CN107227415B - Magnesium intermediate alloy grain refiner containing vanadium and its preparation method and application - Google Patents
Magnesium intermediate alloy grain refiner containing vanadium and its preparation method and application Download PDFInfo
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- CN107227415B CN107227415B CN201710497260.8A CN201710497260A CN107227415B CN 107227415 B CN107227415 B CN 107227415B CN 201710497260 A CN201710497260 A CN 201710497260A CN 107227415 B CN107227415 B CN 107227415B
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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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/1015—Pretreatment of the non-metallic additives by preparing or treating a non-metallic additive preform
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
Abstract
Magnesium intermediate alloy grain refiner and its preparation method and application of the present invention containing vanadium, as mass fraction, the fining agent includes 90~99% magnesium, remaining is the compound of vanadium, and the compound is VC, VN, VCxN1‑xAt least one of, the VCxN1‑xIn, 0 < x < 1.The invention also discloses the preparation methods of several magnesium intermediate alloy grain refiners containing vanadium.Magnesium intermediate alloy grain refiner of the present invention containing vanadium, vfanadium compound can be used as magnesium alloy effectively heterogeneous forming core core, it is prepared into magnesium intermediate alloy, additive amount is easier to control, easy to use, recovery rate is high, it is not limited and (can be added in the magnesium alloy containing Al and without Al) by magnesium alloy ingredient, after being added in magnesium alloy, effective Refining Mg Alloy crystal grain, strengthen magnesium and magnesium alloy, improves the comprehensive mechanical property of magnesium alloy.
Description
Technical field
The invention belongs to the production and processing technical field of magnesium alloy materials, in particular to a kind of magnesium intermediate alloy containing vanadium is brilliant
Grain fining agent and its preparation method and application.
Background technique
Magnesium and magnesium alloy are due to its low-density, high specific strength and specific stiffness, good damping capacity, excellent casting character and
The advantages that easily cutting pin processability, is more and more favored, is expected to industrial in communications and transportation, aerospace and electronic product etc.
Field is widely used.But the room temperature intensity and toughness of magnesium and its alloy are lower, creep resistant and corrosion resistance difference etc., again
Limit its development.And crystal grain refinement is to improve the important means of magnesium and its magnesium alloy comprehensive performance.
It is most simple and efficient method that grain refiner is added into magnesium.The crystal grain refinement of magnesium alloy mainly passes through alloy
Change with Metamorphism treatment and realizes.Currently, the more mature grain refiner of application is metal zirconium, but zirconium has more disadvantage, such as:
In the alloy containing Al easy " poisoning " and lose grain refining efficiency, expensive, alloying temperature is higher, easily settled, recovery rate is low
Deng.Following two categories is concentrated mainly on to the research of the grain refiner containing almag:
(1) solute element is added: it is generally acknowledged that the addition of solute element can be in solid-liquid interface in alloy graining process
Forward position generates constitutional supercooling, promotes forming core.But a part for being added to the alloying element in melt will occur anti-with aluminium or magnesium
It answers and generates compound, some even can form coarse compound, cause alloying element to the Grain Refinement Effect of magnesium alloy
It is unstable.
(2) method of heterogeneous forming core: the wherein rotten method research of carbon is thought to introduce simple substance carbon or carbon containing in alloy melt
Compound, generate effective heterogeneous forming core particle Al4C3Or Al2OC achievees the purpose that refine crystal grain.But its grain refining effect
Unstable, Refining Mechanism is disputable, and carbon is introduced into more difficult in melt, and the addition of carbon seriously affects the corrosion resistance of alloy.
Research new at present, adds Al in the magnesium alloy of RE containing rare earth (Y, Gd, Sm, Ce etc.), and fabricated in situ is made with heterogeneous forming core
Al2RE compound.But it generates this compound particle and needs specific alloying component and process conditions.
200980114447.9 disclosing a kind of method of crystal grain refinement magnesium metal or magnesium base alloy.This method be in magnesium or
Vanadium metal is added in person's magnesium base alloy, utilizes the solute element effect refinement crystal grain of vanadium.Although having been disclosed in this patent containing vanadium
Grain refiner, but this method should range addition solute element, and there are still the defects.
Technical field is produced and processed for magnesium alloy materials, it is also necessary to which exploitation is alternative and effective and is applied to institute
Have or the general grain refiner of most of magnesium alloy.
