CN107299269B - A kind of W-Cr-Al composite material and preparation method of resistance to high temperature oxidation - Google Patents
A kind of W-Cr-Al composite material and preparation method of resistance to high temperature oxidation Download PDFInfo
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- CN107299269B CN107299269B CN201710436304.6A CN201710436304A CN107299269B CN 107299269 B CN107299269 B CN 107299269B CN 201710436304 A CN201710436304 A CN 201710436304A CN 107299269 B CN107299269 B CN 107299269B
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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
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- 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
Abstract
The invention discloses a kind of W-Cr-Al composite material and preparation methods of resistance to high temperature oxidation, wherein the doped alloys element of resistance to high temperature oxidation W-Cr-Al composite material is Cr and Al, each component is constituted by mass percentage are as follows: Cr 8-16%, Al 1-4%, surplus W.The doped alloys interphase powder into W powder, prepares alloy sample by discharge plasma sintering.In the oxygen containing atmosphere of 800-1200 DEG C of high temperature, Cr and Al are aoxidized form Cr respectively2O3With Al2O3Fine and close passivation protection layer prevents oxygen from further going deep into, to significantly improve antioxygenic property of the W sill in high temperature aerobic environment.
Description
One, 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 composite material and preparation method.
Two, background technique
Controlled thermonuclear fusion can be the ideal energy in human society future, 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 coolant failure occurs in fusion reactor, air will enter in the reactor of vacuum, and PFMs will
Bear 1200 DEG C of transient temperature.In practical applications, in humid air the synergistic effect of oxygen and vapor so that tungsten material
Rapid oxidation.In order to research and develop the intelligent tungsten alloy of self-passivation, researchers at home and abroad use doping Cr element to the antioxygen of tungsten
Changing performance is improved.W-Cr bianry alloy forms compact oxidation layer Cr2O3, but it is exposed to Cr in high-temperature oxidation environment for a long time2O3
Oxide layer is difficult to keep stable, is unable to maintain that long-term passivation.Therefore active element is added into W-Cr Binary Alloy System, mentions
The antioxygenic property of high alloy.
Currently, research report, which adulterates the more active element of W-Cr alloy, mainly Ti, Y, Ni element etc..However use Al
Element doping W-Cr alloy has not been reported.Cr, Al doping W based alloy can significantly improve the antioxygenic property of W alloy.
Three, summary of the invention
The present invention is intended to provide a kind of W-Cr-Al composite material and preparation method of resistance to high temperature oxidation, through oversintering system
The resistance to high temperature oxidation of standby resistance to high temperature oxidation W-Cr-Al composite material is significantly improved with water resistant mist high temperature oxidation resistance.
The W-Cr-Al composite material of resistance to high temperature oxidation of the present invention, doped alloys element are Cr and Al, and wherein each component is pressed
Mass percent is constituted are as follows: Cr 8-16%, Al 1-4%, surplus W.
The preparation method of the W-Cr-Al composite material of resistance to high temperature oxidation of the present invention, includes the following steps:
Step 1: powder processed
Tungsten powder and Cr/Al mesophase alloy powder are stirred 2 hours in 400 revs/min of mixed powder machine, obtain W-
Cr-Al composite powder；During being stirred, the one third of the fixing fabric structure of powder in 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 powder is packed into graphite jig, then graphite jig is put into discharge plasma sintering furnace, room temperature
Under to sintering stove evacuation, be successively warming up to 1200 DEG C of heat preservations 15 minutes, 1600 DEG C of heat preservation 3min, be down to room after heat preservation
Temperature to get arrive W-Cr-Al composite material.
In sintering process, heating rate is 100 DEG C/min, and rate of temperature fall is 100 DEG C/min.
In sintering process, it is filled with argon gas when being warming up to 1000 DEG C as protection gas and carries out negative pressure sintering, is controlled in sintering
Pressure is no more than 47.3MPa.
The 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 are aoxidized form Cr respectively2O3With Al2O3Fine and close passivation
Protective layer prevents oxygen from further going deep into, to improve W matrix antioxygenic property.Compared with traditional mechanical ball mill preparation,
Cr/Al mesophase alloy powder can advantageous inhibition Cr, Al element activity, be oxidized when preventing material from preparing.Sintering is tied again
Cr and W is spread 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-die.In high-temperature oxidation process, Cr and Al are aoxidized form Cr respectively2O3With Al2O3It is fine and close
Passivation protection layer, prevent oxygen further deeply, to improve W matrix antioxygenic property.With study more W- at present
Cr bianry alloy is compared, and doping Al element has adsorbed impurity, surely changes Cr2O3Oxide layer.
Four, specific embodiment
Embodiment 1:
Resistance to high temperature oxidation W-Cr-Al composite material in the present embodiment, doped alloys element are Cr and Al, wherein each component
It constitutes by mass percentage are as follows: Cr 8%, Al 4%, surplus W.
In the present embodiment resistance to high temperature oxidation W-Cr-Al composite material the preparation method is as follows:
1, powder processed: tungsten powder and Cr/Al mesophase alloy powder are stirred 2 hours in 400 revs/min of mixed powder machine,
Obtain W-Cr-Al composite powder；The particle size of tungsten powder is 1 micron, and the particle size of Cr/Al mesophase alloy powder is 10 micro-
Rice.
