CN102345069A - Large block micrometer-grain/nanometer-grain double-phase Fe-Al-Cr material and preparation method thereof - Google Patents
Large block micrometer-grain/nanometer-grain double-phase Fe-Al-Cr material and preparation method thereof Download PDFInfo
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- CN102345069A CN102345069A CN2011101653618A CN201110165361A CN102345069A CN 102345069 A CN102345069 A CN 102345069A CN 2011101653618 A CN2011101653618 A CN 2011101653618A CN 201110165361 A CN201110165361 A CN 201110165361A CN 102345069 A CN102345069 A CN 102345069A
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Abstract
The invention discloses a large block micrometer-grain/nanometer-grain double-phase Fe-Al-Cr material and a preparation method thereof, wherein the material is composed by the compositions of 70-80% Fe, 10-15% Al and 5-20% Cr; the method comprises the steps of: first, weighing the reaction materials according to the proportion; second, dry grinding the weighed powder for 8-16h, then placing the mixed reaction materials in a die, and pressing the mixed reaction materials into a green body at the pressure of 30-60MPa; putting the pressed green body of 1-2kg into a reactor, and adding the ignition agent; and then blowing the reactor with argon at the room temperature to exhaust the air therein, heating until the temperature reaches 200 DEG C, then discharging the gas again after half a hour of heat preservation, and filling the argon of 3-6 MPa to continuously heat. When the temperature reaches 260-320 DEG C, the ignition agent reacts and discharges a large quantity of heat, accordingly, the reaction materials are reacted with one another, the reaction fondant is deposited in a large high heat conduction copper die in situ, the reaction can be completed within a plurality of seconds; and finally, the prepared Fe-Al-Cr material is put in a box-type resistance furnace to undergo isothermal treatment for 8-24h at 800-1000 DEG C, so the material is obtained.
Description
Technical field
The present invention relates to the Fe-Al-Cr material preparation method.
Background technology
The room temperature fragility of intermetallic compound has hindered it to be used widely, and nanometer and alloying are to solve the brittle effective way of room temperature.At present the preparation method of bulk nano-crystalline material mainly contains two kinds of ascending method and descending methods; Promptly obtain the high energy consumption of block materials, expensive method through the compacting sintering by nano-powder; Perhaps obtain the method for nanocrystalline material through amorphous crystallization or large plastometric set etc., but these methods only are applicable to different materials and can't amplification production by block materials.
Summary of the invention
The purpose of this invention is to provide a kind of blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material and preparation method thereof.
The present invention is blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material and preparation method thereof, and the composition of its material is Fe 70-80%, Al 10-15%, Cr 5-20%; The diameter of material can reach 150～200mm, and thickness reaches 8～12mm; The grain-size of nanometer crystalline phase wherein accounts for more than 70～75% less than the nanocrystalline of 30nm between 5～80nm in the material; The micron crystalline phase distributes with bar form, and length is 0.5～10 μ m; Vickers hardness number is 2.5～3.0GPa; Yield strength is 680～810Mpa.
The step of its preparation method is:
(1) mass ratio according to ferric oxide, aluminium, chromium is 24～7: 11～3.5: 0.8～1.2 ratio takes by weighing reaction mass;
(2) with the powder that takes by weighing at ball mill for dry grinding 8-16 hour, press down at the pressure of 30-60MPa with pressing machine in the stainless steel mould of then reaction mass that mixes being packed into and process base substrate; Pack into 1～2 kilogram of base substrate that presses in the reactor and put into detonator, detonator accounts for the 0.1-0.2% of reaction mass mass percent;
(3) under the room temperature with the argon purge reaction vessel with the air post-heating in the amount discharge container, by the time temperature rises to exhaust once more after 200 ℃ of insulation half an hour, the argon gas that charges into 3～6MPa then continues heating.When temperature reached 260-320 ℃, a large amount of heat was emitted in the detonator reaction, thus the reaction of initiation reaction storeroom, and the reaction melt in-situ deposition is in high heat conduction large size copper mold.Reaction can be accomplished in tens seconds, and reaction product is furnace cooling under argon shield.Take out material after the room temperature, with the by product Al of surface coverage
2O
3Peel off removal;
(4) the as cast condition Fe-Al-Cr material of preparation is put into chamber type electric resistance furnace and is carried out 800～1000 ℃ of isothermal processes 8-24 hours after, prepare blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material.
Usefulness of the present invention is less energy-consumption, low cost, high-level efficiency, but and the preparation blocks of large micron of suitability for industrialized production crystalline substance/nanocrystalline two-phase Fe-Al-Cr material.
The blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material diameter that the present invention obtains can reach 150-200mm, and thickness reaches 8-12mm.Characterize through X-ray diffraction technology and transmission electron microscope, this material has Fe
3The unordered body-centered cubic structure of Al does not have other impurity phases.The grain-size of nanometer crystalline phase wherein accounts for more than the 70-75% less than the nanocrystalline of 30nm between 5-80nm.The micron crystalline phase distributes with bar form, and length is 0.5-10 μ m.
To blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material through gone Vickers' hardness and room temperature compression performance the test.The hardness test condition is: load 198g, dwell time 15s.The compressive strength specimen size: the cylinder of diameter 5mm height 5mm, displacement of pressing head speed is 0.1mm/min.The vickers hardness number of blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material is 2.5-3.0GPa, and yield strength is 680-810MPa.
Embodiment
Embodiment 1:
According to ferric oxide: aluminium: the mass ratio of chromium is to take by weighing reaction mass at 22: 11: 1.2; The powder that weighs up ball mill for dry grinding 8 hours, is pressed down at the pressure of 40MPa with pressing machine in the stainless steel mould of then reaction mass that mixes being packed into and processes the reaction base substrate.1 kilogram of reaction base substrate is put into the copper mold of reactor, and detonator is placed in the base substrate bottom, and (account for 0.2% of reaction mass mass percent, sulphur: aluminium: Manganse Dioxide: the mass ratio of saltpetre is 1.25: 1: 1: 2).Under the room temperature with the argon purge reaction vessel with the air in the amount discharge container, by the time temperature rises to exhaust once more after 200 ℃ of insulation half an hour, the argon gas that charges into 3MPa then continues heating.When temperature reached 260 ℃ of left and right sides, a large amount of heat was emitted in the detonator reaction, thus the reaction of initiation reaction storeroom.Reaction can be accomplished in tens seconds, and reaction product furnace cooling under argon shield takes out after room temperature, with the by product Al of surface coverage
2O
3Peel off removal.The as cast condition Fe-Al-Cr material of preparation is put into heat treatment furnace through 800 ℃, after 24 hours isothermal processes, prepare blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material.Characterize through X-ray diffraction technology and transmission electron microscope, this material has Fe
3The unordered body-centered cubic structure of Al does not have other impurity phases.The grain-size of nanometer crystalline phase wherein accounts for more than 70% less than the nanocrystalline of 30nm between 8-70nm.The micron crystalline phase distributes with bar form, and length is 0.5-8 μ m.The vickers hardness number of blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material is 2.6GPa, and yield strength is 690MPa.
Embodiment 2:
According to ferric oxide: aluminium: the mass ratio of chromium is to take by weighing reaction mass at 11: 5: 1; The powder that weighs up ball mill for dry grinding 8 hours, is pressed down at the pressure of 60MPa with pressing machine in the stainless steel mould of then reaction mass that mixes being packed into and processes the reaction base substrate.1.5 kilograms of reaction base substrates are put into the copper mold of reactor, and detonator is placed in the base substrate bottom, and (account for 0.13% of reaction mass mass percent, sulphur: aluminium: Manganse Dioxide: the mass ratio of saltpetre is 1.25: 2: 1: 2).Under the room temperature with the argon purge reaction vessel with the air in the amount discharge container, by the time temperature rises to exhaust once more after 200 ℃ of insulation half an hour, the argon gas that charges into 5MPa then continues heating.When temperature reached 260 ℃ of left and right sides, a large amount of heat was emitted in the detonator reaction, thus the reaction of initiation reaction storeroom.Reaction can be accomplished in tens seconds, and reaction product furnace cooling under argon shield takes out after room temperature, with the by product Al of surface coverage
2O
3Peel off removal.The as cast condition Fe-Al-Cr material of preparation is put into heat treatment furnace through 900 ℃, after 12 hours isothermal processes, prepare blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material.Characterize through X-ray diffraction technology and transmission electron microscope, this material has Fe
3The unordered body-centered cubic structure of Al does not have other impurity phases.The grain-size of nanometer crystalline phase wherein accounts for more than 75% less than the nanocrystalline of 30nm between 5-70nm.The micron crystalline phase distributes with bar form, and length is 0.5-10 μ m.The vickers hardness number of blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material is 2.6GPa, and yield strength is 780MPa.
