CN103469132B - A kind for the treatment of process improving magnesium alloy materials intensity and toughness - Google Patents
A kind for the treatment of process improving magnesium alloy materials intensity and toughness Download PDFInfo
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Abstract
The invention discloses a kind for the treatment of process improving magnesium alloy materials intensity and toughness, comprise solution treatment and ageing treatment, the method is also included in the sub-zero treatment after ageing treatment and the ultrasonic field shock treatment in sub-zero treatment process.Sub-zero treatment process comprises from room temperature, speed of cooling 1 ~ 10
oc/min, is cooled to-196 by magnesium alloy materials
o12 ~ 30h is incubated under the very low temperature of C.Ultrasonic field shock treatment is preferably carried out in the later stage of sub-zero treatment, and the intensity of ultrasonic field is 1 ~ 50Kw/m
2, sound field frequency is 10 ~ 40KHZ, and the treatment time of ultrasonic field is 60 ~ 200S.It is 170 that magnesium alloy after sub-zero treatment and ultrasonic field shock treatment is placed in temperature
oin the baking oven of C, soaking time is 2 ~ 6h, and subsequently the magnesium alloy in baking oven is placed in air, clear-cutting forestland is to room temperature.The present invention can make magnesium alloy materials dense structure, has high competency and high-strong toughness simultaneously.
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 improving 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, is easy to shape, so the high tough magnesium alloy materials of preparation, be the trend of materials application and development.
From prior art, be typically employed in fusion process and add fining agent and refined crystalline strengthening is carried out to crystal grain or generates the method such as enhanced granule by reaction in－situ, reach the mechanical property improving magnesium alloy materials.It is the patent No. is 201110400274.6 that the existing Chinese patent improving magnesium alloy materials obdurability mainly contains two: one, 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 AZ31 magnesium alloy in fusion process, ultrasonic wave is adopted to be incorporated in magnesium alloy by SiC ceramic particulate, utilize crystal grain thinning technology, improve casting flaw, put forward heavy alloyed intensity and toughness; Two are patent No.s 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
3bC prealloy dissolves, and leaves standstill insulation, stirs or aluminium alloy die casting or extrusion casting is shaped after ultrasonication, can obtain particle reinforced magnesium base compound material.The method of above two kinds of enhancing 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 carrys out reinforced magnesium alloy material in fusion process, but, the ability that employing aforesaid method improves magnesium alloy obdurability is very limited, be difficult to prepare the magnesium alloy materials of high-strong toughness to meet 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 improving magnesium alloy materials intensity and toughness, and by the magnesium alloy materials of the method process compared with prior art, toughness and tenacity is largely increased, thus can meet industrial needs better.
For solving the problems of the technologies described above, the present invention adopts a kind of like this treatment process improving magnesium alloy materials intensity and toughness, the method comprises the solution treatment and ageing treatment carried out successively magnesium alloy materials, after the method is also included in ageing treatment, the sub-zero treatment that magnesium alloy materials is carried out and in sub-zero treatment process to the ultrasonic field shock treatment that magnesium alloy materials carries out.
In the present invention, the process of described sub-zero treatment comprises, from room temperature, and speed of cooling 1 ~ 10
oc/min, is cooled to-196 by magnesium alloy materials
o12 ~ 30h is incubated under the very low temperature of C.
In the present invention, described ultrasonic field shock treatment of carrying 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, sound field frequency is 10 ~ 40KHZ, and 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 end 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 temperature is 170
oin the baking oven of C, soaking time is 2 ~ 6h, and subsequently the magnesium alloy materials in baking oven is placed in air, clear-cutting forestland is to room temperature.
The quench treatment of carrying out after method of the present invention is also included in solution treatment, before ageing treatment, the process of described quench treatment comprises the magnesium alloy materials after by solution treatment and puts into 35 ~ 45
oquench in the water of C, be then cooled to room temperature.
In the present invention, the process of described solution treatment comprises magnesium alloy materials 400 ~ 470
o3 ~ 7h is incubated at the temperature of C.
In the present invention, the process of described ageing treatment comprises magnesium alloy materials 100 ~ 150
o12 ~ 30h is incubated at the temperature of C.
In the present invention, described magnesium alloy materials is preferably particle reinforce magnesium alloy materials.
