CN106435419A - Production method for AZ91D alloy with ultra-fine grain solidification structure - Google Patents
Production method for AZ91D alloy with ultra-fine grain solidification structure Download PDFInfo
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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
- C22F1/06—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/09—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using pressure
- B22D27/11—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using pressure making use of mechanical pressing devices
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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
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
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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
- C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
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Abstract
The invention discloses a production method for AZ91D alloy with the ultra-fine grain solidification structure. The method includes the steps of 1, preprocessing and 2, high-pressure solidifying of samples. In the step 1, diffusion annealing is carried out on an AZ91D alloy ingot and the AZ91D alloy ingot is cut into the samples; and in the step 2, the samples in the step 1 are placed into a CS-1B type high-pressure cubic press for high-pressure solidification and then products are obtained. According to the production method for the AZ91D alloy with the ultra-fine grain solidification structure, the obtained products are high in strength and plasticity. In the AZ91D alloy obtained through the method, the grain size of a Mg substrate is reduced to 10 micrometers from 350 micrometers of virgin alloy, the dendritic structure is obviously refined, and the mode of distributing a beta-Mg17Al12 phase among dendritic crystals in a skeleton shape in a netted form of the virgin alloy is changed into the mode of distributing the beta-Mg17Al12 phase among the dendritic crystals in the shape of nanoscale particles in a dispersed form.
Description
Technical field
The present invention relates to a kind of preparation method of the AZ91D alloy with Ultra-fine Grained solidified structure, particularly belong to alloy system
Standby technical field.
Background technology
Magnesium alloy has good electric conductivity, heat conductivity, capability of electromagnetic shielding and high specific strength, specific stiffness, damping property etc.
Feature, is current practice structural metallic materials the lightest, in Aero-Space, automobile and 3C (computer, communication and consumption electricity
Sub- product) etc. industry have broad application prospects.However, magnesium alloy because intensity is relatively low, poor toughness, plastic working difficult,
The problems such as high temperature creep property difference, limit its application further industrially.Therefore, improved by various technologies of preparing
Magnesium alloy mechanical property, expands the emphasis that magnesium alloy range of application is the research and development of magnesium alloy technical field.
AZ91D is the representative alloy of Mg-Al system.The either sand casting of open report, permanent mold casting still solidify
Die casting faster, its as-cast structure is all thicker, and main hardening constituent β-Mg17Al12How to be linked to be net distribution in " skeleton shape " to exist
α-Mg interdendritic, not only β-Mg17Al12The invigoration effect of phase can not give full play to, and also can reduce the power of casting AZ91D alloy
Learn performance.Therefore, for improving AZ91D alloy mechanical property further, expand its range of application, refine AZ91D solidified structure, change
Kind β-Mg17Al12The form of phase just seems particularly significant with distribution.
Control the key means that process of setting is refinement cast magnesium alloy tissue.It is directed in process of setting both at home and abroad at present
The casting main refinement measure taken of AZ91D alloy is：Melt overheat method, solvent treatment method, alloying element additive process and molten
Body paddling process etc..But thinning effect is limited, average grain size is extremely difficult to less than hundred microns, and β-Mg17Al12Phase point
Cloth and form do not obtain improvement substantially.Therefore, research is a kind of can prepare the AZ91D with Ultra-fine Grained solidified structure
The method of alloy, it appears particularly necessary.
Content of the invention
For solving the deficiencies in the prior art, it is an object of the invention to provide a kind of have Ultra-fine Grained solidified structure
The preparation method of AZ91D alloy, products obtained therefrom has higher intensity and good plasticity.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that：
A kind of preparation method of the AZ91D alloy with Ultra-fine Grained solidified structure, comprises the following steps：
(1) pretreatment：Take AZ91D alloy cast ingot to be diffused annealing, cut into sample；
(2) sample High Pressure Solidification is processed：Sample in step (1) is placed in CS-1B type high pressure cubic hinge press and carries out height
Pressure solidification is processed, and obtains final product.
