CN103469132A - Treating method for improving g strength and toughness of magnesium alloy materials - Google Patents
Treating method for improving g strength and toughness of magnesium alloy materials Download PDFInfo
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Abstract
The invention discloses a treating method for improving strength and toughness of magnesium alloy materials. The treating method for improving the strength and the toughness of the magnesium alloy materials comprises solution treatment and aging treatment, and further comprises subzero treatment after the aging treatment and ultrasonic filed shock treatment in the process of the subzero treatment. The process of the subzero treatment comprises the steps of cooling the magnesium alloy materials to ultralow temperature at minus 196DEG C from the starting room temperature at the cooling speed 1-10DEG C/min, and holding the temperature for 12-30 hours. Preferably, the ultrasonic filed shock treatment is carried out at the late period of the subzero treatment, the intensity of an ultrasonic field is 1-50Kw/m2, the frequency of the ultrasonic field is 10-40KHz, and the treating time in the ultrasonic field is 60-200 seconds. The magnesium alloy materials after the subzero treatment and the ultrasonic field shock treatment are put into an oven which is 170DEG C at temperature, the holding time is 2-6 hours, and then the magnesium alloy materials in the oven are put in air to recover to the room temperature naturally. The treating method for improving the strength and the toughness of the magnesium alloy materials enables the magnesium alloy materials to be compact in structure and high in hardness and roughness.
Description
Technical field
The present invention relates to a kind of enhanced processing method of magnesium alloy materials, particularly relate to a kind for the treatment of process that improves magnesium alloy materials intensity and toughness.
Background technology
Magnesium alloy materials, as one of the lightest metal alloy compositions, has higher specific tenacity and specific rigidity simultaneously, and heat-conductivity conducting is good, damping vibration attenuation, electromagnetic shielding, be easy to shape, so the high tough magnesium alloy materials of preparation is material application and the trend developed.
From prior art, usually adopt and in fusion process, add fining agent to carry out refined crystalline strengthening to crystal grain or generate the method such as enhanced granule by reaction in－situ, reach the mechanical property of improving magnesium alloy materials.The existing Chinese patent that improves the magnesium alloy materials obdurability mainly contains two: the one, and the patent No. is 201110400274.6, name is called the patent of invention of a kind of method of ultrasonic field and fining agent composite refining AZ31 magnesium alloy crystal grain, it passes through the AZ31 magnesium alloy in fusion process, adopt ultrasonic wave that the SiC ceramic particle is incorporated in magnesium alloy, utilize the crystal grain thinning technology, improve casting flaw, put forward heavy alloyed intensity and toughness; The 2nd, the patent No. is 201210580241.9, and name is called a kind of in-situ authigenic Al
3bC strengthens the patent of invention of magnesium base composite material and preparation method thereof, and the method is passed through Al-A
3the BC prealloy dissolves, and standing insulation after stirring or ultrasonication is shaped aluminium alloy die casting or extrusion casting, can obtain particle reinforced magnesium base compound material.Above two kinds of methods that strengthen magnesium alloy materials intensity and toughness, all by utilizing refined crystalline strengthening or reaction in－situ to generate the toughness and tenacity that enhanced granule is carried out the reinforced magnesium alloy material in fusion process, but, adopt aforesaid method to improve the ability of magnesium alloy obdurability very limited, the magnesium alloy materials that is difficult to prepare high-strong toughness meets industrial needs, therefore, in the urgent need to seeking a kind of novel method, significantly improve the obdurability of magnesium alloy materials, to meet growing industrial needs.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind for the treatment of process that improves magnesium alloy materials intensity and toughness, and compared with prior art, toughness and tenacity is largely increased the magnesium alloy materials of processing by the method, thereby can meet better industrial needs.
For solving the problems of the technologies described above, the present invention adopts a kind of like this treatment process that improves magnesium alloy materials intensity and toughness, the method comprises solution treatment and the ageing treatment that magnesium alloy materials is carried out successively, after the method also is included in ageing treatment, the sub-zero treatment that magnesium alloy materials is carried out and the ultrasonic field shock treatment of in the sub-zero treatment process, magnesium alloy materials being carried out.
