CN109226767A - Prepare the high pressure high temperature synthetic method of second phase particles simulation material in aluminium alloy - Google Patents
Prepare the high pressure high temperature synthetic method of second phase particles simulation material in aluminium alloy Download PDFInfo
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- CN109226767A CN109226767A CN201810839353.9A CN201810839353A CN109226767A CN 109226767 A CN109226767 A CN 109226767A CN 201810839353 A CN201810839353 A CN 201810839353A CN 109226767 A CN109226767 A CN 109226767A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0483—Alloys based on the low melting point metals Zn, Pb, Sn, Cd, In or Ga
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
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Abstract
The invention discloses a kind of methods for preparing second phase particles simulation material in aluminium alloy based on high pressure high temperature condition, specifically based on the chemical component metering ratio of second phase particles in aluminium alloy, biscuit is suppressed using pure metal powder, apply GPa grades of high pressures on diamond cubic hinge press, then, it is heated to high temperature and keeps the temperature a period of time, finally, being cooled to room temperature in the case where keeping high pressure effect.Using high pressure high temperature synthetic method of the present invention, it can prepare that, chemical component mutually identical as second phase particles object in aluminium alloy be accurate, sample size meets the simulation material that Conventional electrochemical test needs, thus to lay the foundation using the corrosion electrochemical action that simulation electrode method studies second phase particles in aluminium alloy indirectly.
Description
Technical field
The invention belongs to technical field of intermetallic compound, more particularly to are prepared using high pressure high temperature synthetic method
Second phase particles simulation material in aluminium alloy.
Background technique
A variety of addition element such as Zn, Mg, Cu, Si, Fe, Ni, Zr, Ti or impurity element are usually contained in aluminium alloy.These
Different types of intermetallic compound second phase particles, including micron-size crystalline phase are commonly formed in element in aluminium alloy forming process
(such as AlFe, AlFeSi), submicron order disperse phase (such as Al6Mn、Al3) and nanoscale precipitated phase (such as MgZn Zr2、Mg2Si、
Al2Cu) etc..Aluminium alloy is often resulted in when these second phase particles, local corrosion occurs, for example, intercrystalline corrosion and nanoscale crystal boundary are analysed
Mutually closely related out, micron-size crystalline phase then often results in spot corrosion.Intrinsically, these local corrosions belong to electrochemistry corruption
Erosion behavior.Therefore, the electrochemical behavior for accurately grasping second phase particles is to understand, control and eliminate the behavior of aluminium alloy local corrosion
Premise.
Under normal conditions, second phase particles size is very tiny in aluminium alloy, it is difficult to directly adopt Conventional electrochemical test
Method characterizes its corrosion electrochemical action.In order to solve this problem: first is that directly being analyzed using microcell Electrochemical Measurement Technology
The corrosion electrochemical action of second phase particles in aluminium alloy, such as scanning Kelvin probe force microscopy, scan-type electrochemical are micro-
Mirror, micro cell etc..However, microcell Electrochemical Measurement Technology measurement accuracy is low, resolution ratio is low, environmental disturbances are big, nano-probe
Preparation is difficult, is especially difficult to directly characterize the corrosion electrochemical action of nanoscale precipitated phase；Second is that indirect using simulation electrode method
The corrosion electrochemical action for characterizing second phase particles in aluminium alloy, according to the Chemical Composition Characteristics of second phase particles, using founding,
Corresponding simulation material is prepared in the methods of sintering, magnetron sputtering, and then is tested using corrosion electrochemistry method is often seen.Mould
Quasi- electrode method has many advantages, such as that test is simple, signal interference is small, test result is accurate, however, difficulty is how to prepare energy
It enough accurately reflects second phase particles property and composition characteristic, sample is dimensioned for the simulation material of Conventional electrochemical measurement, that is, want
Guarantee that simulation material is mutually identical as second phase particles object, chemical component is accurate, sample size meets test request (sample section
Face size is in 1cm × 1cm or more) etc..
