CN101994060B - Ferrum-aluminium-chromium (Fe-Al-Cr) intermetallic compound powder metallurgy material and preparation method thereof - Google Patents
Ferrum-aluminium-chromium (Fe-Al-Cr) intermetallic compound powder metallurgy material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ferrum-aluminium-chromium (Fe-Al-Cr) intermetallic compound powder metallurgy material and a preparation method thereof. The Fe-Al-Cr intermetallic compound powder metallurgy material consists of the following raw materials in percentage according to atomic number: 28 to 40 percent of Al, 3 to 5 percent of Cr and the balance of Fe, wherein Cr is added in the form of Fe-20 percent Cr prealloy powder. The preparation method of the Fe-Al-Cr intermetallic compound powder metallurgy material comprises the following steps of: mixing Fe powder, Al powder and the Fe-20 percent Cr prealloy powder uniformly; performing ball-milling on the mixture under the protection of argon; annealing and performing hot-pressing sintering treatment to obtain the Fe-Al-Cr intermetallic compound powder metallurgy material. The alloy element Cr is added in the form of the Fe-20 percent Cr prealloy powder with the density similar to that of the Fe, so the Cr loss in the sintering process can be avoided, the diffusion of the Cr to a Fe-Al matrix is promoted, and alloy toughening effect is improved.
Description
One, technical field
The present invention relates to a kind of metallurgical material, specifically a kind of Fe-Al-Cr intermetallic compound powder metallurgical material and preparation method thereof.
Two, background technology
Fe-Al intermetallic compound (Fe
3Al and FeAl) because density is little, intensity is high, anti-oxidant, anti-sulphur corrosion and abrasion resistance properties are excellent, and its toughness is higher than common stupalith, is the new structural material that has the important application potentiality in aeronautical material and the high-temperature structural material field.Yet, the same with other intermetallic compound, its room temperature fragility and more than 600 ℃ during high temperature the intensity two large problems that sharply descends hindered its practical application.Domestic and international for this reason many investigators attempt to solve moulding and application problem through crystal grain thinning and alloy (solid solution) highly malleablized.In Fe-Al intermetallic compound base body, add alloying element, through the degree of order and the friendship slippage ability of regulating material, crystal grain thinning, change defective configuration etc. can make Fe-Al intermetallic compound base material have good comprehensive performances.Traditional Fe-Al inter-metallic compound material preparation method is smelting process and fusion casting, and is relatively more difficult with smelting method for preparing because the fusing point of Fe-Al inter-metallic compound material is high, is easy to generate component segregation; In addition, temperature was low during the Fe-Al intermetallic compound that makes with fusion casting existed moulds the district, poor processability, all lower (Fe of as cast condition of the hardness of material, intensity
3Al hardness is 25～28HRC, and compression yield strength is 300～600MPa, and the FeAl intensity of as cast condition is about 370MPa).
Existing research shows, proper if alloying element kind, content are selected, the interpolation of alloying element can improve the over-all properties of Fe-Al intermetallic compound to a certain extent.1994; " Acta Metallurgica Sinica " (30; 1994,515-521) reported that employing liquid condition shaping technology (founding) adds the mechanical behavior under high temperature that the B element can effectively improve the Fe-Al intermetallic compound in the Fe-Al intermetallic compound, but reduced its temperature-room type plasticity to a certain extent.
Cr improves the most effectively one of alloying element of Fe-Al intermetallic compound temperature-room type plasticity, and what prepare at present that the Fe-Al-Cr intermetallic compound mostly adopts is liquid forming technology, like founding.Nineteen ninety-five, and " applied science journal " (13,1995,393-399) reported the Fe of alloying elements cr to the founding preparation
3The influence of Al alloy compression performance, the adding of Cr can suitably improve the compression plasticity of alloy.Domestic only in 1993; " mechanical engineering material " (17; 1993,10-12) reported employing prepared by mechanical alloy Fe-Al-Cr intermetallic compound, FeAl+Cr is mutually because solution strengthening, dispersion-strengthened and grain-boundary strengthening make bending resistance and compressive strength that obvious increase all arranged.But the adding of this research interalloy element Cr is the form adding with Cr simple substance powder; The shortcoming of this kind alloying elements cr addition manner is: (1) is in the ma process of Fe-Al-Cr alloy powder; Cr is difficult to the diffusion in the Fe-Al alloy substrate, is unfavorable for the homogenization of composition of Cr; (2) prepare in the process at the Fe-Al-Cr intermetallic compound,, therefore exist Cr to be prone to problems such as oxidization burning loss because of the oxidation activity of simple substance Cr is very high.