In the present invention, the process of described sub-zero treatment comprises, from room temperature, and speed of cooling 1～10
oc/min, be cooled to magnesium alloy materials-196
obe incubated 12～30h under the very low temperature of C.
In the present invention, the described ultrasonic field shock treatment that magnesium alloy materials is carried out is preferably carried out in the later stage of sub-zero treatment, and the intensity of described ultrasonic field is 1～50Kw/m
2, the sound field frequency is 10～40KHZ, the treatment time of ultrasonic field is 60～200S.
In the present invention, the later stage of described sub-zero treatment is that sub-zero treatment is from setting concluding time t≤0.5h.
In the present invention, the magnesium alloy materials after sub-zero treatment and ultrasonic field shock treatment can be placed in to temperature is 170
oin the baking oven of C, soaking time is 2～6h, subsequently the magnesium alloy materials in baking oven is placed in to air, naturally returns to room temperature.
The quench treatment of carrying out after method of the present invention also is included in solution treatment, before ageing treatment, the process of described quench treatment comprises puts into 35～45 by the magnesium alloy materials after solution treatment
oquenched in the water of C, then be cooled to room temperature.
In the present invention, the process of described solution treatment comprises magnesium alloy materials 400～470
obe incubated 3～7h at the temperature of C.
In the present invention, the process of described ageing treatment comprises magnesium alloy materials 100～150
obe incubated 12～30h at the temperature of C.
In the present invention, described magnesium alloy materials is preferably the granule reinforced magnesium alloy material.
After adopting above-mentioned treatment process, the present invention has following beneficial effect:
From tissue signature, when magnesium alloy materials carries out sub-zero treatment, because of the very low temperature effect, thereby magnesium alloy materials can shrink and produce the microplasticity distortion, viscous deformation causes a large amount of dislocations of the inner generation of magnesium alloy materials, when sub-zero treatment, produce like this on the basis of dislocation, by applying the ultrasonic field shock effect of some strength, utilize cavitation effect and the acoustic streaming shock effect of ultrasonic field, can impel magnesium alloy materials middle-high density dislocation to carry out rapid movement, the rapid movement of dislocation can bring out in magnesium alloy materials inside the generation nano twin crystal, the generation of nano twin crystal makes magnesium alloy materials have the tissue signature of nanoscale coherence crystal face, thereby make magnesium alloy materials possess the mechanical property of high strength and high tenacity simultaneously.
As a kind of preferred implementation of the present invention, the intensity of described ultrasonic field is 1～50Kw/m
2the sound field frequency is 10～40KHZ, the treatment time of ultrasonic field is 60～200S, and the later stage in sub-zero treatment is carried out the ultrasonic field shock treatment to magnesium alloy materials, the described sub-zero treatment later stage is preferably sub-zero treatment in the time range of setting concluding time t≤0.5h, i.e. in half an hour before sub-zero treatment finishes.After adopting this technical scheme, the high speed moment impact energy produced due to ultrasonic field sharply raises the temperature on magnesium alloy materials surface and is sharply cooling, this high-frequency energy is from transfer material inside, magnesium alloy materials surface, thereby cause viscous deformation and the recoverable strain that material structure is inhomogeneous, and impel the rapid movement of magnesium alloy materials middle-high density dislocation, make in magnesium alloy materials to produce a large amount of nano twin crystals, thereby make the obdurability of magnesium alloy materials obtain increasing substantially.And, when the later stage in sub-zero treatment is carried out the ultrasonic field shock treatment to magnesium alloy materials, due to the later stage in sub-zero treatment, the inner dislocation produced of magnesium alloy materials is more, therefore bring out and produce more nano twin crystal at the magnesium alloy materials within, thereby make magnesium alloy materials possess higher obdurability.
As a further improvement on the present invention, the magnesium alloy materials after sub-zero treatment and ultrasonic field shock treatment is placed in to temperature is 170 in the present invention
oin the baking oven of C, soaking time is 2～6h, subsequently the magnesium alloy materials in baking oven is placed in to air, naturally returns to room temperature.After adopting this technical scheme, utilize high low temperature treatment process, can make the mechanical property of magnesium alloy materials better.