2, it is sintered: W-Cr-Al composite powder being packed into graphite jig, then graphite jig is put into discharge plasma sintering furnace
In, at room temperature to sintering stove evacuation, 1200 DEG C of heat preservations 15 minutes, 1600 DEG C of heat preservation 3min are successively warming up to, are being warming up to
It is filled with argon gas at 1000 DEG C as protection gas and carries out negative pressure sintering, control pressure is no more than 47.3MPa in sintering；After heat preservation
Room temperature is down to get W-Cr-Al composite material is arrived.
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 are aoxidized form Cr respectively2O3With Al2O3Fine and close passivation
Protective layer prevents oxygen from further going deep into, to improve W matrix antioxygenic property.W-Cr-Al composite material has 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 composite material in the present embodiment, doped alloys element are Cr and Al, wherein each component
It constitutes by mass percentage are as follows: Cr 12%, Al 2%, surplus W.
In the present embodiment resistance to high temperature oxidation W-Cr-Al composite material the preparation method is as follows:
1, powder processed: tungsten powder and Cr/Al mesophase alloy powder are stirred 2 hours in 400 revs/min of mixed powder machine,
Obtain W-Cr-Al composite powder；The particle size of tungsten powder is 5 microns, and the particle size of Cr/Al mesophase alloy powder is 15 micro-
Rice.
2, it is sintered: W-Cr-Al composite powder being packed into graphite jig, then graphite jig is put into discharge plasma sintering furnace
In, at room temperature to sintering stove evacuation, 1200 DEG C of heat preservations 15 minutes, 1600 DEG C of heat preservation 3min are successively warming up to, are being warming up to
It is filled with argon gas at 1000 DEG C as protection gas and carries out negative pressure sintering, control pressure is no more than 47.3MPa in sintering；After heat preservation
Room temperature is down to get W-Cr-Al composite material is arrived.
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 are aoxidized form Cr respectively2O3With Al2O3Fine and close passivation
Protective layer prevents oxygen from further going deep into, to improve W matrix antioxygenic property.W-Cr-Al composite material has 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 composite material in the present embodiment, doped alloys element are Cr and Al, wherein each component
It constitutes by mass percentage are as follows: Cr 12%, Al 4%, surplus W.
The preparation method of resistance to high temperature oxidation W-Cr-Al composite material, includes the following steps: in the present embodiment
1, powder processed: tungsten powder and Cr/Al mesophase alloy powder are stirred 2 hours in 400 revs/min of mixed powder machine,
Obtain W-Cr-Al composite powder；The particle size of tungsten powder is 10 microns, and the particle size of Cr/Al mesophase alloy powder is 20 micro-
Rice.
2, it is sintered: W-Cr-Al composite powder being packed into graphite jig, then graphite jig is put into discharge plasma sintering furnace
In, at room temperature to sintering stove evacuation, 1200 DEG C of heat preservations 15 minutes, 1600 DEG C of heat preservation 3min are successively warming up to, are being warming up to
It is filled with argon gas at 1000 DEG C as protection gas and carries out negative pressure sintering, control pressure is no more than 47.3MPa in sintering；After heat preservation
Room temperature is down to get W-Cr-Al composite material is arrived.
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 are aoxidized form Cr respectively2O3With Al2O3Fine and close passivation
Protective layer prevents oxygen from further going deep into, to improve W matrix antioxygenic property.W-Cr-Al composite material has 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 (3)
1. a kind of preparation method of the W-Cr-Al composite material of resistance to high temperature oxidation, it is characterised in that include the following steps:
Step 1: powder processed
Tungsten powder and Cr/Al mesophase alloy powder are stirred 2 hours in 400 revs/min of mixed powder machine, obtain W-Cr-Al
Composite powder；
Step 2: sintering
W-Cr-Al composite powder is packed into graphite jig, then graphite jig is put into discharge plasma sintering furnace, it is right at room temperature
It is sintered stove evacuation, 1200 DEG C of heat preservations 15 minutes, 1600 DEG C of heat preservation 3min is successively warming up to, room temperature is down to after heat preservation, i.e.,
W-Cr-Al composite material is obtained, each component is constituted by mass percentage are as follows: Cr 8-16%, Al 1-4%, surplus W；
In sintering process, heating rate is 100 DEG C/min, and rate of temperature fall is 100 DEG C/min.
2. preparation method according to claim 1, 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.
3. preparation method according to claim 1, it is characterised in that:
In sintering process, it is filled with argon gas when being warming up to 1000 DEG C as protection gas and carries out negative pressure sintering, controls pressure in sintering
No more than 47.3MPa.
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| CN201710436304.6A CN107299269B (en) | 2017-06-12 | 2017-06-12 | A kind of W-Cr-Al composite material and preparation method of resistance to high temperature oxidation |
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| CN107299269B true CN107299269B (en) | 2019-01-11 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
Citations (2)
| 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 |
-
2017
- 2017-06-12 CN CN201710436304.6A patent/CN107299269B/en active Active
Patent Citations (2)
| 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)
| Title |
|---|
| 机械合金化法制备不同Cr含量的W-Cr纳米合金粉末;肖鹏等;《中国有色金属学报》;20071130;第17卷(第11期);第1780页 |
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