Three, summary of the invention
The present invention is for avoiding above-mentioned existing in prior technology weak point, a kind of Fe-Al-Cr intermetallic compound powder metallurgical material and preparation method thereof is provided, preparing the deficiency that this kind material exists with the liquid forming technology of avoiding founding.
Technical solution problem of the present invention adopts following technical scheme:
The characteristics of Fe-Al-Cr intermetallic compound powder metallurgical material of the present invention are to be constructed as follows by its raw material of atom number per-cent: Al is 28-40%, and Cr is 3-5%, and surplus is Fe;
Said Cr is the form adding with Fe-20%Cr prealloy powder.
The preparing method's of Fe-Al-Cr intermetallic compound powder metallurgical material of the present invention characteristics are to operate as follows:
A, put into the Stainless Steel Ball grinding machine after Fe powder, Al powder and Fe-20%Cr prealloy powder mixed, mixed powder 0.5 hour with 150 rev/mins rotating speeds, uniform mixed powder;
B, under argon shield with step a gained mixed powder ball milling 60-70 hour, obtain nano-crystalline Fe-Al-Cr powdered alloy;
C, said nano-crystalline Fe-Al-Cr powdered alloy is put into the electron tubes type heat treatment furnace; Feed mobile hydrogen as protective atmosphere; Be warming up to 750 ℃ with 5 ℃/minute speed, be incubated and cool to room temperature with the furnace after 0.5 hour, the nano-crystalline Fe-Al-Cr powdered alloy after the acquisition annealing of coming out of the stove;
D, the nano-crystalline Fe after the said annealing-Al-Cr powdered alloy 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 then, when temperature reaches 450 ℃, be forced into 10MPa; Insulation begins gradually pressure boost to 25MPa and keep when finishing; In pressurization, be heated to 1250 ℃ and be incubated 1 hour, come out of the stove after cooling to room temperature with the furnace, obtain Fe-Al-Cr intermetallic compound powder metallurgical material with 10 ℃/minute heat-up rate.
The preparing method's of Fe-Al-Cr intermetallic compound powder metallurgical material of the present invention characteristics also are: the particle diameter of Fe powder and Al powder among the said step a≤10 μ m, the particle diameter of said Fe-20%Cr prealloy powder≤198 μ m.
The preparing method's of Fe-Al-Cr intermetallic compound powder metallurgical material of the present invention characteristics also are: among the said step b, the rotating speed of said ball mill is 700 rev/mins, and ball material weight ratio is 10: 1.
The preparing method's of Fe-Al-Cr intermetallic compound powder metallurgical material of the present invention characteristics also are: in the said steps d, said pressure boost gradually to the rate of pressurization of 25MPa is 170-200Pa/min.
The Fe-Al intermetallic compound of rich Fe has DO
3With two kinds of ordered structures of B2, be DO when Al atom number per-cent is for 22.5-33% under the room temperature
3Structure, structural formula are Fe
3Al; Al atom number per-cent is the B2 structure during for 33-51%, and structural formula is FeAl.DO
3With B2 all be ordered intermetallic compound, DO
3The structurally ordered Du Genggao of type.Two types of material selection Al atomic percentage concs of the present invention are respectively 28% and 35%, 40%, promptly distinguish corresponding DO
3Structure and B2 structure.The intermetallic compound that obtains is respectively Fe
3Al (Cr) and FeAl (Cr) alloy material.
Compared with present technology, beneficial effect of the present invention is embodied in:
1, interalloy element Cr of the present invention is to adopt the density Fe-20%Cr pre-alloyed powder close with Fe to add; This adding mode of Cr element can effectively be avoided Cr loss in the sintering process; Promote the diffusion of Cr in the Fe-Al matrix; Improve the homogenizing of alloying constituent, improve the effect of alloy highly malleablized.
2, the present invention adopts mechanical alloying and heat pressing process to prepare the Fe-Al-Cr inter-metallic compound material; Can avoid in traditional founding because of the disadvantageous effect of component segregation material structure and performance, obtain composition evenly, organize tiny mmaterial or goods.
