CN108359919B - A kind of mandatory method for oxidation preparing the pure magnesium of gradient structure and magnesium alloy - Google Patents
A kind of mandatory method for oxidation preparing the pure magnesium of gradient structure and magnesium alloy Download PDFInfo
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- CN108359919B CN108359919B CN201810114797.6A CN201810114797A CN108359919B CN 108359919 B CN108359919 B CN 108359919B CN 201810114797 A CN201810114797 A CN 201810114797A CN 108359919 B CN108359919 B CN 108359919B
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000011777 magnesium Substances 0.000 title claims abstract description 47
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 45
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 15
- 230000003647 oxidation Effects 0.000 title claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 75
- 239000002344 surface layer Substances 0.000 claims abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 239000001307 helium Substances 0.000 claims abstract description 17
- 229910052734 helium Inorganic materials 0.000 claims abstract description 17
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000005684 electric field Effects 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 5
- 238000011282 treatment Methods 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- 238000004321 preservation Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 abstract description 24
- 239000000463 material Substances 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 13
- 239000010410 layer Substances 0.000 description 11
- 238000005299 abrasion Methods 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000008901 benefit Effects 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000013532 laser treatment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010010 raising Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The present invention relates to a kind of mandatory method for oxidation for preparing the pure magnesium of gradient structure and magnesium alloy, it is passed through the helium of different volumes ratio and the mixed gas (helium: oxygen=1:1~1:10) of oxygen in the lehr first, the furnace pressure (0.1~1MPa) in annealing furnace is controlled simultaneously, then it is made annealing treatment under compound outfield, apply ultrasonic wave (30KHz~50KHz) when annealing heat preservation, apply electric field (5~10KV/m) when furnace cooling, obtaining crystallite dimension when away from 0~0.5cm of surface layer is 20~100 μm, crystallite dimension is 100~300 μm when apart from 0.5~1.5cm of surface layer, crystallite dimension is greater than 300 μm of the pure magnesium of gradient structure and magnesium alloy when being greater than 1.5 apart from surface layer, improve the hardness of material, oxidative resistance and resistance to Mill property.The equipment that the present invention uses is simple, production cost is low, is suitable for large-scale production.
Description
Technical field
The invention belongs to metal heat treatmet fields, and in particular to a kind of to prepare the mandatory of the pure magnesium of gradient structure and magnesium alloy
Method for oxidation.
Background technique
Magnesium and magnesium alloy are structural metallic materials most light at present, it has, and density is low, machinability is good, damping shock absorption
Performance is good, good heat conductivity, specific stiffness and specific strength are high, part size is stable, effectiveness is good, good recycling etc. is a series of
Advantage.Magnesium and magnesium alloy are widely used in automobile, aircraft and communication product, 3C Product communication field and biomaterial medicine etc.
Field.Therefore magnesium alloy is described as " green engineering material that 21 century most develops future " by someone.
Since magnesium is the active element of comparison, easily aoxidize in air, the pure magnesium of traditional casting and magnesium alloy it is resistance to
Oxidisability is poor, and the method for the surface anti-oxidation corrosion treatment of magnesium alloy includes chemical conversion, anodic oxidation, coating, physics
Vapor deposition, laser treatment, ion implanting etc., complex process is at high cost and have certain pollution to environment, significantly limits
The application field of magnesium and magnesium alloy.It is therefore desirable to develop, a kind of cost is relatively low, pollution-free and effective raisings magnesium and magnesium conjunction
Oxidative resistance, the method for hardness and wearability of gold, to expand the application field of magnesium and magnesium alloy, have great importance and
Necessity.
Summary of the invention
To solve the problems, such as that oxidizable current pure magnesium and magnesium alloy, hardness and wearability are poor, the present invention provides one
Kind prepares the mandatory method for oxidation of the pure magnesium of gradient structure and magnesium alloy.