Magnesium alloy materials of the present invention is preferably the granule reinforced magnesium alloy material, due to the granule reinforced magnesium alloy when prepared by melting, effect with dispersion-strengthened, dislocations strengthening, thereby there is high strength characteristics, like this on its original strengthening basis, after sub-zero treatment of the present invention and the ultrasonic field shock treatment in the sub-zero treatment process, further brought into play the effect that dislocations strengthening, nano twin crystal are strengthened, the obdurability of this magnesium alloy materials is greatly improved.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
A kind for the treatment of process that improves magnesium alloy materials intensity and toughness, the method comprises solution treatment and the ageing treatment that magnesium alloy materials is carried out successively, after the method also is included in ageing treatment, the sub-zero treatment that magnesium alloy materials is carried out and the ultrasonic field shock treatment of in the sub-zero treatment process, magnesium alloy materials being carried out.
Sub-zero treatment process of the present invention comprises, from room temperature, and speed of cooling 1～10
oc/min, be cooled to magnesium alloy materials-196
obe incubated 12～30h under the very low temperature of C.
The ultrasonic field shock treatment that the present invention carries out magnesium alloy materials is preferably carried out in the later stage of sub-zero treatment, and the intensity of described ultrasonic field is 1～50Kw/m
2, the sound field frequency is 10～40KHZ, the treatment time of ultrasonic field is 60～200S.
In the present invention, the later stage of described sub-zero treatment refers to that sub-zero treatment is from setting concluding time t≤0.5h, i.e. in half an hour before sub-zero treatment finishes.
It is 170 that the present invention preferably is placed in temperature by the magnesium alloy materials after sub-zero treatment and ultrasonic field shock treatment
oin the baking oven of C, soaking time is 2～6h, subsequently the magnesium alloy materials in baking oven is placed in to air, naturally returns to room temperature.
The quench treatment of carrying out after method of the present invention also is included in solution treatment, before ageing treatment, the process of described quench treatment comprises puts into 35～45 by the magnesium alloy materials after solution treatment
oquenched in the water of C, then be cooled to room temperature.
In the present invention, the process of described solution treatment comprises magnesium alloy materials 400～470
obe incubated 3～7h at the temperature of C.
In the present invention, the process of described ageing treatment comprises magnesium alloy materials 100～150
obe incubated 12～30h at the temperature of C.
In the present invention, described magnesium alloy materials is preferably the granule reinforced magnesium alloy material.Described granule reinforced magnesium alloy can outer addition or reaction in－situ synthesis method by routine be thought of a way, when prepared by melting, wild phase is preferably to enhanced granule and is incorporated in magnesium alloy materials and is prepared from.The advantage of this granule reinforced magnesium alloy material is, it has retained the effect of its dispersion-strengthened, dislocations strengthening, thereby made the magnesium magnesium alloy materials have high strength characteristics in the preparation.Like this on its original strengthening basis, by the present invention after above-mentioned sub-zero treatment and the ultrasonic field shock treatment in the sub-zero treatment process, further brought into play the effect that dislocations strengthening, nano twin crystal are strengthened, thereby made the obdurability of this magnesium alloy materials obtain increasing substantially.
In the present invention, the device of implementing sub-zero treatment can adopt commercially available deep cooling cabinet or the case that has heat-insulation and heat-preservation, do not shield ultrasonic field, and the low-temperature receiver of employing is liquid nitrogen.The device of implementing the ultrasonic field shock treatment can adopt commercially available ultrasonic generator, described ultrasonic generator can produce the electric oscillation signal that frequency is greater than 10kHz, be converted to the compressional wave mechanical vibrational energy of same frequency by transverter, by horn, the small amplitude of transverter (being generally 4 μ m) is transformed to 20～80 μ m again, then by various forms of tool heads, vibrational energy is delivered on magnesium alloy materials.
