CN107299269A - A kind of W Cr Al composites of resistance to high temperature oxidation and preparation method thereof - Google Patents

A kind of W Cr Al composites of resistance to high temperature oxidation and preparation method thereof Download PDF

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Publication number
CN107299269A
CN107299269A CN201710436304.6A CN201710436304A CN107299269A CN 107299269 A CN107299269 A CN 107299269A CN 201710436304 A CN201710436304 A CN 201710436304A CN 107299269 A CN107299269 A CN 107299269A
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powder
composites
high temperature
sintering
preparation
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CN107299269B (en
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罗来马
黄科
刘家琴
昝祥
刘东光
朱晓勇
吴玉程
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Hefei University of Technology
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Hefei University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04—Alloys based on tungsten or molybdenum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses W Cr Al composites of a kind of resistance to high temperature oxidation and preparation method thereof, the wherein doped alloys element of resistance to high temperature oxidation W Cr Al composites is Cr and Al, and each component is configured to by mass percentage：Cr 8 16%, Al 1 4%, surplus is W.Into W powder, doped alloys interphase powder, alloy sample is prepared by discharge plasma sintering.In the oxygen containing atmosphere of 800 1200 DEG C of high temperature, Cr and Al aoxidizes to form Cr respectively2O3With Al2O3Fine and close passivation protection layer, prevents oxygen from further going deep into, so as to significantly improve antioxygenic property of the W sills in high temperature aerobic environment.