Specifically, the preparation method of the aforementioned AZ91D alloy with Ultra-fine Grained solidified structure, comprises the following steps：
(1) pretreatment：AZ91D alloy cast ingot is taken to be diffused annealing, wire cutting becomes sample；
(2) sample High Pressure Solidification is processed：Sample in step (1) is placed in CS-1B type high pressure cubic hinge press and carries out height
Pressure solidification is processed, and sets freezing pressure and preset temperature, pressure rise to freezing pressure is heated rapidly to preset temperature simultaneously
Afterwards, carry out heat-insulation pressure keeping at such a temperature, subsequently stop heating, naturally cool to room temperature under dwell condition, obtain final product after release.
The preparation method of the aforementioned AZ91D alloy with Ultra-fine Grained solidified structure, in step (2), freezing pressure be 2～
4GPa.
The preparation method of the aforementioned AZ91D alloy with Ultra-fine Grained solidified structure, in step (2), preset temperature is 850 DEG C
～950 DEG C.
The preparation method of the aforementioned AZ91D alloy with Ultra-fine Grained solidified structure, in step (2), a length of during heat-insulation pressure keeping
15min～20min.
The preparation method of the aforementioned AZ91D alloy with Ultra-fine Grained solidified structure, in step (1), specimen size is diameter 6
～12mm, length 6mm.Diameter is bigger, and rate of cooling is slower, and solidified structure average grain size is bigger.
In order to ensure the science, rationally, effectively of the present invention program, inventor has carried out series of experiments.
First, sample preparation
AZ91D alloy cast ingot is taken to be diffused annealing, preferably wire cutting becomes the sample of diameter 6mm, length 6mm.Sample chi
Very little bigger, rate of cooling is slower, and crystallite dimension is bigger, and performance is lower.Wherein, AZ91D alloy cast ingot composition is that (quality is divided
Number, %)：Al 9.163, Zn 0.538, Mn 0.218, the rest is Mg.Horizontal high voltage is entered using CS-1B type high pressure cubic hinge press
Experiment.Fig. 1 is high pressure cubic apparatus sample graphite group encapsulation schematic diagram.From in figure, graphite group encapsulation includes boron nitride crucible
With the graphite crucible being placed in outside boron nitride crucible, in WC supercharging post, the symmetrical both sides being pressurized post positioned at WC set for integral installation
There is pyrophillite, hexahedro in graphite group encapsulation is provided with hammer.Sample is placed in the boron nitride crucible in graphite group encapsulation, so
Afterwards the graphite assembling group encapsulation is put into the cavity position of high pressure cubic apparatus, after tup be aligned, start High Pressure Solidification experiment.If
Determine freezing pressure and preset temperature, pressure rise to freezing pressure 2～4GPa is heated rapidly to 850 DEG C of preset temperature simultaneously
After～950 DEG C, carry out heat-insulation pressure keeping 15min～20min at such a temperature, subsequently stop heating, under dwell condition, be cooled to room
Temperature, obtains final product after release.
2nd, experimental result and analysis
1st, observation by light microscope
Observed using Axio Scope A1 pol type optical microscope (OM) and analyze technic metal microscopic structure.As Fig. 2
Shown.Fig. 2 is respectively AZ91D alloy cast ingot tissue and the present invention has the OM picture of Ultra-fine Grained solidified structure AZ91D alloy.By scheming
2A understands, AZ91D alloy cast ingot is organized as thick arborescent structure, and average grain size is about 350 μm.Fig. 2 B is 4GPa high pressure
Under effect, heating fusion temperature is 850 DEG C, the AZ91D with Ultra-fine Grained solidified structure obtaining after insulation 20min power-off cooling
Alloy.Contrast Fig. 2A understand, high pressure solidification microstructure maximum feature, one is that in unit area, nucleus number significantly increases, two be α-
Mg crystal is the shorter equiax crystal of arm lengths, and its average grain size is only 10 μm about.Fig. 2 C and Fig. 2 D is respectively
Under the effect of 4GPa high pressure, the AZ91D alloy with Ultra-fine Grained solidified structure of acquisition under 900 DEG C and 950 DEG C heating melting conditions
Pattern.Comparison diagram 2B understands, during the lower solidification of high pressure effect, arm lengths of dendrite, and that is, equiax crystal crystallite dimension is as well as molten
The body degree of superheat raises and grows, and has occurred substantially to grow up, as shown in Figure 2 D under 950 DEG C (melt superheat degree is more than 100 DEG C).Can
See, during the lower solidification of GPa high pressure effect, melt superheat degree is still one of important factor in order of impact solidification thickness.