Summary of the invention
As previously mentioned, characterizing second phase particles corrosion electrochemical action in aluminium alloy indirectly to meet simulation electrode method
It is required that key is how accurately to prepare, mutually identical as second phase particles object, chemical component is accurate, sample size is suitble to often again
Advise the simulation material that electro-chemical test needs.For this purpose, the present invention is with the following method: according to target second phase particles in aluminium alloy
Chemical component measure ratio, Synthetic block and is assembled at biscuit using the compacting of pure metal powder first, is then assemblied in diamond
On cubic hinge press and apply GPa grades of high pressures, when being heated to the high temperature more than second phase particles normal pressure fusing point and keeping the temperature one section
Between, it is finally cooled to room temperature in the case where keeping high pressure effect, the second phase particles for meeting above-mentioned requirements can be prepared through the method
Simulation material.
The present invention has the advantages that for most metal materials under high pressure effect, fusing point is big compared under condition of normal pressure
Amplitude improves.For example, pure Al fusing point is about 660 DEG C under condition of normal pressure, but under the effect of 5GPa high pressure, fusing point can be increased to about
1000℃.It follows that under the hyperpressure effect that diamond cubic hinge press generates, it can be using higher than the second phase
The heating temperature of particle normal pressure fusing point is sintered, at this point, atom diffusion is fast, crystal grain is grown up rapidly, Elemental redistribution is uniform；
Secondly, forming very strict sealing effect, energy in diamond cubic hinge press working chamber in the case where GPa grades of high pressures act on
It is enough that chemical component caused by biscuit element vaporization at high temperature or oxidation is effectively avoided to significantly change, to guarantee the second phase grain of preparation
Submodule intends material composition and design content consistency；In addition, can effectively avoid preparation when being cooled down under high pressure effect
Split-phase occurs for second phase particles simulation material, to guarantee the phase unicity of simulation material.Therefore, it is synthesized using high pressure high temperature
Method can accurately prepare that object is mutually identical, chemical component is accurate, sample size meets Conventional electrochemical test needs second
Phase particle simulation material, thus for second phase particles in simulation electrode method research aluminium alloy corrosion electrochemical action establish it is solid
Basis.
Second phase particles simulation material preparation step is as follows in aluminium alloy of the present invention:
(1) prefabricated biscuit processing.It is measured according to the chemical component of second phase particles in aluminium alloy than (molar ratio), weighs phase
The pure metal powder for answering element, carried out on batch mixer it is uniformly mixed, then, according to diamond cubic hinge press graphite bush
Inner cavity dimensioned green compact mold, then weighs appropriate mixing and pours into green compact mold, and finally compacting powder is plain on a hydraulic press
Base, sample size needed for which is at least greater than Conventional electrochemical test.
(2) sintering processes.The powder biscuit suppressed is pressed into graphite bush inner cavity, after both ends are using graphite flake sealing
It is assembled into Synthetic block, then Synthetic block is mounted in diamond cubic hinge press working chamber, after applying 1-5GPa high pressure, is led to
Electric heating 50-200 DEG C and keeps the temperature 10-60 minutes to second phase particles normal pressure fusing point is above, is sintered.In general,
On-load pressure is higher, and higher, soaking time, which can be set, in heating temperature accordingly can suitably shorten.
(3) cooling treatment.After the completion of sintering, in the case where keeping the effect of 1-5GPa high pressure, power-off is cooled to room temperature, then release
Sample is taken out, second phase particles simulation material can be obtained.
Detailed description of the invention
Fig. 1 is the XRD spectrum of 1 synthetic sample of embodiment.
Fig. 2 is the SEM power spectrum surface analysis result of 1 synthetic sample of embodiment.
Fig. 3 is the SEM power spectrum surface analysis result of 2 synthetic sample of embodiment.
Fig. 4 is the SEM power spectrum surface analysis result of 3 synthetic sample of embodiment.
Fig. 5 is the SEM power spectrum surface analysis result of 4 synthetic sample of embodiment.
Fig. 6 is the SEM power spectrum surface analysis result of 5 synthetic sample of embodiment.
Fig. 7 is the XRD spectrum of 1 synthetic sample of comparative example.
Specific embodiment
The present invention is described in further detail below with reference to embodiment, but protection scope of the present invention is not limited to listed implementation
Scheme:
With most typical precipitated phase MgZn in industrial widely used 7000 line aluminium alloy below the present invention2Phase (according to
Mg-Zn binary phase diagraml is it is found that MgZn2Phase normal pressure fusing point is about 600 DEG C) for, high pressure high temperature synthetic method is made further
It is described in detail, green compact mold used in following embodiment and comparative example is previously according on diamond cubic hinge press
Chamber size prepares in graphite bush, and size is greater than size needed for Conventional electrochemical test sample.