A kind of detailed process of mandatory method for oxidation preparing the pure magnesium of gradient structure and magnesium alloy of the present invention is such as
Under: it is passed through the mixed gas of helium and oxygen in the lehr first, while controlling the furnace pressure in annealing furnace, then annealing furnace is fast
Speed is warming up to annealing temperature, makes annealing treatment under compound outfield to the pure magnesium of as cast condition and magnesium alloy, applies when annealing is kept the temperature super
Sound wave, when furnace cooling, apply electric field, obtain the pure magnesium and magnesium alloy of gradient structure, improve hardness, the oxidative resistance of material
And wearability.
Helium in the mixed gas for being passed through helium and oxygen in the lehr: the volume ratio of oxygen is 1:1~1:10.
Pressure in the control annealing furnace is 0.1~1MPa.
The frequency for applying ultrasonic wave when annealing heat preservation is 30KHz~50KHz.
The current density for applying electric field when the furnace cooling is 5~10KV/m.
The annealing furnace heating rate is 100~300 DEG C/min.
The annealing temperature is 450 DEG C~570 DEG C, and soaking time is 30min~120min.
Crystallite dimension reaches 20~100 μm when the gradient structure is away from 0~0.5cm of surface layer (surface layer), apart from surface layer
Crystallite dimension reaches 100~300 μm when 0.5~1.5cm (internal layer), and crystallite dimension is greater than 300 μ when being greater than 1.5cm apart from surface layer
m。
The method of the present invention the utility model has the advantages that
The present invention makes it obtain gradient group at high temperature the logical oxygen that pressurizes in the pure magnesium of as cast condition and magnesium alloy annealing process
The pure magnesium and magnesium alloy knitted, and then achieve the effect that crystal grain refinement (as shown in Figure 1), its hardness, resistance to oxidation are improved to reach
The purpose of property and wearability.Apply ultrasonic wave in annealing insulating process, apply electric field energy in cooling procedure and keep oxygen abundant
Ground enters sample, to change the grain size on pure magnesium and magnesium alloy surface layer to reach and improve its hardness, oxidative resistance and resistance to
The purpose of mill property.The gradient structure that crystal grain refinement generates equiax crystal is conducive to improve its hardness, to improve the wearability of material；
The gradient structure of the oxide and generation crystal grain refinement of oxygen and magnesium Surface Realize is conducive to completely cut off sample re-oxidation under high temperature
And then improve oxidative resistance.The present invention has easy to operate, at low cost, free of contamination advantage simultaneously.
Detailed description of the invention
Fig. 1 is the metallograph of the pure magnesium of as cast condition (99.95wt.%) made from embodiment 4.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, a kind of pure magnesium of acquisition gradient structure and magnesium alloy
Mandatory oxidation technology specific implementation process it is as follows: be passed through the gaseous mixture of different proportion helium and oxygen in the lehr first
Body, while the furnace pressure in annealing furnace is controlled, then being made annealing treatment under compound outfield, annealing applies ultrasonic wave when keeping the temperature,
Apply electric field when furnace cooling, obtain the pure magnesium and magnesium alloy of gradient structure, improves the hardness of material, oxidative resistance and wear-resisting
Property.
Embodiment 1
The pure magnesium of as cast condition (99.95wt.%) sample is taken to be put into annealing furnace, when progress annealing temperature is 450 DEG C, keeps the temperature respectively
Between be 120min annealing experiment.Wherein helium: the volume ratio of oxygen is 1:1, and pressure is 0.1MPa, ultrasonic wave frequency in annealing furnace
Rate is 30KHz, electric field strength 5KV/m, and control annealing furnace heating rate is 100 DEG C/min.Then Vickers hardness is carried out to it
With oxidative resistance and wearability test, the results showed that reach 50 μm away from surface layer grain size, internal layer crystallite dimension reaches 162 μ
M, Vickers hardness 49.3, its hardness improves about 37.6% compared with the pure magnesium of as cast condition, and oxidative resistance improves about 79.3%,
Coefficient of friction reaches 0.48, abrasion loss 0.34%.