2nd, scanning electron microscopic observation
Observe and analyze technic metal microscopic structure using LEO JSM 5400 type scanning electron microscope (SEM).As shown in Figure 3.
Fig. 3-A and Fig. 3-B is the SEM figure under AZ91D alloy cast ingot different amplification, and from figure, AZ91D alloy cast ingot is organized
By nascent-Mg+ (- Mg+ β-Mg17Al12) eutectic structure and the white mesophase β-Mg that formed because of interdendritic richness aluminum17Al12Group
Become, wherein eutectic β-Mg17Al12Xiang Duocheng " skeleton shape " is linked to be net distribution in-Mg interdendritic.Fig. 3-C and Fig. 3-D is difference
Under amplification, what 4GPa high pressure obtained under acting on after 850 DEG C of heating fusings has Ultra-fine Grained solidified structure AZ91D alloy
SEM schemes.With Fig. 3-A, in 3-B, AZ91D As-cast Microstructure is compared and is understood, has Ultra-fine Grained solidified structure under high pressure effect
The maximum feature of AZ91D alloy is：Under low power, (Fig. 3-C) second is mutually in granular form Dispersed precipitate on matrix, under high power (Fig. 3-
D) it is closely sized to being distributed on crystal boundary of graininess the second phase even dispersion of nm level.EDS inspection result shows, graininess second
In phase the atomic percentage of Mg, Al and Zn be respectively 58.34%, 36.12% and 5.54%, in matrix Al and Zn dissolubility
3.50% (mass fraction, similarly hereinafter) and 0.35% respectively；Compared with original AZ91D As-cast Microstructure, there is ultra-fine crystal solidification
β-Mg in tissue AZ91D alloy17Al12Dissolved with more Zn (original 2.48%), (original dissolved with more Al in matrix
2.46%).In conjunction with the XRD spectrum shown in Fig. 4, High Pressure Solidification AZ91D alloy structure is still by-Mg matrix and β-Mg17Al12Mutually group
Become.
3rd, X-ray diffraction analysis
Carry out material phase analysis using 2500/PC type X-ray diffractometer, scanning step be 0.3 °, 20 ° with 90 ° (2 θ) it
Between measurement obtain XRD diffraction spectra.As shown in Figure 4.XRD as shown in Figure 4 composes-Mg after High Pressure Solidification that can be visible in detail
Diffraction maximum half-peak breadth substantially widen, β-Mg17Al12Phase diffraction maximum has steamed bun peak to be inclined to, and this further illustrates original thick
After AZ91D alloy cast ingot solidifies under the effect of 4GPa high pressure, not only-Mg matrix is significantly refined, and is distributed interdendritic
β-Mg17Al12Phase morphology is also greatly improved with distribution, β-Mg17Al12By " skeleton shape " in AZ91D alloy cast ingot even
Continuous be distributed in interdendritic and be changed into nm grade particles shape even dispersion be distributed on crystal boundary.
4th, compression performance
Room temperature compression experiment, strain rate are carried out using WDW3100 microcomputer controlled electronic universal testerFor 0.001s-1, by data such as the subsidiary computerized data logger automatic data collection stress of universal testing machine, strains in compression process.Knot
Fruit such as Fig. 5 is shown.From in figure, the comprcssive strength of AZ91D alloy cast ingot is 263MPa, and section expansion rate is 14%；And
Under the effect of 4GPa high pressure, its comprcssive strength of AZ91D alloy of solidification is up to 402MPa, and section expansion rate is 20%.High Pressure Solidification
Not only greatly improve magnesium alloy strength, also improve magnesium alloy plasticity to a certain extent.
