CN111334694B - Method for modifying LPSO structure in magnesium alloy through primary nano disperse phase - Google Patents
Method for modifying LPSO structure in magnesium alloy through primary nano disperse phase Download PDFInfo
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 59
- 239000000843 powder Substances 0.000 claims abstract description 92
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 58
- 239000001301 oxygen Substances 0.000 claims abstract description 58
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 27
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- 239000002243 precursor Substances 0.000 claims abstract description 22
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 20
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- 238000011065 in-situ storage Methods 0.000 claims abstract description 10
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 10
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- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 5
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
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- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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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
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
-
- 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
- B22F3/02—Compacting only
-
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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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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- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
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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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention provides a method for modifying an LPSO structure in a magnesium alloy by a primary nano dispersed phase, which belongs to the technical field of non-ferrous metal alloy preparation and comprises the following steps: preparing an LPSO alloy ingot by a conventional magnesium alloy smelting method, and processing the LPSO alloy ingot into fine scraps to obtain LPSO pre-alloy powder; carrying out mechanical alloying oxygen doping treatment on the LPSO prealloying powder by an air oxidation method or a magnesium oxide decomposition method to obtain magnesium alloy precursor powder with oxygen solid solution; and then, sintering and forming the precursor powder after cold pressing to obtain the primary nano dispersed phase modified LPSO structural alloy. The invention introduces the oxide nanometer dispersed phase with ultra-high melting point in the LPSO structure in situ, and realizes the modification of the LPSO structure which can not be heat treated. And the prepared LPSO has small grain size and high thermal stability. The method has the advantages of simple process, low equipment environment requirement, excellent mechanical property of the prepared material and good application prospect.
Description
Technical Field
The invention relates to the technical field of non-ferrous metal alloy preparation, in particular to a method for modifying an LPSO structure in a magnesium alloy by using a primary nano dispersed phase.
Background
As the lightest metal structure material, the magnesium alloy has wide application prospect in the field of light weight. However, the defects of low absolute strength, poor heat resistance and the like of the traditional magnesium alloy seriously limit the popularization and the application of the magnesium alloy in various fields. If the service temperature of the conventional Mg-Al series alloy exceeds 120 ℃, the strength is sharply reduced, which is mainly because a large amount of Mg exists in the alloy17Al12A low melting precipitated phase. The rare earth magnesium alloy (Mg-RE series) is a typical representative of high-strength heat-resistant magnesium alloy in the existing magnesium alloy system. Rare earth elements are added into the existing magnesium alloy, and a precipitated phase rich in rare earth and high in melting point and thermal stability is formed through subsequent thermal mechanical treatment, so that the strength of the alloy is improved. The Mg-RE alloy can obtain high strength and even ultrahigh strength through solid solution strengthening, precipitation strengthening, composite strengthening and other ways. However, the heat resistance of the rare earth-rich refractory compound formed in the Mg-RE alloy is still low, the service temperature is generally not more than 200 ℃, otherwise most precipitated phases are subjected to rapid Ostwald ripening to coarsen and grow up, and the strengthening effect is lost. In recent years, it is important to discover that a novel long-period stacking ordered structure (LPSO structure for short) is formed after certain processing by further adding Zn element into the rare earth magnesium alloy. A large number of researches show that the LPSO structure has higher thermal stability and plays a great role in promoting the strengthening and toughening and heat resistance of the magnesium alloy.
However, as the research on the structure and performance of LPSO is further advanced, it is found that the LPSO type Mg-RE series alloy still has the following two main problems: on the one hand, the LPSO structure itself is still a metal type compound, the deformation of which is still a kink mechanism mainly based on basal plane dislocation slip motion and has strong anisotropy. In particular, LPSO oriented at 45 ° is liable to undergo basal plane slip, and the heat resistance is not satisfactory. Therefore, how to effectively inhibit basal plane dislocation movement in LPSO and further improve the heat resistance of LPSO itself is one of the keys to improving the overall heat resistance of LPSO type Mg-RE series alloy. According to the principle that the nano precipitated phase can hinder dislocation slip and further improve heat resistance, the nano precipitated phase can be introduced into the LPSO structure, so that the heat resistance of the LPSO structure is further improved, and the anisotropy is reduced. Unfortunately, the LPSO structure is thermodynamically stable and is a non-heat treatable microstructure, and there is no report of in-situ precipitated phases in LPSO at present. Chinese patent CN107058924A discloses a high-strength high-plasticity heat-resistant magnesium alloy for regulating LPSO structure and nano precipitated phase and a preparation method thereof, and ECAP processing is carried out on Mg-Y-Zn series alloy to obtain ultra-fine grain rare earth magnesium alloy, wherein the average grain size of a magnesium matrix is 0.6-1.3 mu m. Then, the LPSO structure in the alloy is regulated and controlled by means of a double heat treatment system, a nano precipitated phase is introduced, and the high-strength-toughness heat-resistant magnesium alloy is prepared by utilizing three mechanisms of fine grain strengthening, LPSO strengthening and nano precipitated phase strengthening. However, the nano precipitated phase is still precipitated in the magnesium alloy matrix, has no direct effect on the LPSO structure, and cannot modify and optimize the LPSO structure.