In the present invention, the ultrasonic field shock treatment in described sub-zero treatment and sub-zero treatment later stage, and the insulation of the baking oven after sub-zero treatment processing, but recirculation operates 2～3 times.
Embodiment 1:
Adopt the ZK61 magnesium alloy rod to carry out intensive treatment as sample, the weight percentage of this each composition of magnesium alloy is Al≤0.05%, Zn:5.0～6.0%, Mn≤0.1%, Zr:0.3～0.9%, Si≤0.05%, Fe≤0.05%, Cu≤0.05%, Ni≤0.005%, other: 0.31%, surplus is Mg.
Solution treatment; Described magnesium alloy rod is placed in heat treatment furnace, 400
obe incubated 3h at the temperature of C.
Quench treatment; Magnesium alloy rod after solution treatment is put into to 35
oquenched in the water of C, then be cooled to room temperature.
Ageing treatment; Magnesium alloy rod after quench treatment is placed in heat treatment furnace, 100
obe incubated 12h at the temperature of C, then magnesium alloy rod naturally cooled to room temperature.
Sub-zero treatment and ultrasonic field shock treatment; Magnesium alloy rod after ageing treatment is placed in deep cooling box, from room temperature, speed of cooling 1
oc/min, be cooled to magnesium alloy rod-196
obe incubated 12h under the very low temperature of C, when magnesium alloy rod has been incubated to 11.5～12h, magnesium alloy rod applied to ultrasonic field shock treatment, ultrasound field intensity 1Kw/m
2, sound field frequency 10KHZ, supersound process time 60S.
It is 170 that magnesium alloy rod after sub-zero treatment and ultrasonic field shock treatment is placed in to temperature
oin the baking oven of C, soaking time is 2h, subsequently the magnesium alloy rod in baking oven is placed in to air, naturally returns to room temperature.
Magnesium alloy rod is after treatment carried out to performance and inspect, the tensile strength (δ of magnesium alloy rod
b) be 338Mpa, yield strength (δ
0.2) be 221Mpa, elongation (φ) is 23%.From examining report, can draw: the obdurability of magnesium alloy materials has obtained synchronously significantly improving.
Embodiment 2:
Adopt the AZ61 magnesium alloy rod to carry out intensive treatment as sample, the weight percentage of this each composition of magnesium alloy is Al:5.5～6.5%, Zn:0.5～1.5%, Mn:0.15～0.4%, Si≤0.10%, Fe≤0.005%, Cu≤0.05%, Ni≤0.005%, other≤0.35%, surplus: Mg.
Solution treatment; Described magnesium alloy rod is placed in heat treatment furnace, 470
obe incubated 7h at the temperature of C.
Quench treatment; Magnesium alloy rod after solution treatment is put into to 40
oquenched in the water of C, then be cooled to room temperature.
Ageing treatment; Magnesium alloy rod after quench treatment is placed in heat treatment furnace, 150
obe incubated 30h at the temperature of C, then magnesium alloy rod naturally cooled to room temperature.
Sub-zero treatment and ultrasonic field shock treatment; Magnesium alloy rod after ageing treatment is placed in deep cooling box, from room temperature, speed of cooling 10
oc/min, be cooled to magnesium alloy rod-196
obe incubated 30h under the very low temperature of C, when magnesium alloy rod has been incubated to 29.5～30h, magnesium alloy rod applied to ultrasonic field shock treatment, ultrasound field intensity 50Kw/m
2, sound field frequency 40KHZ, supersound process time 200S.
It is 170 that magnesium alloy rod after sub-zero treatment and ultrasonic field shock treatment is placed in to temperature
oin the baking oven of C, soaking time is 6h, subsequently the magnesium alloy rod in baking oven is placed in to air, naturally returns to room temperature.
Magnesium alloy rod is after treatment carried out to performance and inspect, the tensile strength (δ of magnesium alloy rod
b) be 298Mpa, yield strength (δ
0.2) be 206Mpa, elongation (φ) is 20.5%.From examining report, can draw: the obdurability of magnesium alloy materials has obtained synchronously significantly improving.