Test method:
Energy disperse spectroscopy is attached to using JSM-6010LA type Scanning Electron microscope (SEM) and carries out constituent analysis；
Material phase analysis is carried out using Bruker D8 type X-ray diffractometer (XRD).
Embodiment 1:
By MgZn2The chemical component of phase measures ratio, weighs suitable technical pure Zn powder and pure Mg powder, pours into after mixing
In green compact mold, the powder biscuit having a size of φ 30mm × 30mm is suppressed on a hydraulic press；Then, the biscuit suppressed is pressed into
In graphite bush of the inner cavity having a size of φ 30mm × 40mm, Synthetic block is sealed and be assembled into both ends with φ 30mm × 5mm graphite flake,
And then be assemblied in diamond cubic hinge press working chamber, after applying 5GPa pressure, electrified regulation is to about 800 DEG C and keeps the temperature
10 minutes, pressure is then kept, power-off is cooled to room temperature rear release and takes out sample.
Fig. 1 is the XRD spectrum of 1 synthetic sample of embodiment, it can be seen that MgZn is contained only in sample2The diffraction maximum of phase.Fig. 2
For the SEM power spectrum surface analysis result of 1 synthetic sample of embodiment, it can be seen that (Mg+Al+Si)/Zn atomic ratio is close to 1 in sample:
2, very close MgZn2The chemical component of phase measures ratio, wherein Al, Si are from impurity element in powder, usually to replace shape
Formula replaces MgZn2Mg atom in phase.Fig. 1 and Fig. 2 shows accurately prepare object phase using high pressure high temperature synthetic method
Identical, chemical component is accurate, size meets the second phase particles simulation material that Conventional electrochemical test needs.
Embodiment 2
By MgZn2The chemical component of phase measures ratio, weighs suitable technical pure Zn powder and pure Mg powder, pours into after mixing
In green compact mold, the powder biscuit having a size of φ 30mm × 50mm is suppressed on a hydraulic press；Then, the biscuit suppressed is pressed into
In graphite bush inner cavity, and it is assembled into Synthetic block, and then be assemblied in diamond cubic hinge press working chamber, applies 1GPa
Electrified regulation keeps the temperature 60 minutes to about 650 DEG C after pressure, then keeps pressure, and power-off is cooled to room temperature rear release and takes out sample.
Fig. 3 is the power spectrum surface analysis of 2 synthetic sample of embodiment results, it can be seen that (Mg+Al+Si)/Zn atom in sample
Than showing to contain only MgZn in sample close to 1:22A type of intermetallic compound phase.
Embodiment 3
By MgZn2The chemical component of phase measures ratio, weighs suitable technical pure Zn powder and pure Mg powder, pours into after mixing
In green compact mold, the powder biscuit having a size of φ 30mm × 50mm is suppressed on a hydraulic press；Then, the powder biscuit that will be suppressed
In indentation graphite bush inner cavity and it is assembled into Synthetic block, and then is assemblied in diamond cubic hinge press working chamber, is applied
Electrified regulation keeps the temperature 40 minutes to about 700 DEG C after 2GPa pressure, and after then holding pressure and power-off are cooled to room temperature, release is taken
Sample out.
Fig. 4 is the SEM power spectrum surface analysis of 3 synthetic sample of embodiment results, it can be seen that (Mg+Al+Si)/Zn in sample
Atomic ratio shows to contain only MgZn in sample close to 1:22A type of intermetallic compound phase.
Embodiment 4
By MgZn2The chemical component of phase measures ratio, weighs suitable technical pure Zn powder and pure Mg powder, pours into after mixing
In green compact mold, the powder biscuit having a size of φ 30mm × 50mm is suppressed on a hydraulic press；Then, the powder biscuit that will be suppressed
In indentation graphite bush inner cavity and it is assembled into Synthetic block, and then is assemblied in diamond cubic hinge press working chamber, is applied
Electrified regulation keeps the temperature 30 minutes to about 700 DEG C after 3GPa pressure, then keeps pressure, and power-off is cooled to room temperature rear release and takes out
Sample.