Embodiment 2
The pure magnesium of as cast condition (99.95wt.%) sample is taken to be put into annealing furnace, when progress annealing temperature is 570 DEG C of heat preservations respectively
Between be 45min annealing experiment.Wherein helium: the volume ratio of oxygen is 1:1, and pressure is 0.1MPa, ultrasonic wave frequency in annealing furnace
Rate is 30KHz, electric field strength 5KV/m, and control annealing furnace heating rate is 100 DEG C/min.Then Vickers hardness is carried out to it
With oxidative resistance and wearability test, the results showed that reach 56 μm away from surface layer grain size, internal layer crystallite dimension reaches 178 μ
M, Vickers hardness 50.4, its hardness improves about 45.6% compared with the pure magnesium of as cast condition, and oxidative resistance improves about 74.3%,
Coefficient of friction reaches 0.46, abrasion loss 0.36%.
Embodiment 3
The pure magnesium of as cast condition (99.95wt.%) sample is taken to be put into annealing furnace, progress annealing temperature is 490 DEG C of soaking times
The annealing experiment of 90min.Wherein helium: the volume ratio of oxygen is 1:2, and pressure is 0.2MPa in annealing furnace, and ultrasonic frequency is
35KHz, electric field strength 6KV/m, control annealing furnace heating rate are 100 DEG C/min.Then Vickers hardness and resistance to is carried out to it
Oxidisability and wearability test, the results showed that reach 38 μm away from surface layer grain size, internal layer crystallite dimension reaches 126 μm,
Vickers hardness is 48.8, its hardness improves about 42.5% compared with the pure magnesium of as cast condition, and oxidative resistance improves about 84.9%, friction
Coefficient reaches 0.46, abrasion loss 0.32%.
Embodiment 4
The pure magnesium of as cast condition (99.95wt.%) sample is taken to be put into annealing furnace, progress annealing temperature is 510 DEG C of soaking times
The annealing experiment of 90min.Wherein helium: the volume ratio 1:4 that oxygen is, pressure is 0.4MPa in annealing furnace, and ultrasonic frequency is
40KHz, electric field strength 7KV/m, control annealing furnace heating rate are 200 DEG C/min.Then Vickers hardness and resistance to is carried out to it
Oxidisability and wearability test, the results showed that reach 46 μm away from surface layer grain size, internal layer crystallite dimension reaches 129 μm (such as
Shown in Fig. 1), Vickers hardness 49.3, its hardness improves about 47.9% compared with the pure magnesium of as cast condition, and oxidative resistance improves about
80.3%, coefficient of friction reaches 0.44, and abrasion loss is about 0.30%.
The metallograph of Fig. 1 reflects the pure magnesium of as cast condition (99.95wt.%) after annealing with the effect of crystal grain refinement
Fruit, and gradient structure is formed to achieve the purpose that improve its hardness, oxidative resistance and wearability.
Embodiment 5
The pure magnesium of as cast condition (99.95wt.%) sample is taken to be put into annealing furnace, progress annealing temperature is 520 DEG C of soaking times
The annealing experiment of 100min.Wherein helium: the volume ratio of oxygen is 1:5, and pressure is 0.5MPa in annealing furnace, and ultrasonic frequency is
40KHz, electric field strength 7KV/m, control annealing furnace heating rate are 200 DEG C/min.Then Vickers hardness and resistance to is carried out to it
Oxidisability and wearability test, the results showed that reach 38 μm away from surface layer grain size, internal layer crystallite dimension reaches 114 μm,
Vickers hardness is 51.2, its hardness improves about 46.8% compared with the pure magnesium of as cast condition, and oxidative resistance improves about 86.6%, friction
Coefficient reaches 0.46, and abrasion loss is about 0.30%.