Summary of the invention
In view of the drawbacks of the prior art, the purpose of the present invention is to provide a kind of magnesium intermediate alloy grain refiner containing vanadium
And its preparation method and application, the fining agent utilizes vfanadium compound, plays heterogeneous forming core refinement crystal grain.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, the magnesium intermediate alloy grain refiner containing vanadium, as mass fraction, the fining agent includes 90~99% magnesium,
Remaining is the compound of vanadium, and the compound is VC, VN, VCxN1-xAt least one of, the VCxN1-xIn, 0 < x < 1.
2, the preparation method of the magnesium intermediate alloy grain refiner containing vanadium, includes the following steps:
(1) compound powder for weighing magnesium powder and vanadium according to the ratio is placed in agate pot ball milling mixing under the protection of argon gas
6~12h, using alcohol or acetone as ball-milling medium, ratio of grinding media to material is 6~10:1；
(2) by the mixed-powder vacuum drying after ball milling, after powder is placed in cylindric graphite jig, be 25 in pressure
~40MPa, temperature keep the temperature 30~60min, the cooling magnesium intermediate alloy sintering block obtained containing vanadium under the conditions of being 450~550 DEG C.
Further, the ball milling uses planetary ball mill, using intermittent ball milling mode, i.e. ball milling 3h, pause 15
~20min.
Further, the preparation method further includes step (3): vehicle falls magnesium intermediate alloy sintering block of the gained containing vanadium
Surface scale preheats 1~2h at 350~400 DEG C, then squeezes under the conditions of 350~400 DEG C of temperature, extrusion ratio 89:1
Obtain the magnesium intermediate alloy grain refiner wire rod containing vanadium.
Further, the diameter of the graphite jig is 70mm, the magnesium intermediate alloy grain refiner line after extruding containing vanadium
Material diameter is 9mm.
3, the preparation method of the magnesium intermediate alloy grain refiner containing vanadium, includes the following steps:
(1) weigh magnesium powder and vanadium compound powder be placed in agate pot under the protection of argon gas ball milling mixing 6~
12h, using alcohol or acetone as ball-milling medium, ratio of grinding media to material is 6~10:1, after by the mixed-powder vacuum drying after ball milling, and press
Type is made, forms magnesium vfanadium compound green compact；
(2) magnesium ingot is placed in the stainless steel crucible for having applied BN coating, heat up melting in resistance furnace, in coverture or
CO2With SF6Under mixed gas protected, magnesium ingot is fused into magnesium liquid, at 720~750 DEG C by the magnesium vfanadium compound green compact in step (1)
It is pressed into magnesium liquid, until completely melted, the temperature of Serum Magnesium is adjusted to 720 DEG C, after keeping the temperature 30min, stirs 5~10min,
Surface slag is destroyed, is poured into 150~200 DEG C of preheating of cylindric low-carbon steel mold, the magnesium intermediate alloy casting containing vanadium is obtained
Ingot；
(3) gained ingot casting in step (2) is removed end to end according to cylinder size is squeezed, after turning to suitable dimension
1~2h is preheated at 350~400 DEG C, squeezing temperature is 350~400 DEG C, extrusion ratio 89:1, and squeezing and obtaining diameter is containing for 9mm
The magnesium intermediate alloy grain refiner wire rod of vanadium.
Further, the adding proportion of the compound powder and magnesium ingot of the magnesium powder and vanadium need to be satisfied among the magnesium containing vanadium
It include the magnesium of 90~99wt% in alloy grain fining agent.
4, the magnesium intermediate alloy grain refiner containing vanadium is as the application in magnesium alloy refiner, the magnesium alloy packet
It includes containing Al and without the magnesium alloy of Al, the additive amount of the fining agent is 0.02~0.4wt.%.
The beneficial effects of the present invention are:
1, the present invention provides a kind of novel magnesium alloy grain refining agent containing vanadium, the existence form of vanadium is the carbonization of vanadium
The carbonitride of the nitride or/and vanadium of object or/and vanadium can be used as magnesium alloy effectively heterogeneous forming core particle, and be prepared into magnesium
Intermediate alloy, additive amount are easy to control, easy to use, and recovery rate is high, are not limited by magnesium alloy ingredient (containing Al and without Al
Magnesium alloy in can add).