Fig. 5 is the SEM energy spectrum analysis of 4 synthetic sample of embodiment, it can be seen that (Mg+Al+Si)/Zn atomic ratio in sample
Close to 1:2, this shows to contain only MgZn in sample2A type of intermetallic compound phase.
Embodiment 5
By MgZn2The chemical component of phase measures ratio, weighs suitable technical pure Zn powder and pure Mg powder, pours into after mixing
In green compact mold, the powder biscuit having a size of φ 30mm × 50mm is suppressed on a hydraulic press；Then, the powder biscuit that will be suppressed
In indentation graphite bush inner cavity and it is assembled into Synthetic block, and then is assemblied in diamond cubic hinge press working chamber, is applied
Electrified regulation keeps the temperature 20 minutes to about 750 DEG C after 4GPa pressure, then keeps pressure, and power-off is cooled to room temperature rear release and takes out
Sample.
Fig. 6 is the SEM energy spectrum analysis of 5 synthetic sample of embodiment, it can be seen that (Mg+Al+Si)/Zn atomic ratio in sample
Close to 1:2, this shows to contain only MgZn in sample2A type of intermetallic compound phase.
Comparative example 1
By MgZn2The chemical component of phase measures ratio, weighs suitable technical pure Zn powder and pure Mg powder, pours into after mixing
In green compact mold, the powder biscuit having a size of φ 30mm × 50mm is suppressed on a hydraulic press；Then, the powder biscuit that will be suppressed
In indentation graphite bush inner cavity and it is assembled into Synthetic block, and then is assemblied in diamond cubic hinge press working chamber, is applied
Electrified regulation to about 650 DEG C and keeps the temperature 60 minutes after 1GPa pressure, is cooled to room temperature finally, laying down pressure and powering off, takes out sample
Product.
Fig. 7 is the XRD spectrum of 1 synthetic sample of comparative example, it can be seen that in addition to MgZn in synthetic sample2Phase diffraction
Except peak, also contain Zn phase diffraction maximum, after the completion of this illustrates sintering processes, lays down high pressure effect and cooled down, it is difficult to be obtained only
Containing single MgZn2The synthetic sample of phase.
Claims (1)
1. a kind of high pressure high temperature synthetic method for preparing second phase particles simulation material in aluminium alloy, it is characterised in that: described
Method includes the following steps:
(1) prefabricated biscuit measures ratio according to the chemical component of second phase particles in aluminium alloy, weighs the pure of enough contained elements
Metal powder is uniformly mixed on batch mixer；Added according to chamber size in the graphite bush used on diamond cubic hinge press
Work green compact mold, mixing is poured into green compact mold, and mixing is finally pressed into the powder biscuit of corresponding size on a hydraulic press；
(2) the powder biscuit suppressed in step (1) is pressed into graphite bush inner cavity by sintering processes, will be covered using graphite flake
Pipe sealing two ends are simultaneously assembled into Synthetic block, and then are mounted in diamond cubic hinge press working chamber, apply pressure 1-
After 5GPa, then electrified regulation to temperature is higher by described in step (1) 50-200 DEG C of fusing point of second phase particles normal pressure, and heat preservation sintering
10-60 minutes；
(3) cooling treatment, after the completion of sintering, in the case where keeping the effect of 1-5GPa high pressure, power-off is cooled to room temperature, and then release is taken out
The second phase particles simulation material is made in sample.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113637861A (en) * | 2021-08-13 | 2021-11-12 | 湘潭大学 | Zn-Se alloy and preparation method and application thereof |
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| EP1396470A2 (en) * | 2002-05-24 | 2004-03-10 | Dalsa Semiconductor Inc. | Fabrication of microstructures with vacuum-sealed cavity |
| CN101397647A (en) * | 2008-11-03 | 2009-04-01 | 清华大学 | Cu-In-Ga-Se or Cu-In-Al-Se solar cell absorption layer target material and preparation method thereof |
| CN103551573A (en) * | 2013-10-22 | 2014-02-05 | 中国科学院金属研究所 | Previous particle boundary precipitation preventable high-temperature alloy powder hot isostatic pressing process |
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| CN113637861A (en) * | 2021-08-13 | 2021-11-12 | 湘潭大学 | Zn-Se alloy and preparation method and application thereof |
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