Fig. 6 is the fracture apperance SEM figure of the AZ91D alloy with Ultra-fine Grained solidified structure.The compression of AZ91D alloy cast ingot is disconnected
Section (fracture) after splitting is in about 45 ° with compression axis, and fracture is smooth and bright；Fracture SEM picture shown in from Fig. 6 a can be seen that,
Its fracture is to occur along a specific crystallographic plane (cleavage surface), and cleavage surface is big and smooth, and cleavage step is more straight, allusion quotation
The cleavage fracture of type.And as Fig. 6 b understands, what High Pressure Solidification obtained has its compression fracture of Ultra-fine Grained solidified structure AZ91D alloy
The cleavage area of plane is obviously reduced, and cleavage step highly significant reduces, and cleavage step is to be linked to be slope, fluctuating by less step
Uneven；There is a tear-strap cleavage step bonding pad up and down, amplifies (Fig. 6 c) further and can be clearly seen that at tear-strap two ends
There is shearing dimple.Show that the compression failure mode with Ultra-fine Grained solidified structure AZ91D alloy of High Pressure Solidification is closed compared with AZ91D
Golden ingot casting changes, and fracture mode is closer to quasi-cleavage crack.
For controlling metal or alloy process of setting, traditional method is to change solidification group by adjusting chemical composition and temperature
Knit, and generally ignore another thermodynamic parameter pressure of impact process of setting.Pressure is all attached most importance to temperature and chemical composition
The thermodynamic variable wanted, also has important impact to the process of setting of metal or alloy, when especially pressure reaches GPa level,
Greatly changed the thermodynamics and kineticses of metal or alloy process of setting.Theoretical according to existing High Pressure Solidification, pressure is total
It is so that forming core activation energy is reduced, increase nucleation rate；Suppression atoms permeating, makes atoms permeating activation energy increase, and thus increases crystal
Activation energy, reduces crystal growth rate.
Freezing pressure has strong influence to the acquisition of ultra-fine arborescent structure, when solidifying under the effect of GPa level high pressure, molten
Mass diffusivity can exponentially reduce again, then easily form solute atoms enrichment region in the base, have in crystals heterogeneous
The presence of equiax crystal considerably increases crystal nucleation rate, and the speed of growth of crystal also suffers from suppressing simultaneously, so in superelevation
Under Pressure Solidification, the arborescent structure of alloy is significantly refined.It is larger that heating-up temperature is that melt superheat degree also has to solidified structure
Impact, too high heating-up temperature not only can make solidified structure be roughened, and makes crystals growth turn to dendrite by globular crystal.
Spontaneous nano-scale particle shape β-Mg17Al12There is an optimal High Pressure Solidification experimental parameter in being formed of phase, freezing pressure is excessive,
More Al can be promoted to dissolve in Mg matrix, graininess β-Mg17Al12Phase amount can reduce；Freezing pressure is too small, β-Mg17Al12
Meet and still can be linked to be in " skeleton shape " netted or semicontinuous be distributed in interdendritic.
In the present invention, there is the AZ91D alloy of Ultra-fine Grained solidified structure, its Characteristics of As-cast Structure is by nano-scale particle
Shape β-Mg17Al12Mutually form with α-Mg matrix, α-Mg is in globular crystal, average grain size is about 10 μm, Al in α-Mg matrix
Solid solution capacity is up to 3.50wt%, far above the 2.48wt% of original AZ91D alloy；β-Mg17Al12Mutually it is in granular form, a size of nm
Level, Dispersed precipitate is in α-Mg interdendritic, β-Mg17Al12Mutually it is in granular form shared percentage by volume and be about 8%.