Embodiment 6
It takes as cast condition AZ91D sample to be put into annealing furnace, it is real to carry out the annealing that annealing temperature is 450 DEG C of soaking time 120min
It tests.Wherein helium: the volume ratio 1:6 that oxygen is, pressure is 0.6MPa, ultrasonic frequency 45KHz, electric field strength in annealing furnace
For 7KV/m, control annealing furnace heating rate is 300 DEG C/min.Then Vickers hardness and oxidative resistance and wear-resisting are carried out to it
Property test, the results showed that reach 47 μm away from surface layer grain size, internal layer crystallite dimension reaches 159 μm, and Vickers hardness is
112.8, its hardness improves about 48.4% compared with as cast condition AZ91D, and oxidative resistance improves about 85.3%, and coefficient of friction reaches
0.32, abrasion loss 0.26%.
Embodiment 7
It takes as cast condition AM50A sample to be put into annealing furnace, it is real to carry out the annealing that annealing temperature is 520 DEG C of soaking time 45min
It tests.Wherein helium: the volume ratio 1:8 that oxygen is, pressure is 0.8MPa, ultrasonic frequency 45KHz, electric field strength in annealing furnace
For 8KV/m, control annealing furnace heating rate is 200 DEG C/min.Then Vickers hardness and oxidative resistance and wear-resisting are carried out to it
Property test, the results showed that reach 55 μm away from surface layer grain size, internal layer crystallite dimension reaches 137 μm, Vickers hardness 81.6,
Its hardness improves about 45.8% compared with as cast condition AM50A, and oxidative resistance improves about 83.3%, and coefficient of friction reaches 0.34,
Abrasion loss is 0.28%.
Embodiment 8
It takes as cast condition AS41A sample to be put into annealing furnace, it is real to carry out the annealing that annealing temperature is 490 DEG C of soaking time 75min
It tests.Wherein helium: the volume ratio 1:10 that oxygen is, pressure is 1MPa, ultrasonic frequency 50KHz, electric field strength in annealing furnace
For 10KV/m, control annealing furnace heating rate is 300 DEG C/min.Then Vickers hardness and oxidative resistance and wear-resisting are carried out to it
Property test, the results showed that reach 38 μm away from surface layer grain size, internal layer crystallite dimension reaches 155 μm, and Vickers hardness is
126.4, its hardness improves about 48.8% compared with as cast condition AS41A, and oxidative resistance improves about 84.3%, and coefficient of friction reaches
0.30, abrasion loss 0.24%.
Comparative example 1
The pure magnesium of as cast condition (99.95wt.%) sample is taken to be put into annealing furnace, carrying out annealing temperature under atmospheric conditions is 580 DEG C
Soaking time is the annealing experiment of 60min.Then Vickers hardness and oxidative resistance and wearability test are carried out to it, as a result table
Bright to reach 285 μm away from surface layer grain size, internal layer crystallite dimension reaches 330 μm, Vickers hardness 35.7, with the pure magnesium phase of as cast condition
About 20.6% is improved than its hardness, oxidative resistance improves about 45.3%, and coefficient of friction reaches 0.5, abrasion loss 0.42%.
Comparative example 2
The pure magnesium of as cast condition (99.95wt.%) sample is taken to be put into annealing furnace, progress annealing temperature is 490 DEG C of soaking times
The annealing experiment of 90min.Wherein helium: the volume ratio of oxygen is 1:2, and pressure is 0.2MPa in annealing furnace, and ultrasonic frequency is
35KHz, no electric field apply, and control annealing furnace heating rate is 100 DEG C/min.Then Vickers hardness and oxidative resistance are carried out to it
And wearability test, the results showed that reach 85 μm away from surface layer grain size, internal layer crystallite dimension reaches 184 μm, and Vickers is hard
Degree is 44.8, its hardness improves about 38.5% compared with the pure magnesium of as cast condition, and oxidative resistance improves about 54.7%, and coefficient of friction reaches
To 0.48, abrasion loss 0.34%.