Description

A kind of W-Cr-Al composites of resistance to high temperature oxidation and preparation method thereof
First, technical field
The present invention relates to a kind of metallic composite and preparation method thereof, specifically a kind of W- of resistance to high temperature oxidation Cr-Al composites and preparation method thereof.
2nd, background technology
Controlled thermonuclear fusion can be following preferable energy of human society, it is considered to be can effectively solve human future energy One of main outlet of source demand.Tungsten have high-melting-point, highly thermally conductive, minimum to the adsorbance of deuterium and tritium, radioactivity is low, not with H Reaction, the features such as anti-sputtering ability is strong, from the point of view of current research, tungsten is considered as most promising PFMs (Plasma Facing Materials).But when the accident of cooling agent failure occurs in fusion reactor, air will enter in the reactor of vacuum, and PFMs will Bear 1200 DEG C of transient temperature.In actual applications, the synergy of oxygen and vapor causes tungsten material in humid air Rapid oxidation.In order to research and develop the intelligent tungsten alloy of self-passivation, domestic and international researcher employs antioxygen of the doping Cr elements to tungsten Changing performance is improved.W-Cr bianry alloys formation compact oxidation layer Cr2O3, but Cr in high-temperature oxidation environment is exposed to for a long time2O3 Oxide layer is difficult to keep stable, it is impossible to maintain long-term passivation.Therefore active element is added into W-Cr Binary Alloy Systems, carried The antioxygenic property of high alloy.
At present, the more active element of research report doping W-Cr alloys mainly has Ti, Y, Ni element etc..But use Al Element doping W-Cr alloys have no report.Cr, Al doping W based alloys can significantly improve the antioxygenic property of W alloy.
3rd, the content of the invention
The present invention is intended to provide W-Cr-Al composites of a kind of resistance to high temperature oxidation and preparation method thereof, through oversintering system The resistance to high temperature oxidation of standby resistance to high temperature oxidation W-Cr-Al composites is significantly improved with water resistant mist high temperature oxidation resistance.
The W-Cr-Al composites of resistance to high temperature oxidation of the present invention, its doped alloys element is Cr and Al, and wherein each component is pressed Mass percent is configured to：Cr 8-16%, Al 1-4%, surplus is W.
The preparation method of the W-Cr-Al composites of resistance to high temperature oxidation of the present invention, comprises the following steps：
Step 1：Powder processed
Tungsten powder is stirred with Cr/Al mesophase alloys powder in 400 revs/min of mixed powder machine and mixed 2 hours, W- is obtained Cr-Al composite powders；Stir in mixed process, the fixing fabric structure of powder is 1/3rd of batch mixing tank volume.
The particle size of tungsten powder is 1-10 microns, and the particle size of Cr/Al mesophase alloy powder is 10-20 microns.
Step 2：Sintering
W-Cr-Al composite powders are loaded into graphite jig, then graphite jig are put into discharge plasma sintering stove, room temperature Under to sintering stove evacuation, be warming up to successively 1200 DEG C be incubated 15 minutes, 1600 DEG C insulation 3min, insulation terminate after be down to room Temperature, that is, obtain W-Cr-Al composites.
In sintering process, heating rate is 100 DEG C/min, and rate of temperature fall is 100 DEG C/min.
In sintering process, argon gas is filled with when being warming up to 1000 DEG C and carries out controlling in negative pressure sintering, sintering as protection gas Pressure is no more than 47.3MPa.
Beneficial effects of the present invention are embodied in：
In the oxygen containing atmosphere of 800-1200 DEG C of high temperature, Cr and Al aoxidizes to form Cr respectively2O3With Al2O3Fine and close passivation Protective layer, prevents oxygen from further going deep into, so as to improve W matrix antioxygenic properties.Compared with prepared by traditional mechanical ball mill, Cr/Al mesophase alloys powder can be favourable suppression Cr, Al element activity, prevent when material from preparing be oxidized.Sintering is tied again Cr and W spreads in the brilliant following insulating process of temperature, forms unlimited substitution solid solution, and solution strengthening improves hardness, simultaneously Improve the antioxygenic property of W intra-dies.In high-temperature oxidation process, Cr and Al aoxidizes to form Cr respectively2O3With Al2O3It is fine and close Passivation protection layer, prevent oxygen further deeply, so as to improve W matrix antioxygenic properties.With studying more W- at present Cr bianry alloys are compared, and doping Al elements have adsorbed impurity, surely change Cr2O3Oxide layer.
4th, embodiment
Embodiment 1：
Resistance to high temperature oxidation W-Cr-Al composites in the present embodiment, its doped alloys element is Cr and Al, wherein each component It is configured to by mass percentage：Cr 8%, Al 4%, surplus is W.
The preparation method of resistance to high temperature oxidation W-Cr-Al composites is as follows in the present embodiment：
1st, powder processed：Tungsten powder is stirred with Cr/Al mesophase alloys powder in 400 revs/min of mixed powder machine and mixed 2 hours, Obtain W-Cr-Al composite powders；The particle size of tungsten powder is 1 micron, and the particle size of Cr/Al mesophase alloy powder is micro- for 10 Rice.
2nd, sinter：W-Cr-Al composite powders are loaded into graphite jig, then graphite jig is put into discharge plasma sintering stove In, at room temperature to sintering stove evacuation, 1200 DEG C are warming up to successively and is incubated 15 minutes, 1600 DEG C of insulation 3min, is being warming up to Argon gas is filled with 1000 DEG C to carry out controlling pressure to be no more than 47.3MPa in negative pressure sintering, sintering as protection gas；After insulation terminates Room temperature is down to, that is, obtains W-Cr-Al composites.
In sintering process, heating rate is 100 DEG C/min, and rate of temperature fall is 100 DEG C/min.
In the oxygen containing atmosphere of 800-1200 DEG C of high temperature, Cr and Al aoxidizes to form Cr respectively2O3With Al2O3Fine and close passivation Protective layer, prevents oxygen from further going deep into, so as to improve W matrix antioxygenic properties.W-Cr-Al composites have good High temperature oxidation resistance, is the 6%-13% of pure tungsten gain in weight in 20 hours gains in weight of 800-1200 DEG C of high-temperature oxydation.
Embodiment 2：
Resistance to high temperature oxidation W-Cr-Al composites in the present embodiment, its doped alloys element is Cr and Al, wherein each component It is configured to by mass percentage：Cr 12%, Al 2%, surplus is W.
The preparation method of resistance to high temperature oxidation W-Cr-Al composites is as follows in the present embodiment：
1st, powder processed：Tungsten powder is stirred with Cr/Al mesophase alloys powder in 400 revs/min of mixed powder machine and mixed 2 hours, Obtain W-Cr-Al composite powders；The particle size of tungsten powder is 5 microns, and the particle size of Cr/Al mesophase alloy powder is micro- for 15 Rice.
2nd, sinter：W-Cr-Al composite powders are loaded into graphite jig, then graphite jig is put into discharge plasma sintering stove In, at room temperature to sintering stove evacuation, 1200 DEG C are warming up to successively and is incubated 15 minutes, 1600 DEG C of insulation 3min, is being warming up to Argon gas is filled with 1000 DEG C to carry out controlling pressure to be no more than 47.3MPa in negative pressure sintering, sintering as protection gas；After insulation terminates Room temperature is down to, that is, obtains W-Cr-Al composites.
In sintering process, heating rate is 100 DEG C/min, and rate of temperature fall is 100 DEG C/min.
In the oxygen containing atmosphere of 800-1200 DEG C of high temperature, Cr and Al aoxidizes to form Cr respectively2O3With Al2O3Fine and close passivation Protective layer, prevents oxygen from further going deep into, so as to improve W matrix antioxygenic properties.W-Cr-Al composites have good High temperature oxidation resistance, is the 6%-13% of pure tungsten gain in weight in 20 hours gains in weight of 800-1200 DEG C of high-temperature oxydation.
Embodiment 3：
Resistance to high temperature oxidation W-Cr-Al composites in the present embodiment, its doped alloys element is Cr and Al, wherein each component It is configured to by mass percentage：Cr 12%, Al 4%, surplus is W.
The preparation method of resistance to high temperature oxidation W-Cr-Al composites, comprises the following steps in the present embodiment：
1st, powder processed：Tungsten powder is stirred with Cr/Al mesophase alloys powder in 400 revs/min of mixed powder machine and mixed 2 hours, Obtain W-Cr-Al composite powders；The particle size of tungsten powder is 10 microns, and the particle size of Cr/Al mesophase alloy powder is micro- for 20 Rice.
2nd, sinter：W-Cr-Al composite powders are loaded into graphite jig, then graphite jig is put into discharge plasma sintering stove In, at room temperature to sintering stove evacuation, 1200 DEG C are warming up to successively and is incubated 15 minutes, 1600 DEG C of insulation 3min, is being warming up to Argon gas is filled with 1000 DEG C to carry out controlling pressure to be no more than 47.3MPa in negative pressure sintering, sintering as protection gas；After insulation terminates Room temperature is down to, that is, obtains W-Cr-Al composites.
In sintering process, heating rate is 100 DEG C/min, and rate of temperature fall is 100 DEG C/min.
In the oxygen containing atmosphere of 800-1200 DEG C of high temperature, Cr and Al aoxidizes to form Cr respectively2O3With Al2O3Fine and close passivation Protective layer, prevents oxygen from further going deep into, so as to improve W matrix antioxygenic properties.W-Cr-Al composites have good High temperature oxidation resistance, is the 6%-13% of pure tungsten gain in weight in 20 hours gains in weight of 800-1200 DEG C of high-temperature oxydation.