The intensity of material is a mechanical performance index extremely sensitive to composition, organizational structure.From Fig. 2,3, former
Begin to organize the AZ91D alloy of thick (350 μm of crystallite dimension) crystallite dimension after 4GPa, 850 DEG C of High Pressure Solidifications to refine to 10 μm.
According to Hall-Petch formula (σs=σ0+kd-1/2In formula：σ is the yield strength of alloy；σ0It is relevant with crystal type with k
Constant；D is crystallite dimension), the yield strength of alloy is inversely proportional to the square root of crystallite dimension.And the Hall-Petch of magnesium alloy
Very big (k=280～320MPa μm of constant k value-1/2), the strengthening effect that therefore magnesium alloy grains produce is extremely notable.
Therefore, high pressure solidification microstructure refinement contributes maximum to the raising of magnesium alloy strength.Secondly, after High Pressure Solidification, Al is in the base
Dissolubility bring up to 3.50% by 2.48% in virgin alloy, solution strengthening also has certain tribute to the lifting of alloy strength
Offer.Furthermore, the β-Mg in solidified structure17Al12From isolate matrix netted be changed into nm grade particles shape Dispersed precipitate, not only make
The effect of matrix can give full play to, simultaneously the higher graininess β-Mg of the hardness of Dispersed precipitate17Al12Mutually also can play certain
Dispersion-strengthened action.As can be seen here, the magnesium alloy of High Pressure Solidification is because of the common work of refined crystalline strengthening, dispersion-strengtherning and solution strengthening
With making alloy strength increase substantially, 402MPa being brought up to by the 263MPa of original AZ91D alloy cast ingot, improves nearly 50%.
What the lower solidification of high pressure effect obtained has Ultra-fine Grained solidified structure AZ91D alloy while intensity improves, and it is moulded
Property is also improved.High Pressure Solidification makes AZ91D alloy grain size significantly be refined, and reaches 10 μm；With
Crystallite dimension refines, and crystal boundary proportion increases, and the effect that crystal boundary is coordinated will be obvious, and material deformation is more uniform, material
Compressive strength and plasticity be all improved.Additionally, having improvement and second phase of Ultra-fine Grained solidified structure AZ91D alloy plasticity
Shape with much relations are distributed with.β-Mg in original AZ91D As-cast Microstructure17Al12Mutually it is distributed in dendrite in continuous net-shaped
Between, matrix phase is surrounded, alloy easily mutually ftractures along continuous second very much；And after High Pressure Solidification, β-Mg17Al12It is in mutually nm
On crystal boundary, this may be also that plasticity obtains and improves one of reason to a certain extent to grade particles shape Dispersed precipitate.
The invention has benefit that：A kind of AZ91D alloy with Ultra-fine Grained solidified structure that the present invention provides
Preparation method, by AZ91D alloy cast ingot GPa level high pressure effect under solidified, by control freezing pressure, heating-up temperature and
Alloy material needed for solidification cooling rate acquisition.The AZ91D alloy with Ultra-fine Grained solidified structure of the present invention has higher
Mechanical property.One side Mg matrix grain size is reduced to 10 μm by 350 μm of virgin alloy, and arborescent structure obtains significantly thin
Change；On the other hand, β-Mg17Al12It is linked to be net distribution by virgin alloy in " skeleton " shape to be changed in nanometer in interdendritic
Grade particles shape Dispersed precipitate is in interdendritic；Furthermore, Mg matrix solid solution Al amount significantly increases, and is increased by the 2.4wt% of virgin alloy
3.50wt% under high pressure, increased 24%.Make especially under freezing pressure 4GPa, 850 DEG C of heating conditions of heating-up temperature
The standby AZ91D alloy obtaining, the comprcssive strength under room temperature is 402MPa, and section expansion rate is 20%.Show High Pressure Solidification AZ91D
Alloy has higher intensity and good plasticity.