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 very low temperature effect, magnesium alloy materials can shrink thus produce micro-plastic deformation, viscous deformation causes magnesium alloy materials inside to produce a large amount of dislocation, produce when sub-zero treatment 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, magnesium alloy materials middle-high density dislocation can be impelled to carry out rapid movement, the rapid movement of dislocation can bring out generation nano twin crystal in magnesium alloy materials inside, the generation of nano twin crystal makes magnesium alloy materials have the tissue signature of nanoscale coherence crystal face, thus 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
2sound field frequency is 10 ~ 40KHZ, the treatment time of ultrasonic field is 60 ~ 200S, and in the later stage of sub-zero treatment, ultrasonic field shock treatment is carried out to magnesium alloy materials, the described sub-zero treatment later stage is preferably sub-zero treatment from the time range of setting end time t≤0.5h, in the half an hour namely before sub-zero treatment terminates.After adopting this technical scheme, the high speed moment impact energy produced due to ultrasonic field makes the temperature on magnesium alloy materials surface sharply raise and quick refrigeration, this high-frequency energy is inner from magnesium alloy materials surface transfer material, thus the viscous deformation causing material structure uneven and recoverable strain, 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, thus the obdurability of magnesium alloy materials is obtained increase substantially.And, when carrying out ultrasonic field shock treatment in the later stage of sub-zero treatment to magnesium alloy materials, due to the later stage in sub-zero treatment, the dislocation that magnesium alloy materials inside produces is more, therefore bring out at magnesium alloy materials within and produce more nano twin crystal, thus 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 temperature by the present invention is 170
oin the baking oven of C, soaking time is 2 ~ 6h, and subsequently the magnesium alloy materials in baking oven is placed in air, clear-cutting forestland is to room temperature.After adopting this technical scheme, utilize high/low temperature treatment process, the mechanical property of magnesium alloy materials can be made better.
Magnesium alloy materials of the present invention is preferably particle reinforce magnesium alloy materials, because particle reinforce magnesium alloy is when prepared by melting, there is the effect of dispersion-strengthened, dislocations strengthening, thus 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 sub-zero treatment process, further play the effect of dislocations strengthening, nano twin crystal strengthening, 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 improving magnesium alloy materials intensity and toughness, the method comprises the solution treatment and ageing treatment carried out successively magnesium alloy materials, after the method is also included in ageing treatment, the sub-zero treatment that magnesium alloy materials is carried out and in sub-zero treatment process to the ultrasonic field shock treatment that magnesium alloy materials carries out.
Sub-zero treatment process of the present invention comprises, from room temperature, and speed of cooling 1 ~ 10
oc/min, is cooled to-196 by magnesium alloy materials
o12 ~ 30h is incubated under the very low temperature of C.
The present invention preferably carries out in the later stage of sub-zero treatment the ultrasonic field shock treatment that magnesium alloy materials carries out, and the intensity of described ultrasonic field is 1 ~ 50Kw/m
2, sound field frequency is 10 ~ 40KHZ, and 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 end time t≤0.5h, in the half an hour namely before sub-zero treatment terminates.
It is 170 that magnesium alloy materials after sub-zero treatment and ultrasonic field shock treatment is preferably placed in temperature by the present invention
oin the baking oven of C, soaking time is 2 ~ 6h, and subsequently the magnesium alloy materials in baking oven is placed in air, clear-cutting forestland is to room temperature.
The quench treatment of carrying out after method of the present invention is also included in solution treatment, before ageing treatment, the process of described quench treatment comprises the magnesium alloy materials after by solution treatment and puts into 35 ~ 45
oquench in the water of C, be then cooled to room temperature.
In the present invention, the process of described solution treatment comprises magnesium alloy materials 400 ~ 470
o3 ~ 7h is incubated at the temperature of C.
In the present invention, the process of described ageing treatment comprises magnesium alloy materials 100 ~ 150
o12 ~ 30h is incubated at the temperature of C.
In the present invention, described magnesium alloy materials is preferably particle reinforce magnesium alloy materials.Described particle reinforce magnesium alloy by the outer addition of routine or XD method namely in think of a way, when prepared by melting, wild phase is preferably enhanced granule and is incorporated in magnesium alloy materials and is prepared from.The advantage of this particle reinforce magnesium alloy materials is, it remains the effect of its dispersion-strengthened, dislocations strengthening in the preparation, thus makes magnesium magnesium alloy materials have high strength characteristics.Like this on its original strengthening basis, after the sub-zero treatment above-mentioned by the present invention and the ultrasonic field shock treatment in sub-zero treatment process, further play the effect of dislocations strengthening, nano twin crystal strengthening, thus the obdurability of this magnesium alloy materials has been obtained increase substantially.