Embodiment 3:
According to ferric oxide: aluminium: the mass ratio of chromium is to take by weighing reaction mass at 7: 3: 0.8; The powder that weighs up ball mill for dry grinding 8 hours, is pressed down at the pressure of 50MPa with pressing machine in the stainless steel mould of then reaction mass that mixes being packed into and processes the reaction base substrate.2 kilograms of reaction base substrates are put into the copper mold of reactor, and detonator is placed in the base substrate bottom, and (account for 0.1% of reaction mass mass percent, sulphur: aluminium: Manganse Dioxide: the mass ratio of saltpetre is 1.25: 3: 1: 2).Under the room temperature with the argon purge reaction vessel with the air in the amount discharge container, by the time temperature rises to exhaust once more after 200 ℃ of insulation half an hour, the argon gas that charges into 6MPa then continues heating.When temperature reached 260 ℃ of left and right sides, a large amount of heat was emitted in the detonator reaction, thus the reaction of initiation reaction storeroom.Reaction can be accomplished in tens seconds, and reaction product furnace cooling under argon shield takes out after room temperature, with the by product Al of surface coverage
2O
3Peel off removal.The as cast condition Fe-Al-Cr material of preparation is put into heat treatment furnace through 1000 ℃, after 8 hours isothermal processes, prepare blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material.Characterize through X-ray diffraction technology and transmission electron microscope, this material has Fe
3The unordered body-centered cubic structure of Al does not have other impurity phases.The grain-size of nanometer crystalline phase wherein accounts for more than 71% less than the nanocrystalline of 30nm between 5-70nm.The micron crystalline phase distributes with bar form, and length is 0.8-10 μ m.The vickers hardness number of blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material is 2.9GPa, and yield strength is 810MPa.
Claims (3)
1. blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material, the composition that it is characterized in that material is Fe70-80%, Al 10-15%, Cr 5-20%; The diameter of material can reach 150～200mm, and thickness reaches 8～12mm; The grain-size of nanometer crystalline phase wherein accounts for more than 70～75% less than the nanocrystalline of 30nm between 5～80nm in the material; The micron crystalline phase distributes with bar form, and length is 0.5～10 μ m; Vickers hardness number is 2.5～3.0GPa; Yield strength is 680～810Mpa.
2. blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr preparation methods the steps include:
(1) mass ratio according to ferric oxide, aluminium, chromium is 24～7: 11～3.5: 0.8～1.2 ratio takes by weighing reaction mass;
(2), press down at the pressure of 30～60MPa in the mould of then reaction mass that mixes being packed into and process base substrate with the powder that takes by weighing dry grinding 8～16 hours; Pack into 1～2 kilogram of base substrate that presses in the reactor and put into detonator, detonator accounts for the 0.1-0.2% of reaction mass mass percent;
(3) at room temperature use the argon purge reaction vessel with the air post-heating in the amount discharge container, by the time temperature rises to exhaust once more after 200 ℃ of insulation half an hour, and the argon gas that charges into 3～6MPa then continues heating.When temperature reaches 260-320 ℃; A large amount of heat is emitted in the detonator reaction; Thereby the reaction of initiation reaction storeroom; The reaction melt in-situ deposition is in high heat conduction large size copper mold; Be reflected in tens seconds and accomplish; Reaction product is taken out material after under argon shield, cooling to room temperature with the furnace, with the by product Al of surface coverage
2O
3Peel off removal;
(4) the as cast condition Fe-Al-Cr material of preparation is put into chamber type electric resistance furnace and is carried out 800～1000 ℃ of isothermal processes 8-24 hours after, prepare blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr material.
3. blocks of large micron crystalline substance/nanocrystalline two-phase Fe-Al-Cr preparation methods according to claim 2, the mass ratio that it is characterized in that sulphur in the detonator, aluminium, Manganse Dioxide, saltpetre is 1.25: 1～3: 1: 2.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747298A (en) * | 2012-06-06 | 2012-10-24 | 兰州理工大学 | Austenitic stainless steel and preparation method |
| CN105039978A (en) * | 2015-08-05 | 2015-11-11 | 南京航空航天大学 | Method for preparing Fe-Al-Cr alloy layer through combination of magnetron sputtering aluminizing, arc-added glow chromizing and recoil ion implantation |
| CN111778441A (en) * | 2020-07-09 | 2020-10-16 | 兰州理工大学 | Preparation method of ultrahigh-strength and plastic 1045 steel |
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| CN101818307A (en) * | 2009-04-03 | 2010-09-01 | 兰州理工大学 | Fe-Al-Cr blocky nanocrystalline material and preparation method thereof |
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| CN101818307A (en) * | 2009-04-03 | 2010-09-01 | 兰州理工大学 | Fe-Al-Cr blocky nanocrystalline material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102747298A (en) * | 2012-06-06 | 2012-10-24 | 兰州理工大学 | Austenitic stainless steel and preparation method |
| CN105039978A (en) * | 2015-08-05 | 2015-11-11 | 南京航空航天大学 | Method for preparing Fe-Al-Cr alloy layer through combination of magnetron sputtering aluminizing, arc-added glow chromizing and recoil ion implantation |
| CN111778441A (en) * | 2020-07-09 | 2020-10-16 | 兰州理工大学 | Preparation method of ultrahigh-strength and plastic 1045 steel |
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Application publication date: 20120208 |