Brief description
Fig. 1 is high pressure cubic apparatus sample graphite group encapsulation schematic diagram；
Fig. 2 is the optical microscope of the AZ91D alloy with Ultra-fine Grained solidified structure of the present invention；
Fig. 3 is the SEM figure of the AZ91D alloy with Ultra-fine Grained solidified structure；
Fig. 4 is the XRD figure of the AZ91D alloy with Ultra-fine Grained solidified structure；
Fig. 5 is the stress-strain curve of the AZ91D alloy with Ultra-fine Grained solidified structure；
Fig. 6 is the fracture apperance SEM figure of the AZ91D alloy with Ultra-fine Grained solidified structure；
The implication of in figure reference：Fig. 1：1- pyrophillite, 2- graphite crucible, 3-WC is pressurized post, 4- boron nitride crucible, 5-
Sample, 6- hammer；Fig. 2：A-AZ91D alloy cast ingot, B-4GPa, 850 DEG C, C-4GPa, 900 DEG C, D-4GPa, 950 DEG C；Fig. 3：A-
AZ91D alloy cast ingot, 100 times of amplification, B-AZ91D alloy cast ingot, 500 times of amplification, C-4GPa, 850 DEG C, 100 times of amplification, D-
4GPa, 850 DEG C, 500 times of amplification；Fig. 4 and Fig. 5：A-4GPa, 850 DEG C, b-AZ91D alloy cast ingot；Fig. 6：A-AZ91D alloy is cast
Ingot, amplifies 200 times, and b- AZ91D of the present invention alloy amplifies 200 times, c- AZ91D of the present invention alloy, amplifies 500 times.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further introduced.
Embodiment 1
A kind of preparation method of the AZ91D alloy with Ultra-fine Grained solidified structure, comprises the following steps：
(1) pretreatment：AZ91D alloy cast ingot is taken to be diffused annealing, wire cutting becomes the sample of diameter 10mm, length 6mm；
(2) sample High Pressure Solidification is processed：Sample in step (1) is placed in CS-1B type high pressure cubic hinge press and carries out height
Pressure solidification is processed, and sets freezing pressure and preset temperature, pressure rise to freezing pressure 2GPa is heated rapidly to preset simultaneously
After 950 DEG C of temperature, carry out heat-insulation pressure keeping at such a temperature, subsequently stop heating 18min, under dwell condition, naturally cool to room
Temperature, obtains final product after release.
Embodiment 2
A kind of preparation method of the AZ91D alloy with Ultra-fine Grained solidified structure, comprises the following steps：
(1) pretreatment：AZ91D alloy cast ingot is taken to be diffused annealing, wire cutting becomes the sample of diameter 12mm, length 6mm；
(2) sample High Pressure Solidification is processed：Sample in step (1) is placed in CS-1B type high pressure cubic hinge press and carries out height
Pressure solidification is processed, and sets freezing pressure and preset temperature, pressure rise to freezing pressure 3GPa is heated rapidly to preset simultaneously
After 900 DEG C of temperature, carry out heat-insulation pressure keeping at such a temperature, subsequently stop heating 20min, under dwell condition, naturally cool to room
Temperature, obtains final product after release.
Embodiment 3
A kind of preparation method of the AZ91D alloy with Ultra-fine Grained solidified structure, comprises the following steps：
(1) pretreatment：AZ91D alloy cast ingot is taken to be diffused annealing, wire cutting becomes the sample of diameter 6mm, length 6mm；
(2) sample High Pressure Solidification is processed：Sample in step (1) is placed in CS-1B type high pressure cubic hinge press and carries out height
Pressure solidification is processed, and sets freezing pressure and preset temperature, pressure rise to freezing pressure 4GPa is heated rapidly to preset simultaneously
After 850 DEG C of temperature, carry out heat-insulation pressure keeping at such a temperature, subsequently stop heating 15min, under dwell condition, naturally cool to room
Temperature, obtains final product after release.