Claims (5)

1. the W-Cr-Al composites of a kind of resistance to high temperature oxidation, it is characterised in that each component is configured to by mass percentage：Cr 8-16%, Al 1-4%, surplus are W.
2. a kind of preparation method of the W-Cr-Al composites of the resistance to high temperature oxidation described in claim 1, it is characterised in that including Following steps：
Step 1：Powder processed
Tungsten powder is stirred with Cr/Al mesophase alloys powder in 400 revs/min of mixed powder machine and mixed 2 hours, W-Cr-Al is obtained Composite powder；
Step 2：Sintering
W-Cr-Al composite powders are loaded into graphite jig, then graphite jig is put into discharge plasma sintering stove, it is right at room temperature Stove evacuation is sintered, 1200 DEG C are warming up to successively and is incubated 15 minutes, 1600 DEG C of insulation 3min, insulation is down to room temperature after terminating, i.e., Obtain W-Cr-Al composites.
3. preparation method according to claim 2, it is characterised in that：
The particle size of tungsten powder is 1-10 microns, and the particle size of Cr/Al mesophase alloy powder is 10-20 microns.
4. preparation method according to claim 2, it is characterised in that：
In sintering process, heating rate is 100 DEG C/min, and rate of temperature fall is 100 DEG C/min.
5. preparation method according to claim 2, it is characterised in that：
In sintering process, argon gas is filled with when being warming up to 1000 DEG C and carries out controlling pressure in negative pressure sintering, sintering as protection gas No more than 47.3MPa.
CN201710436304.6A 2017-06-12 2017-06-12 A kind of W-Cr-Al composite material and preparation method of resistance to high temperature oxidation Active CN107299269B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108817387A (en) * 2018-07-09 2018-11-16 合肥工业大学 A kind of preparation method of the tungsten-based composite material with high rigidity and high temperature oxidation resistance
CN113528987A (en) * 2021-06-18 2021-10-22 河钢承德钒钛新材料有限公司 Tungsten alloy composite material and 3D printing method thereof
CN114559040A (en) * 2022-03-08 2022-05-31 北京工业大学 Aluminum-containing self-passivated tungsten alloy and preparation method and application thereof

Citations (2)

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Publication number Priority date Publication date Assignee Title
GB1086708A (en) * 1966-02-01 1967-10-11 Gen Electric Co Ltd Improvements in or relating to metal bodies and their manufacture
CN101126137A (en) * 2007-09-26 2008-02-20 西安理工大学 Method for preparing chromium-tungsten solid solution alloy material by powder pressure sintering

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1086708A (en) * 1966-02-01 1967-10-11 Gen Electric Co Ltd Improvements in or relating to metal bodies and their manufacture
CN101126137A (en) * 2007-09-26 2008-02-20 西安理工大学 Method for preparing chromium-tungsten solid solution alloy material by powder pressure sintering

Non-Patent Citations (1)

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Title
肖鹏等: "机械合金化法制备不同Cr含量的W-Cr纳米合金粉末", 《中国有色金属学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108817387A (en) * 2018-07-09 2018-11-16 合肥工业大学 A kind of preparation method of the tungsten-based composite material with high rigidity and high temperature oxidation resistance
CN108817387B (en) * 2018-07-09 2020-02-14 合肥工业大学 Preparation method of tungsten-based composite material with high hardness and high-temperature oxidation resistance
CN113528987A (en) * 2021-06-18 2021-10-22 河钢承德钒钛新材料有限公司 Tungsten alloy composite material and 3D printing method thereof
CN114559040A (en) * 2022-03-08 2022-05-31 北京工业大学 Aluminum-containing self-passivated tungsten alloy and preparation method and application thereof

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