Embodiment 3:
At first prepare the SiC particle and strengthen the AZ31 magnesium alloy rod, then the SiC particle of usining strengthens the AZ31 magnesium alloy rod and carries out intensive treatment as sample, the weight percentage of described each composition of AZ31 magnesium alloy is Al:3.0～4.0%, Mn:0.15～0.5%, Zn:0.2～0.8%, Cu:0.05%, Ni:0.005%, Si:0.15%, other: 0.37%, surplus is Mg.
Pack the AZ31 magnesium alloy ingot into 720
oin the C crucible, input N around here
2as shielding gas, protected, after all melting, degassed, skim; The SiC powder is ground to form after nano particle (granularity is less than 100nm) presses 30% weighing of particulates reinforcements theoretical weight, fully dry, then the SiC nano particle of oven dry is put into to crucible, parallel induction stirring and hand mixing, churning time is 5min.Standing 2 ~ the 3min of melt after stirring, treat that temperature is raised to 720 again
oduring C, be cast into diameter 100mm ingot casting; Described 100mm ingot casting is carried out to hot extrusion, extrusion temperature 220
oc, extrusion ratio 30:1, the SiC particle that obtains diameter 28mm strengthens the AZ31 magnesium alloy rod.
Solution treatment; Described SiC particle is strengthened to the AZ31 magnesium alloy rod and be placed in heat treatment furnace, 420
obe incubated 5h at the temperature of C.
Quench treatment; Magnesium alloy rod after solution treatment is put into to 45
oquenched in the water of C, then be cooled to room temperature.
Ageing treatment; Magnesium alloy rod after quench treatment is placed in heat treatment furnace, 130
obe incubated 20h at the temperature of C, then magnesium alloy rod naturally cooled to room temperature.
Sub-zero treatment and ultrasonic field shock treatment; Magnesium alloy rod after ageing treatment is placed in deep cooling box, from room temperature, speed of cooling 6
oc/min, be cooled to magnesium alloy rod-196
obe incubated 20h under the very low temperature of C, when magnesium alloy rod has been incubated to 19.5～20h, magnesium alloy rod applied to ultrasonic field shock treatment, ultrasound field intensity 30Kw/m
2, sound field frequency 30KHZ, supersound process time 120S.
It is 170 that magnesium alloy rod after sub-zero treatment and ultrasonic field shock treatment is placed in to temperature
oin the baking oven of C, soaking time is 4h, subsequently the magnesium alloy rod in baking oven is placed in to air, naturally returns to room temperature.
Magnesium alloy rod is after treatment carried out to performance and inspect, the tensile strength (δ of magnesium alloy rod
b) be 320Mpa, yield strength (δ
0.2) be 200Mpa, elongation (φ) is 17%.From examining report, can draw: the obdurability of magnesium alloy materials has obtained synchronously significantly improving.
To sum up, after adopting method of the present invention, can make magnesium alloy materials dense structure, have high competency and high-strong toughness, the present invention has carried out a kind of new breakthrough by prior heat treatment.
Claims (9)
1. a treatment process that improves magnesium alloy materials intensity and toughness, the method comprises solution treatment and the ageing treatment that magnesium alloy materials is carried out successively, it is characterized in that: after the method also is included in ageing treatment, the sub-zero treatment that magnesium alloy materials is carried out and the ultrasonic field shock treatment of in the sub-zero treatment process, magnesium alloy materials being carried out.
2. the treatment process of raising magnesium alloy materials intensity according to claim 1 and toughness is characterized in that: the process of described sub-zero treatment comprises, from room temperature, and speed of cooling 1～10
oc/min, be cooled to magnesium alloy materials-196
obe incubated 12～30h under the very low temperature of C.
3. the treatment process of raising magnesium alloy materials intensity according to claim 1 and 2 and toughness, it is characterized in that: the described ultrasonic field shock treatment that magnesium alloy materials is carried out was carried out in the later stage of sub-zero treatment, and the intensity of described ultrasonic field is 1～50Kw/m
2, the sound field frequency is 10～40KHZ, the treatment time of ultrasonic field is 60～200S.