Embodiment 4
A kind of preparation method of the AZ91D alloy with Ultra-fine Grained solidified structure, comprises the following steps：
(1) pretreatment：AZ91D alloy cast ingot is taken to be diffused annealing, wire cutting becomes the sample of diameter 9mm, length 6mm；
(2) sample High Pressure Solidification is processed：Sample in step (1) is placed in CS-1B type high pressure cubic hinge press and carries out height
Pressure solidification is processed, and sets freezing pressure and preset temperature, pressure rise to freezing pressure 4GPa is heated rapidly to preset simultaneously
After 900 DEG C of temperature, carry out heat-insulation pressure keeping at such a temperature, subsequently stop heating 16min, under dwell condition, naturally cool to room
Temperature, obtains final product after release.
Embodiment 5
A kind of preparation method of the AZ91D alloy with Ultra-fine Grained solidified structure, comprises the following steps：
(1) pretreatment：AZ91D alloy cast ingot is taken to be diffused annealing, wire cutting becomes the sample of diameter 8mm, length 6mm；
(2) sample High Pressure Solidification is processed：Sample in step (1) is placed in CS-1B type high pressure cubic hinge press and carries out height
Pressure solidification is processed, and sets freezing pressure and preset temperature, pressure rise to freezing pressure 2.5GPa is heated rapidly to pre- simultaneously
If after 930 DEG C of temperature, carry out heat-insulation pressure keeping at such a temperature, subsequently stop heating 19min, under dwell condition, naturally cool to room
Temperature, obtains final product after release.
Claims (6)
1. a kind of preparation method of the AZ91D alloy with Ultra-fine Grained solidified structure it is characterised in that：Comprise the following steps：
(1) pretreatment：Take AZ91D alloy cast ingot to be diffused annealing, cut into sample；
(2) sample High Pressure Solidification is processed：Sample in step (1) is placed in CS-1B type high pressure cubic hinge press enter horizontal high voltage coagulate
Gu processing, obtain final product.
2. the AZ91D alloy with Ultra-fine Grained solidified structure according to claim 1 preparation method it is characterised in that：
Comprise the following steps：
(1) pretreatment：AZ91D alloy cast ingot is taken to be diffused annealing, wire cutting becomes sample；
(2) sample High Pressure Solidification is processed：Sample in step (1) is placed in CS-1B type high pressure cubic hinge press enter horizontal high voltage coagulate
Gu processing, set freezing pressure and preset temperature, by pressure rise to freezing pressure, after being heated rapidly to preset temperature simultaneously,
Carry out heat-insulation pressure keeping at such a temperature, subsequently stop heating, naturally cool to room temperature under dwell condition, obtain final product after release.
3. the AZ91D alloy with Ultra-fine Grained solidified structure according to claim 2 preparation method it is characterised in that：
In described step (2), freezing pressure is 2～4GPa.
4. the AZ91D alloy with Ultra-fine Grained solidified structure according to claim 2 preparation method it is characterised in that：
In described step (2), preset temperature is 850 DEG C～950 DEG C.
5. the AZ91D alloy with Ultra-fine Grained solidified structure according to claim 2 preparation method it is characterised in that：
In described step (2), a length of 15min～20min during heat-insulation pressure keeping.
6. the preparation method of the AZ91D alloy with Ultra-fine Grained solidified structure according to claim 1 and 2, its feature exists
In：In described step (1), specimen size is diameter 6～12mm, length 6mm.
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| CN112159914A (en) * | 2020-09-18 | 2021-01-01 | 衢州学院 | TiAl micron crystal prepared under high pressure and method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20050199363A1 (en) * | 2004-03-15 | 2005-09-15 | Spx Corporation | Magnesium alloy and methods for making |
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| US20050199363A1 (en) * | 2004-03-15 | 2005-09-15 | Spx Corporation | Magnesium alloy and methods for making |
| CN101134234A (en) * | 2007-07-23 | 2008-03-05 | 陕西科技大学 | Internal pressure expansion type casting technique |
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| CN112159914A (en) * | 2020-09-18 | 2021-01-01 | 衢州学院 | TiAl micron crystal prepared under high pressure and method thereof |
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