In the present invention, the device implementing sub-zero treatment can adopt the commercially available deep cooling cabinet having heat-insulation and heat-preservation, do not shield ultrasonic field or case, and the low-temperature receiver of employing is liquid nitrogen.The device implementing 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, the compressional wave mechanical vibrational energy of same frequency is converted to by transverter, by horn, small for transverter amplitude (being generally 4 μm) is transformed to 20 ~ 80 μm 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 baking oven isothermal holding after sub-zero treatment, can recirculation operate 2 ~ 3 times.
Embodiment 1:
Adopt ZK61 magnesium alloy rod to carry out intensive treatment as sample, the weight percentage of each composition of this 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
o3h is incubated at the temperature of C.
Quench treatment; Magnesium alloy rod after solution treatment is put into 35
oquench in the water of C, be then 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, is cooled to-196 by magnesium alloy rod
obe incubated 12h under the very low temperature of C, when being incubated 11.5 ~ 12h to magnesium alloy rod, ultrasonic field shock treatment applied to magnesium alloy rod, ultrasound field intensity 1Kw/m
2, sound field frequency 10KHZ, sonication treatment time 60S.
It is 170 that magnesium alloy rod after sub-zero treatment and ultrasonic field shock treatment is placed in temperature
oin the baking oven of C, soaking time is 2h, and subsequently the magnesium alloy rod in baking oven is placed in air, clear-cutting forestland is to room temperature.
Carry out performance to magnesium alloy rod after treatment to inspect, the tensile strength (δ of magnesium alloy rod
b) be 338Mpa, yield strength (δ
0.2) be 221Mpa, elongation (φ) is 23%.Can draw from examining report: the obdurability of magnesium alloy materials obtains and synchronously significantly improves.
Embodiment 2:
Adopt AZ61 magnesium alloy rod to carry out intensive treatment as sample, the weight percentage of each composition of this 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
o7h is incubated at the temperature of C.
Quench treatment; Magnesium alloy rod after solution treatment is put into 40
oquench in the water of C, be then 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, is cooled to-196 by magnesium alloy rod
obe incubated 30h under the very low temperature of C, when being incubated 29.5 ~ 30h to magnesium alloy rod, ultrasonic field shock treatment applied to magnesium alloy rod, ultrasound field intensity 50Kw/m
2, sound field frequency 40KHZ, sonication treatment time 200S.
It is 170 that magnesium alloy rod after sub-zero treatment and ultrasonic field shock treatment is placed in temperature
oin the baking oven of C, soaking time is 6h, and subsequently the magnesium alloy rod in baking oven is placed in air, clear-cutting forestland is to room temperature.
Carry out performance to magnesium alloy rod after treatment to inspect, the tensile strength (δ of magnesium alloy rod
b) be 298Mpa, yield strength (δ
0.2) be 206Mpa, elongation (φ) is 20.5%.Can draw from examining report: the obdurability of magnesium alloy materials obtains and synchronously significantly improves.
Embodiment 3:
First SiC particle reinforce AZ31 magnesium alloy rod is prepared, then intensive treatment is carried out using SiC particle reinforce AZ31 magnesium alloy rod as sample, the weight percentage of each composition of described 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.
AZ31 magnesium alloy ingot is loaded 720
oin C crucible, input N around here
2protect as shielding gas, after all melting, degassed, skim; SiC powder is ground to form nano particle (granularity is less than 100nm) by after 30% weighing of particulates reinforcements theoretical weight, fully dry, then the SiC nano particle of oven dry is put into crucible, parallel induction stirring and hand mixing, churning time is 5min.Melt after stirring leaves standstill 2 ~ 3min, treats that temperature is raised to 720 again
oduring C, be cast into diameter 100mm ingot casting; Described 100mm ingot casting is carried out hot extrusion, extrusion temperature 220
oc, extrusion ratio 30:1, obtain the SiC particle reinforce AZ31 magnesium alloy rod of diameter 28mm.
Solution treatment; Described SiC particle reinforce AZ31 magnesium alloy rod is placed in heat treatment furnace, 420
o5h is incubated at the temperature of C.