3, through the Fe-Al-Cr intermetallic compound powder metallurgical material of the inventive method preparation, its performance reaches: ultimate compression strength: 1313-1391MPa, Vickers' hardness: HV538-853.
4, Fe-Al-Cr intermetallic compound powder metallurgical material of the present invention has the huge applications potentiality in aeronautical material and high-temperature structural material field.
Four, description of drawings
Fig. 1 is the surface topography map of the Fe-28Al-5Cr intermetallic compound powder metallurgical material that makes of the present invention;
Fig. 2 is the fracture apperance figure of the Fe-28Al-5Cr intermetallic compound powder metallurgical material that makes of the present invention;
Fig. 3 is the surface topography map of the Fe-40Al-5Cr intermetallic compound powder metallurgical material that makes of the present invention;
Fig. 4 is the fracture apperance figure of the Fe-40Al-5Cr intermetallic compound powder metallurgical material that makes of the present invention;
Fig. 5 is the surface topography map of the Fe-35Al-3Cr intermetallic compound powder metallurgical material that makes of the present invention;
Fig. 6 is the fracture apperance figure of the Fe-35Al-3Cr intermetallic compound powder metallurgical material that makes of the present invention.
Five, embodiment
Embodiment 1:
It is Fe that present embodiment prepares Fe-28Al-5Cr intermetallic compound powder metallurgical material according to the following steps
3Al (Cr) alloy material, wherein Fe-28Al-5Cr is meant that the atom number per-cent of Al in alloy material is 28%, and the atom number per-cent of Cr is 5%, and surplus is Fe.
1, raw material mixes powder
Put into the stainless steel jar mill that internal volume is 100mL after the Fe-20%Cr prealloy powder of the Al powder of the Fe powder of particle diameter≤10 μ m, particle diameter≤10 μ m and particle diameter≤198 μ m mixed; Rotating speed low speed with 150 rev/mins on GN-2 type high energy ball mill mixes powder; Make raw materials mix even; Mixing the powder time is 0.5 hour, gets uniform mixed powder;
2, mechanical alloying powder process
Concrete processing parameter is set to:
Ball-milling medium: GCr15 steel ball;
Ball material weight ratio: 10: 1;
Stacking factor: 0.5;
The ball milling time: 70 hours;
Drum's speed of rotation: 700 rev/mins;
Protective atmosphere: argon gas.
According to above-mentioned processing parameter, mixed powder is carried out mechanical alloying on GN-2 type high energy ball mill.
3, powder annealing
The Fe-28Al-5Cr powdered alloy that step 2 mechanical alloying makes is put into pottery burning boat, put into the electron tubes type heat treatment furnace to the burning boat then and carry out anneal, feed mobile hydrogen as protective atmosphere; Be warming up to 750 ℃ with 5 ℃/minute speed; Be incubated 0.5 hour, cool to room temperature with the furnace, come out of the stove; Eliminate the internal stress of Fe-28Al-5Cr powdered alloy, the nano-crystalline Fe after must annealing-Al-Cr powdered alloy;
4, hot pressed sintering
Nano-crystalline Fe-Al-Cr the powdered alloy that will pass through after the annealing of step 3 gained places 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 then, when temperature reaches 450 ℃, be forced into 10MPa; Insulation begin when finishing with the rate of pressurization of 170-200Pa/min gradually pressure boost to 25MPa and keep; In pressurization, be heated to 1250 ℃ and be incubated 1 hour, come out of the stove after cooling to room temperature with the furnace, obtain dense structure, Fe-28Al-5Cr intermetallic compound powder metallurgical material that crystal grain is tiny with 10 ℃/minute heat-up rate.
Can find out by Fig. 1, at 1250 ℃ of following agglomerating Fe
3The dense structure of Al (Cr), crystal grain is tiny, explain the method that adopts mechanical alloying and hot pressed sintering to combine can obtain to organize tiny, the Fe that density is high
3Al (Cr) material.
Can find out hot pressing Fe by Fig. 2
3Al (Cr) sample bending resistance fracture is more smooth, is along crystalline substance and cleavage fracture characteristic.