The embodiment is a preferred embodiment of the present invention, but present invention is not limited to the embodiments described above, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (5)
1. a kind of mandatory method for oxidation for preparing the pure magnesium of gradient structure and magnesium alloy, it is characterised in that: the method step is such as
Under:
It is passed through the mixed gas of helium and oxygen in the lehr first, while controlling the furnace pressure in annealing furnace, then annealing furnace
It is rapidly heated to annealing temperature, the pure magnesium of as cast condition and magnesium alloy is made annealing treatment under compound outfield, annealing applies when keeping the temperature
Ultrasonic wave, when furnace cooling, apply electric field, obtain the pure magnesium and magnesium alloy of gradient structure；
Furnace pressure in the annealing furnace is 0.1~1MPa；
The frequency for applying ultrasonic wave when annealing heat preservation is 30KHz~50KHz；
The current density for applying electric field when the furnace cooling is 5~10KV/m.
2. the mandatory method for oxidation according to claim 1 for preparing the pure magnesium of gradient structure and magnesium alloy, it is characterised in that:
The volume ratio of helium and oxygen that is passed through in mixed gas in the lehr is 1:1~1:10.
3. the mandatory method for oxidation according to claim 1 for preparing the pure magnesium of gradient structure and magnesium alloy, it is characterised in that:
The annealing furnace heating rate is 100~300 DEG C/min.
4. the mandatory method for oxidation according to claim 1 for preparing the pure magnesium of gradient structure and magnesium alloy, it is characterised in that:
The annealing temperature is 450 DEG C~570 DEG C, and soaking time is 30min~120min.
5. the mandatory method for oxidation according to claim 1 for preparing the pure magnesium of gradient structure and magnesium alloy, it is characterised in that:
Crystallite dimension reaches 20~100 μm when the gradient structure is away from 0~0.5cm of surface layer, brilliant when apart from 0.5~1.5cm of surface layer
Particle size reaches 100~300 μm, and crystallite dimension is greater than 300 μm when being greater than 1.5 apart from surface layer.
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| AU2021230640B2 (en) | 2020-03-03 | 2023-12-14 | Hejie Li | Methods for improving mechanical property and biological stability of magnesium alloy and for manufacturing material and applications |
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| RU2471268C1 (en) * | 2011-12-07 | 2012-12-27 | Федеральное государственное бюджетное учреждение науки Институт физики твердого тела Российской академии наук (ИФТТ РАН) | Method of producing high-temperature superconductor in magnesium-magnesium oxide system |
| CN104087801A (en) * | 2014-07-10 | 2014-10-08 | 重庆大学 | Corrosion-resistant magnesium alloy and method for improving corrosion resistance of corrosion-resistant magnesium alloy |
| CN106636823A (en) * | 2016-12-27 | 2017-05-10 | 常州大学 | Novel magnesium alloy composite material preparation method |
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| JP2002332534A (en) * | 2001-05-10 | 2002-11-22 | Mitsubishi Electric Corp | Magnesium alloy molded body and surface treatment method therefor |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415444A (en) * | 2002-10-18 | 2003-05-07 | 上海大学 | Technical method for thinning the solidification structure of aluminun alloy |
| RU2471268C1 (en) * | 2011-12-07 | 2012-12-27 | Федеральное государственное бюджетное учреждение науки Институт физики твердого тела Российской академии наук (ИФТТ РАН) | Method of producing high-temperature superconductor in magnesium-magnesium oxide system |
| CN104087801A (en) * | 2014-07-10 | 2014-10-08 | 重庆大学 | Corrosion-resistant magnesium alloy and method for improving corrosion resistance of corrosion-resistant magnesium alloy |
| CN106636823A (en) * | 2016-12-27 | 2017-05-10 | 常州大学 | Novel magnesium alloy composite material preparation method |
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