2. the magnesium intermediate alloy grain refiner of the present invention containing vanadium after being added in magnesium alloy, effectively refines magnesium and closes
Gold strengthens magnesium and magnesium alloy, improves the comprehensive mechanical property of magnesium alloy.It is closed using the magnesium of grain refiner prepared by the present invention
Gold, crystallite dimension are about 115 μm (Fig. 1), compared to 320 μm of crystallite dimension (Fig. 2) of the magnesium alloy for being not added with grain refiner,
Grain refining effect is significant.
3. preparation method of the present invention, easy to operate, low in cost, it is suitable for scale industrial production, has wide
Market application prospect.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is the metallograph for being added to the Mg-3Al alloy of VC magnesium intermediate alloy；
Fig. 2 is the metallograph for being not added with the Mg-3Al alloy of fining agent of the present invention；
Fig. 3 is the preparation-obtained 99wt.%Mg-1wt.%VC of embodiment 40.5N0.5Intermediate alloy grain refiner wire rod
It applies in Mg-6Zn alloy as the obtained metallograph of fining agent；
Fig. 4 is the metallograph for being not added with Mg-6Zn alloy of the fining agent under identical smelting technology.
Specific embodiment
Below in conjunction with attached drawing, a preferred embodiment of the present invention will be described in detail.
Embodiment 1
The pure magnesium powder 360g of raw material, VC powder 40g are weighed, by above two powder ball milling mixing, ball-milling medium is alcohol, is pressed
Ratio of grinding media to material is 10:1, is protected as argon gas is passed through after in agate pot, vacuumizing, the ball milling 12h on planetary ball mill, between
It has a rest ball milling mode, i.e. ball milling 3h, suspends 20min, after the mixed-powder vacuum drying after ball milling, mixed-powder is as diameter
In the graphite jig of 70mm, in vacuum hotpressing stove, pressure 40MPa, hot pressing temperature is 550 DEG C, keeps the temperature 60min, and hot pressing obtains
Block is sintered to 90wt.%Mg-10wt.%VC intermediate alloy.
By above-mentioned intermediate alloy sintering block, vehicle preheats 2h at 400 DEG C after falling surface scale to suitable dimension, in crowded
In press, squeezing temperature is 400 DEG C, extrusion ratio 89:1, obtains closing among the 90wt.%Mg-10wt.%VC that diameter is 9mm
Golden grain refiner wire rod.
Embodiment 2
The pure magnesium powder 396g of raw material, VC powder 4g are weighed, by above two powder ball milling mixing, ball-milling medium is acetone, is pressed
It is 8:1 according to ratio of grinding media to material, is placed in agate pot, argon gas protection, the ball milling 6h on planetary ball mill, between is passed through after vacuumizing
It has a rest ball milling mode, i.e. ball milling 3h, suspends 15min.After the mixed-powder vacuum drying after ball milling, mixed-powder is as diameter
In the graphite jig of 70mm, in vacuum hotpressing stove, pressure 30MPa, hot pressing temperature is 450 DEG C, keeps the temperature 30min, and hot pressing obtains
Block is sintered to 99wt.%Mg-1wt.%VC intermediate alloy.
99wt.%Mg-1wt.%VC intermediate alloy is sintered block, vehicle falls after surface scale to suitable dimension 350
1h is preheated at DEG C, in extruder, squeezing temperature is 350 DEG C, extrusion ratio 89:1, obtains the 99wt.%Mg- that diameter is 9mm
1wt.%VC intermediate alloy grain refiner wire rod.
Embodiment 3
Pure Mg powder 360g, VN the powder 40g of raw material is weighed, by above two powder ball milling mixing, ball-milling medium is alcohol, according to
Ratio of grinding media to material is 8:1, is protected as argon gas is passed through after in agate pot, vacuumizing, the ball milling 6h on planetary ball mill, using interval
Ball milling mode, i.e. ball milling 3h suspend 15min.After the mixed-powder vacuum drying after ball milling, mixed-powder is as diameter
In the graphite jig of 70mm, in vacuum hotpressing stove, pressure 40MPa, hot pressing temperature is 450 DEG C, keeps the temperature 30min, and hot pressing obtains
Block is sintered to 90wt.%Mg-10wt.%VN intermediate alloy.
