 350 ℃ with 5 ℃/minute speed; be incubated 0.5 hour; cool to room temperature with the furnace, the annealing composite powder after the acquisition of coming out of the stove eliminates stress.
4, hot pressed sintering
Composite powder after the annealing is placed in the inertia graphite jig, put into the vacuum heating-press sintering stove, be warming up to 450 ℃ with 10 ℃/minute speed, be incubated 0.5 hour, begin pressurization (original pressure is 10MPa) simultaneously, still be heated to 1200 ℃ then, and pressure is increased to 25MPa, be incubated 1 hour with 10 ℃/minute rate of heating.Blank behind the sintering cools to room temperature with the furnace and comes out of the stove, and obtains TiB
2/ FeAl matrix material.
TiB by above prepared
2The specific performance of/FeAl matrix material is as follows, and is listed as second group of array in the table 1:
Bending strength (room temperature): 1320MPa;
Hardness (Vickers): 745HV10;
Fracture toughness property: 9.04MPam
1/2
Embodiment 3, prepare TiB according to the following steps
2/ FeAl matrix material:
1, raw material mixes powder
With granularity is that 10 μ m, massfraction are that 99% Fe powder, granularity are that 10 μ m, massfraction are that 98% Al powder, granularity are that 45 μ m, massfraction are that 99% Ti powder and granularity are that 45 μ m, massfraction are that 98% non-crystalline state B powder is a raw material, according to Fe: Al: Ti: B=42.5: 42.5: 5: 10 atomic ratio, it is 100 milliliters stainless steel jar mill that composite powder is put into internal volume, low speed mixes powder on GN-2 type high energy ball mill, raw material is mixed, and mixing the powder time is 0.5 hour.
2, mechanical alloying powder process
Concrete processing parameter is set to:
Ratio of grinding media to material: 10: 1;
Stacking factor: 0.5;
The ball milling time: 50 hours;
Drum's speed of rotation: 700 rev/mins;
Protective atmosphere: argon gas;
Process control agent: normal heptane (by weight percentage, 1% of the powder gross weight).
According to above-mentioned processing parameter, composite powder is carried out mechanical alloying on GN-2 type high energy ball mill.
3, low-temperature annealing
To put into pottery through the composite powder of mechanical alloying and burn boat; then the burning boat is put into the electron tubes type High Temperature Furnaces Heating Apparatus and carry out the low-temperature annealing processing; feed the mobile high-purity argon gas as protective atmosphere; be warming up to 350 ℃ with 5 ℃/minute speed; be incubated 0.5 hour; cool to room temperature with the furnace, the annealing composite powder after the acquisition of coming out of the stove eliminates stress.
4, hot pressed sintering
Composite powder after the annealing is placed in the inertia graphite jig, put into the vacuum heating-press sintering stove, be warming up to 450 ℃ with 10 ℃/minute speed, be incubated 0.5 hour, begin pressurization (original pressure is 10MPa) simultaneously, still be heated to 1200 ℃ then, and pressure is increased to 25MPa, be incubated 1 hour with 10 ℃/minute rate of heating.Blank behind the sintering cools to room temperature with the furnace and comes out of the stove, and obtains TiB
2/ FeAl matrix material.
TiB by above prepared
2The specific performance of/FeAl matrix material is as follows, and is listed as the 3rd group of array in the table 1:
Bending strength (room temperature): 1210MPa;
Hardness (Vickers): 758HV10;
Fracture toughness property: 5.78MPam
1/2
Matrix material bending strength, hardness and the fracture toughness property of table 1 the present invention preparation
Claims (4)
1. the preparation method of an iron aluminide intermetallic compound-titanium diboride composite material is characterized in that carrying out as follows:
A, with Fe powder, Al powder, Ti powder and non-crystalline state B powder by 42.5～47.5%, 42.5～47.5%, 1.67～5% and 3.33～10% atomic percent batching, put into stainless steel jar mill, rotating speed low speed with 150 rev/mins on ball mill mixed powder 0.5 hour, made powder mixes even;
B, by weight percentage adds the process control agent that accounts for powder gross weight 1% in stainless steel jar mill, described process control agent is the easy volatile organic solvent;
C, under argon shield with mixed powder ball milling 40～50 hours, obtain the mechanical alloying composite powder;
D, the composite powder of described mechanical alloying is put into the electron tubes type low temperature oven, feed the mobile argon gas as protective atmosphere, be warming up to 350 ℃ with 5 ℃/minute speed, be incubated and cool to room temperature with the furnace after 0.5 hour, coming out of the stove obtains the composite powder of annealing;
E, the composite powder after will annealing place in the inertia graphite jig, put into the vacuum heating-press sintering stove, begin pressurization when being warming up to 450 ℃ with 10 ℃/minute speed, be incubated 0.5 hour, original pressure is 10MPa, still is heated to 1200 ℃ and pressure increased to 25MPa with 10 ℃/minute rate of heating then, is incubated 1 hour, cool to room temperature with the furnace, coming out of the stove obtains TiB
2/ FeAl matrix material.
2. the preparation method of iron aluminide intermetallic compound-titanium diboride composite material according to claim 1 is characterized in that among the described step a, the granularity of Fe powder, Al powder＜10 μ m, the granularity of Ti powder, non-crystalline state B powder＜45 μ m.
3. the preparation method of iron aluminide intermetallic compound-titanium diboride composite material according to claim 1 is characterized in that among the described step b, and process control agent is a normal heptane.
4. the preparation method of iron aluminide intermetallic compound-titanium diboride composite material according to claim 1 is characterized in that among the described step c, and the rotating speed of ball mill is 700 rev/mins, and ball material weight ratio is 10: 1.
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| CN102776431B (en) * | 2012-08-20 | 2014-03-12 | 山东交通学院 | Tri-iron aluminide intermetallic compound-titanium nitride ceramic composite and method for preparing same |
| CN102807190A (en) * | 2012-09-07 | 2012-12-05 | 天津大学 | Method for eliminating internal stress of nanodevice |
| CN102832120A (en) * | 2012-09-07 | 2012-12-19 | 天津大学 | Method for applying prestress on nanometer device surface |
| CN104550904B (en) * | 2014-12-17 | 2016-09-14 | 武汉理工大学 | A kind of with Mo-B-O platelike crystal be the lubrication novel TiAl based self-lubricating material of phase and preparation method |
| JP7100320B2 (en) * | 2018-08-07 | 2022-07-13 | 国立大学法人広島大学 | Fe-based sintered body, manufacturing method of Fe-based sintered body, and hot pressing die |
| CN110842177A (en) * | 2019-12-04 | 2020-02-28 | 山东汇丰铸造科技股份有限公司 | High-wear-resistance nodular cast iron winding drum for large winch and manufacturing method thereof |
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| CN1092113A (en) * | 1993-03-13 | 1994-09-14 | 西安工业学院 | The complex phase iron-aluminium intermetalics corrosion and heat resistant alloy |
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Non-Patent Citations (2)
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