The ultimate compression strength of present embodiment gained Fe-28Al-5Cr intermetallic compound powder metallurgical material is 1313MPa, and hardness is HV538, than as cast condition Fe
3Al inter-metallic compound material performance is significantly increased.
Embodiment 2:
It is FeAl (Cr) alloy material that present embodiment prepares Fe-40Al-5Cr intermetallic compound powder metallurgical material according to the following steps; Wherein Fe-40Al-5Cr is meant that the atom number per-cent of Al in alloy material is 40%; The atom number per-cent of Cr is 5%, and surplus is Fe.
1, raw material mixes powder
Put into the stainless steel jar mill that internal volume is 100mL after the Fe-20%Cr prealloy powder of the Al powder of the Fe powder of particle diameter≤10 μ m, particle diameter≤10 μ m and particle diameter≤198 μ m mixed; Rotating speed low speed with 150 rev/mins on GN-2 type high energy ball mill mixes powder; Make raw materials mix even; Mixing the powder time is 0.5 hour, gets uniform mixed powder;
2, mechanical alloying powder process
Concrete processing parameter is set to:
Ball-milling medium: GCr15 steel ball;
Ball-to-powder weight ratio: 10: 1;
Stacking factor: 0.5;
The ball milling time: 70 hours;
Drum's speed of rotation: 700 rev/mins;
Protective atmosphere: argon gas.
According to above-mentioned processing parameter, composite powder is carried out mechanical alloying on GN-2 type high energy ball mill.
3, powder annealing
To put into pottery through the Fe-40Al-5Cr powdered alloy that mechanical alloying makes and burn boat; Put into the electron tubes type heat treatment furnace to the burning boat then and carry out anneal, feed mobile hydrogen, be warming up to 750 ℃ with 5 ℃/minute speed as protective atmosphere; Be incubated 0.5 hour; Cool to room temperature with the furnace, come out of the stove, eliminate the internal stress of Fe-40Al-5Cr powdered alloy.
4, hot pressed sintering
Fe-40Al-5Cr powdered alloy 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 then, when temperature reaches 450 ℃, be forced into 10MPa; Insulation begin when finishing with the rate of pressurization of 170-200Pa/min gradually pressure boost to 25MPa and keep; In pressurization, be heated to 1250 ℃ and be incubated 1 hour, come out of the stove after cooling to room temperature with the furnace, obtain dense structure, Fe-40Al-5Cr intermetallic compound powder metallurgical material that crystal grain is tiny with 10 ℃/minute heat-up rate.
Can find out that by Fig. 3 crystal grain is tiny in the dense structure of 1250 ℃ of following agglomerating FeAl (Cr), explain the method that adopts mechanical alloying and hot pressed sintering to combine can obtain to organize tiny, the FeAl that density is high (Cr) material.
Can find out that by Fig. 4 the bending resistance fracture of hot pressing FeAl (Cr) sample is more smooth, belongs to brittle rupture.But on surface of fracture, can more clearly see something of characteristics such as accurate cleavage facet and dimple, explain that hot pressing FeAl (Cr) presents incomplete brittle rupture, present the characteristic of part ductile rupture.
The ultimate compression strength of the Fe-40Al-5Cr intermetallic compound powder metallurgical material that present embodiment makes: 1391MPa, hardness: HV853 is significantly increased than as cast condition FeAl inter-metallic compound material performance.
Embodiment 3:
It is FeAl (Cr) alloy material that present embodiment prepares Fe-35Al-3Cr intermetallic compound powder metallurgical material according to the following steps; Wherein Fe-35Al-3Cr is meant that the atom number per-cent of Al in alloy material is 35%; The atom number per-cent of Cr is 3%, and surplus is Fe.
1, raw material mixes powder
Put into the stainless steel jar mill that internal volume is 100mL after the Fe-20%Cr prealloy powder of the Al powder of the Fe powder of particle diameter≤10 μ m, particle diameter≤10 μ m and particle diameter≤198 μ m mixed; Rotating speed low speed with 150 rev/mins on GN-2 type high energy ball mill mixes powder; Make raw materials mix even; Mixing the powder time is 0.5 hour, gets uniform mixed powder;
2, mechanical alloying powder process
Concrete processing parameter is set to:
Ball-milling medium: GCr15 steel ball;
Ball-to-powder weight ratio: 10: 1;
Stacking factor: 0.5;
The ball milling time: 70 hours;
Drum's speed of rotation: 700 rev/mins;
Protective atmosphere: argon gas.