90wt.%Mg-10wt.%VN intermediate alloy is sintered block, vehicle falls after surface scale to suitable dimension 350
1h is preheated at DEG C, in extruder, squeezing temperature is 350 DEG C, and extrusion ratio 89:1 is obtained in the Mg-10wt.%VN of Φ 9mm
Between alloy grain fining agent wire rod.
Embodiment 4
Weigh pure Mg powder 100g and VC0.5N0.5Powder 10g, is placed in agate pot, ball milling mixing, ball-milling medium be alcohol or
Acetone is 6:1 according to ratio of grinding media to material, and argon gas protection, the ball milling 6h on planetary ball mill, using interval ball milling are passed through after vacuumizing
Mode, i.e. ball milling 3h suspend 15min.By the mixed-powder vacuum drying after ball milling, and it is pressed into the magnesium vanadium of 12mm × 50mm
Close object green compact.
900g magnesium ingot is placed in the stainless steel crucible for having applied BN coating, heat up melting in resistance furnace, in CO2With SF6It is mixed
It closing under gas shield, magnesium ingot is fused into magnesium liquid, the magnesium vfanadium compound green compact of 12mm × 50mm is pressed into magnesium liquid at 720 DEG C,
Until completely melted, 30min is kept the temperature, 5min is stirred, surface slag is destroyed, is poured into the cylindrical low-carbon punching block of 200 DEG C of preheating
In tool, 99wt.%Mg-1wt.%VC is obtained0.5N0.5Intermediate alloy ingot casting.Then ingot casting is removed end to end, turning is to suitable
1h is preheated after size at 350 DEG C, squeezing temperature is 350 DEG C, extrusion ratio 89:1, and extruding obtains the 99wt.%Mg- of Φ 9mm
1wt.%VC0.5N0.5Intermediate alloy grain refiner wire rod.
Embodiment 5
Raw material is pure Mg powder 400g, VC powder 50g and VN powder 50g, is placed in agate pot, ball milling mixing, ball-milling medium is wine
Essence or acetone are 6:1 according to ratio of grinding media to material, and argon gas protection is passed through after vacuumizing, and the ball milling 12h on planetary ball mill is used
Interval ball milling mode, i.e. ball milling 3h suspend 20min.By the mixed-powder vacuum drying after ball milling, and it is pressed into 12mm × 50mm
Magnesium vfanadium compound green compact.
500g magnesium ingot is placed in the stainless steel crucible for having applied BN coating, heat up melting in resistance furnace, in CO2With SF6It is mixed
It closing under gas shield, magnesium ingot is fused into magnesium liquid, the magnesium vfanadium compound green compact of 12mm × 50mm is pressed into magnesium liquid at 750 DEG C,
Until completely melted, the temperature of Serum Magnesium is adjusted to 720 DEG C, after keeping the temperature 30min, stirs 10min, surface slag is destroyed, is poured
In the cylindrical low-carbon steel mold for infusing 200 DEG C of preheating, the casting of 90wt.%Mg-5wt.%VC-5wt.%VN intermediate alloy is obtained
Ingot.Then ingot casting is removed end to end, preheats 1h after turning to suitable dimension at 400 DEG C, squeezing temperature is 400 DEG C, is squeezed
Than for 89:1, extruding obtains the 90wt.%Mg-5wt.%VC-5wt.%VN intermediate alloy grain refiner wire rod of Φ 9mm.
The preparation-obtained 90wt.%Mg-10wt.%VC intermediate alloy grain refiner wire rod of embodiment 1 is applied
Mg-3Al alloy is as fining agent, additive amount 0.03wt.%, and obtaining metallographic microscope as shown in Figure 1, (crystallite dimension is averagely about
115 μm), Mg-3Al alloy (average grain size of the fining agent under identical smelting technology is not added with corresponding to as shown in Figure 2
About 320 μm), it can be seen that the carbide of vanadium as fining agent can effective Refining Mg Alloy mention to play the role of refined crystalline strengthening
The comprehensive mechanical property of high magnesium alloy.