Quench treatment; Magnesium alloy rod after solution treatment is put into 45
oquench in the water of C, be then 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, is cooled to-196 by magnesium alloy rod
obe incubated 20h under the very low temperature of C, when being incubated 19.5 ~ 20h to magnesium alloy rod, ultrasonic field shock treatment applied to magnesium alloy rod, ultrasound field intensity 30Kw/m
2, sound field frequency 30KHZ, sonication treatment time 120S.
It is 170 that magnesium alloy rod after sub-zero treatment and ultrasonic field shock treatment is placed in temperature
oin the baking oven of C, soaking time is 4h, and subsequently the magnesium alloy rod in baking oven is placed in air, clear-cutting forestland is to room temperature.
Carry out performance to magnesium alloy rod after treatment to inspect, the tensile strength (δ of magnesium alloy rod
b) be 320Mpa, yield strength (δ
0.2) be 200Mpa, elongation (φ) is 17%.Can draw from examining report: the obdurability of magnesium alloy materials obtains and synchronously significantly improves.
To sum up, after adopting method of the present invention, can make magnesium alloy materials dense structure, have high competency and high-strong toughness, prior heat treatment has been carried out a kind of new breakthrough by the present invention.
Claims (8)
1. one kind is improved the treatment process of magnesium alloy materials intensity and toughness, the method comprises the solution treatment and ageing treatment carried out successively magnesium alloy materials, it is characterized in that: after the method is also included in ageing treatment, the sub-zero treatment that magnesium alloy materials is carried out and in sub-zero treatment process to the ultrasonic field shock treatment that magnesium alloy materials carries out; Describedly carry out in the later stage of sub-zero treatment the ultrasonic field shock treatment that magnesium alloy materials carries out, the intensity of described ultrasonic field is 1 ~ 50KW/m
2, sound field frequency is 10 ~ 40KHz, and the treatment time of ultrasonic field is 60 ~ 200s.
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, is cooled to-196 by magnesium alloy materials
o12 ~ 30h is incubated under the very low temperature of C.
3. the treatment process of raising magnesium alloy materials intensity according to claim 1 and toughness, is characterized in that: the later stage of described sub-zero treatment is that sub-zero treatment is from setting end time 0 < t≤0.5h.
4. the treatment process of raising magnesium alloy materials intensity according to claim 1 and toughness, is characterized in that: it is 170 that the magnesium alloy materials after sub-zero treatment and ultrasonic field shock treatment is placed in temperature
oin the baking oven of C, soaking time is 2 ~ 6h, and subsequently the magnesium alloy materials in baking oven is placed in air, clear-cutting forestland is to room temperature.
5. 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 is also included in solution treatment, before ageing treatment, the process of described quench treatment comprises the magnesium alloy materials after by solution treatment and puts into 35 ~ 45
oquench in the water of C, be then cooled to room temperature.
6. the treatment process of raising magnesium alloy materials intensity according to claim 1 and toughness, is characterized in that: the process of described solution treatment comprises magnesium alloy materials 400 ~ 470
o3 ~ 7h is incubated at the temperature of C.
7. the treatment process of raising magnesium alloy materials intensity according to claim 1 and toughness, is characterized in that: the process of described ageing treatment comprises magnesium alloy materials 100 ~ 150
o12 ~ 30h is incubated at the temperature of C.
8. the treatment process of raising magnesium alloy materials intensity according to claim 1 and toughness, is characterized in that: described magnesium alloy materials is particle reinforce magnesium alloy materials.
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| CN106148783B (en) * | 2015-04-01 | 2019-10-15 | 徐万强 | Anticorrosive high-strength deformation nanometer magnesium alloy and its preparation method and application |
| CN105331911B (en) * | 2015-11-30 | 2017-07-18 | 江苏大学 | A kind of deep cooling magnetic field processing method for improving magnesium alloy plastic deformation ability |
| CN108330422B (en) * | 2017-01-17 | 2019-10-01 | 沈阳工业大学 | A kind of cryogenic treatment process improving magnesium alloy toughness |
| CN107574392B (en) * | 2017-08-31 | 2019-04-23 | 中国科学院海洋研究所 | A kind of processing method improving Mg-Y-Nd based alloy corrosion resistance |
| 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 |
| CN109837437B (en) * | 2019-02-27 | 2020-09-01 | 吉林大学 | Variable-temperature controlled rolling preparation method for enabling low-content magnesium alloy to have uniform fine grains |
| CN110408755B (en) * | 2019-08-29 | 2021-04-23 | 中南大学 | Aging method for improving size stability of TiC-Cr-Mo steel-based composite material |
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