According to above-mentioned processing parameter, composite powder is carried out mechanical alloying on GN-2 type high energy ball mill.
3, powder annealing
To put into pottery through the Fe-35Al-3Cr powdered alloy that mechanical alloying makes and burn boat; Put into the electron tubes type heat treatment furnace to the burning boat then and carry out anneal, feed mobile hydrogen, be warming up to 750 ℃ with 5 ℃/minute speed as protective atmosphere; Be incubated 0.5 hour; Cool to room temperature with the furnace, come out of the stove, eliminate the internal stress of Fe-35Al-3Cr powdered alloy.
4, hot pressed sintering
Fe-35Al-3Cr powdered alloy 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 then, when temperature reaches 450 ℃, be forced into 10MPa; Insulation begin when finishing with the rate of pressurization of 170-200Pa/min gradually pressure boost to 25MPa and keep; In pressurization, be heated to 1250 ℃ and be incubated 1 hour, come out of the stove after cooling to room temperature with the furnace, obtain dense structure, Fe-35Al-3Cr intermetallic compound powder metallurgical material that crystal grain is tiny with 10 ℃/minute heat-up rate.
Can be found out in the weave construction of 1250 ℃ of following agglomerating FeAl (Cr) evenly fine and closely by Fig. 5, crystal grain is tiny.Explain that the preparation method who adopts mechanical alloy chemical combination hot pressed sintering to combine can obtain to organize tiny, fine and close FeAl (Cr) material.
Can find out that by Fig. 6 the bending resistance fracture of hot pressing FeAl (Cr) sample is more smooth, presents the brittle rupture characteristic.But on surface of fracture, still can more clearly see something of characteristics such as accurate cleavage facet and dimple, explain that hot pressing FeAl (Cr) presents incomplete brittle rupture, present the characteristic of part ductile rupture.
The ultimate compression strength of the Fe-35Al-3Cr intermetallic compound powder metallurgical material that present embodiment makes: 1325MPa, hardness: HV785 is significantly increased than as cast condition FeAl inter-metallic compound material performance.
Claims (1)
1. the preparation method of a Fe-Al-Cr intermetallic compound powder metallurgical material is characterized in that operating as follows:
A, put into the Stainless Steel Ball grinding machine after Fe powder, Al powder and Fe-20%Cr prealloy powder mixed, mixed powder 0.5 hour with 150 rev/mins rotating speeds, uniform mixed powder; Wherein raw material is 28-40% by atom number per-cent Al, and Cr is 3-5%, and surplus is Fe; The particle diameter of Fe powder and Al powder≤10 μ m, the particle diameter of said Fe-20%Cr prealloy powder≤198 μ m;
B, under argon shield with step a gained mixed powder ball milling 60-70 hour, obtain nano-crystalline Fe-Al-Cr powdered alloy; The rotating speed of said ball mill is 700 rev/mins, and ball material weight ratio is 10: 1;
C, said nano-crystalline Fe-Al-Cr powdered alloy is put into the electron tubes type heat treatment furnace; Feed mobile hydrogen as protective atmosphere; Be warming up to 750 ℃ with 5 ℃/minute speed, be incubated and cool to room temperature with the furnace after 0.5 hour, the nano-crystalline Fe-Al-Cr powdered alloy after the acquisition annealing of coming out of the stove;
D, the nano-crystalline Fe after the said annealing-Al-Cr powdered alloy is placed in the inertia graphite jig; Put into the vacuum heating-press sintering stove, be warming up to 450 ℃, be incubated 0.5 hour then with 10 ℃/minute speed;, temperature is forced into 10MPa when reaching 450 ℃; Insulation begins gradually pressure boost to 25MPa and keep when finishing, rate of pressurization is 170-200Pa/min, in pressurization, is heated to 1250 ℃ and be incubated 1 hour with 10 ℃/minute heat-up rate; Come out of the stove after cooling to room temperature with the furnace, obtain Fe-Al-Cr intermetallic compound powder metallurgical material.
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| Haili Liu et al..Structural evolutions of the Fe-40Al-5Cr powders during mechanical alloying and subsequent heat treatment.《Journal of Alloys and Compounds》.2010,第506卷(第2期),第963-968页. * |
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