By the preparation-obtained 99wt.%Mg-1wt.%VC of embodiment 40.5N0.5Intermediate alloy grain refiner wire rod is answered
Fining agent is used as in Mg-6Zn alloy, additive amount 0.3wt.%, obtaining metallographic microscope as shown in Figure 3, (crystal grain is averaged ruler
Very little about 83 μm), corresponding to Mg-6Zn alloy of the fining agent under identical smelting technology that be not added with as shown in Figure 4, (crystal grain is flat
Equal size is about 187 μm), it can be seen that after addition grain refiner, alloy grain size distribution is more uniform.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (6)
1. the magnesium intermediate alloy grain refiner containing vanadium, which is characterized in that as mass fraction, the fining agent includes 90 ~ 99%
Magnesium, remaining be vanadium compound, the compound be VC, VN, VCxN1-xAt least one of, the VCxN1-xIn, 0 < x < 1；
The magnesium intermediate alloy grain refiner containing vanadium is prepared as follows:
(1) weigh according to the ratio magnesium powder and vanadium compound powder be placed in agate pot under the protection of argon gas ball milling mixing 6 ~
12h, using alcohol or acetone as ball-milling medium, ratio of grinding media to material is 6 ~ 10:1；
(2) by the mixed-powder vacuum drying after ball milling, after powder is placed in cylindric graphite jig, pressure be 25 ~
40MPa, temperature keep the temperature 30 ~ 60min, the cooling magnesium intermediate alloy sintering block obtained containing vanadium under the conditions of being 450 ~ 550 DEG C.
2. the preparation method of the magnesium intermediate alloy grain refiner described in claim 1 containing vanadium, which is characterized in that including walking as follows
It is rapid:
(1) weigh according to the ratio magnesium powder and vanadium compound powder be placed in agate pot under the protection of argon gas ball milling mixing 6 ~
12h, using alcohol or acetone as ball-milling medium, ratio of grinding media to material is 6 ~ 10:1；
(2) by the mixed-powder vacuum drying after ball milling, after powder is placed in cylindric graphite jig, pressure be 25 ~
40MPa, temperature keep the temperature 30 ~ 60min, the cooling magnesium intermediate alloy sintering block obtained containing vanadium under the conditions of being 450 ~ 550 DEG C.
3. the preparation method of the magnesium alloy intermediate alloy grain refiner containing vanadium according to claim 2, which is characterized in that institute
It states ball milling and 15 ~ 20min is suspended using intermittent ball milling mode, i.e. ball milling 3h using planetary ball mill.
4. the preparation method of the magnesium intermediate alloy grain refiner containing vanadium according to claim 2, which is characterized in that further include
Step (3): vehicle falls the surface scale of magnesium intermediate alloy sintering block of the gained containing vanadium, 1 ~ 2h is preheated at 350 ~ 400 DEG C, so
It is squeezed under the conditions of 350 ~ 400 DEG C of temperature, extrusion ratio 89:1 afterwards and obtains the magnesium intermediate alloy grain refiner wire rod containing vanadium.
5. the preparation method of the magnesium intermediate alloy grain refiner containing vanadium according to claim 4, which is characterized in that the stone
The diameter of black mold is 70mm, and the magnesium intermediate alloy grain refiner gauge or diameter of wire after extruding containing vanadium is 9mm.
6. the magnesium intermediate alloy grain refiner described in claim 1 containing vanadium is as the application in magnesium alloy refiner, the magnesium
Alloy includes containing Al and without the magnesium alloy of Al, and the additive amount of the fining agent is 0.02 ~ 0.4 wt.%.
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| CN111304509A (en) * | 2018-12-11 | 2020-06-19 | 长沙理工大学 | VN particle-added refined magnesium alloy and preparation method thereof |
| CN110643871A (en) * | 2019-10-30 | 2020-01-03 | 北京交通大学 | Novel heat-resistant high-strength Mg-Al-Ca-Gd magnesium alloy and preparation method thereof |
| CN113512675B (en) * | 2021-06-04 | 2022-06-03 | 上海航天精密机械研究所 | Ti-Zr-RE-Mg rare earth magnesium alloy grain refiner and preparation method thereof |
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| CN101705395B (en) * | 2009-10-29 | 2012-04-25 | 四川大学 | Vanadium-contained aluminum and aluminum alloy, and preparation methods thereof |
| CN102828061B (en) * | 2012-08-06 | 2016-01-27 | 四川大学 | Multiple elements design grain-refining agent and preparation method thereof |
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