4. the treatment process of raising magnesium alloy materials intensity according to claim 3 and toughness is characterized in that: the later stage of described sub-zero treatment is that sub-zero treatment is from setting concluding time t≤0.5h.
5. the treatment process of raising magnesium alloy materials intensity according to claim 3 and toughness, it is characterized in that: it is 170 that the magnesium alloy materials after sub-zero treatment and ultrasonic field shock treatment is placed in to temperature
oin the baking oven of C, soaking time is 2～6h, subsequently the magnesium alloy materials in baking oven is placed in to air, naturally returns to room temperature.
6. the treatment process of raising magnesium alloy materials intensity according to claim 1 and toughness, it is characterized in that: the quench treatment of carrying out after the method also is included in solution treatment, before ageing treatment, the process of described quench treatment comprises puts into 35～45 by the magnesium alloy materials after solution treatment
oquenched in the water of C, then be cooled to room temperature.
7. the treatment process of raising magnesium alloy materials intensity according to claim 1 and toughness, it is characterized in that: the process of described solution treatment comprises magnesium alloy materials 400～470
obe incubated 3～7h at the temperature of C.
8. the treatment process of raising magnesium alloy materials intensity according to claim 1 and toughness, it is characterized in that: the process of described ageing treatment comprises magnesium alloy materials 100～150
obe incubated 12～30h at the temperature of C.
9. the treatment process of raising magnesium alloy materials intensity according to claim 1 and toughness, it is characterized in that: described magnesium alloy materials is the granule reinforced magnesium alloy material.
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| CN105331911A (en) * | 2015-11-30 | 2016-02-17 | 江苏大学 | Copious cooling and magnetic field treating method for improving plastic processing performance of magnesium alloy |
| CN106148783A (en) * | 2015-04-01 | 2016-11-23 | 徐万强 | Anticorrosive high-strength deformation nanometer Mg alloy and its preparation method and application |
| CN107574392A (en) * | 2017-08-31 | 2018-01-12 | 中国科学院海洋研究所 | A kind of processing method of raising Mg Y Nd based alloy decay resistances |
| CN108330422A (en) * | 2017-01-17 | 2018-07-27 | 沈阳工业大学 | A kind of cryogenic treatment process improving magnesium alloy toughness |
| CN109468559A (en) * | 2017-09-08 | 2019-03-15 | 山东省科学院新材料研究所 | A kind of preparation method of high-performance magnesium-alloy extrudate |
| CN109837437A (en) * | 2019-02-27 | 2019-06-04 | 吉林大学 | A kind of alternating temperature controlled rolling preparation method for making low content magnesium alloy that there is uniform fine grain |
| CN110408755A (en) * | 2019-08-29 | 2019-11-05 | 中南大学 | A kind of aging process improving TiC-Cr-Mo base steel composite material dimensional stability |
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| CN106148783A (en) * | 2015-04-01 | 2016-11-23 | 徐万强 | Anticorrosive high-strength deformation nanometer Mg alloy and its preparation method and application |
| CN106148783B (en) * | 2015-04-01 | 2019-10-15 | 徐万强 | Anticorrosive high-strength deformation nanometer magnesium alloy and its preparation method and application |
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| CN107574392A (en) * | 2017-08-31 | 2018-01-12 | 中国科学院海洋研究所 | A kind of processing method of raising Mg Y Nd based alloy decay resistances |
| CN109468559A (en) * | 2017-09-08 | 2019-03-15 | 山东省科学院新材料研究所 | A kind of preparation method of high-performance magnesium-alloy extrudate |
| CN109468559B (en) * | 2017-09-08 | 2019-11-26 | 山东省科学院新材料研究所 | A kind of preparation method of high-performance magnesium-alloy extrudate |
| CN109837437A (en) * | 2019-02-27 | 2019-06-04 | 吉林大学 | A kind of alternating temperature controlled rolling preparation method for making low content magnesium alloy that there is uniform fine grain |
| CN110408755A (en) * | 2019-08-29 | 2019-11-05 | 中南大学 | A kind of aging process improving TiC-Cr-Mo base steel composite material dimensional stability |
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