On the other hand, the LPSO structure in the general as-cast alloy is coarse, and the improvement space for the material performance is limited, and the preparation of magnesium alloy containing fine LPSO structure is becoming the focus of research more and more. But the fine LPSO structure has lower thermal stability, is easy to grow and coarsen in the high-temperature deformation and heat treatment processes, and loses the strengthening effect. Magnesium alloy containing LPSO structure is mainly prepared by extrusion, rolling and other methods, broken fine LPSO phase in the alloy is in fibrous distribution along the extrusion direction, except anisotropy, the short fiber-shaped LPSO structure is unstable, obvious fiber coarsening can occur when the short fiber-shaped LPSO structure is annealed for a long time at 300 ℃, the good interface matching relation with a matrix is lost, and the strengthening effect is greatly reduced [ Mater. Sci.Eng.A,2013,560,71-79 ]. At present, some researchers begin to prepare superfine LPSO structures by using methods such as rapid solidification powder metallurgy and severe plastic deformation, and certain research results are obtained. For example, Chinese patent CN108950331B discloses a method for preparing a magnesium alloy with fine LPSO structure and high toughness, which adopts Mg-RE-Zn (-Zr/Mn) alloy atomized powder as a raw material, and regulates the structure of the alloy by regulating and controlling parameters such as pressure, temperature, time, heating rate and the like of spark plasma sintering, wherein the prepared LPSO has the grain size of 5-8 μm and still larger size. S.M.Zhu et al [ Mater.Sci.Eng.A,2017,692, 35-42 ] utilize an Equal Channel Angular Pressing (ECAP) method to prepare an ultrafine LPSO structure, the minimum grain size of the ultrafine LPSO structure reaches 300nm, and the ultrafine LPSO structure is LPSO grains with the minimum size reported at present. However, such small-sized LPSO grains appear only at local recrystallization sites, and most of the grain sizes are still on the micrometer scale. In addition, the high temperature thermal stability of LPSO is left to be examined due to the lack of pinning of second phase particles within its structure and at grain boundaries.
Based on the above description, it is necessary to develop a method for modifying LPSO structure to solve the above problems.
Disclosure of Invention
According to the technical problems of unsatisfactory heat resistance, large size, easy coarsening in the heat treatment process and the like of the LPSO structure, the method for modifying the LPSO structure in the magnesium alloy by the primary nano dispersed phase is provided. The invention introduces a nanometer dispersed phase with ultra-high melting point in situ in the LPSO structure while preparing the superfine LPSO crystal grains, so that the modified LPSO structure has more excellent mechanical property and thermal stability. The invention realizes the modification of LPSO mainly by generating a nano dispersed phase through oxygen doping treatment, does not limit the oxygen content in the oxygen doping process of the LPSO pre-alloy powder, and can actually determine the oxygen doping amount according to the specific requirements on the material performance.
The technical means adopted by the invention are as follows:
a method for modifying LPSO structure in magnesium alloy by primary nanometer disperse phase is characterized in that LPSO with preset components is selected and smelted to prepare alloy ingots, and then the alloy ingots are processed into LPSO prealloy powder; carrying out mechanical alloying oxygen doping treatment on the LPSO prealloying powder to obtain magnesium alloy precursor powder with oxygen dissolved in solid solution; and cold press molding and sintering the magnesium alloy precursor powder dissolved with oxygen to obtain the primary nano dispersed phase modified LPSO structural alloy.
The method is specifically carried out according to the following steps:
(1) preparation of LPSO prealloyed powder: LPSO (molecular formula is Mg)85Zn6Y9) Is/are as followsThe chemical composition is Mg: 63.40 wt%; zn: 12.04 wt%; y: 24.56 wt.% of Mg85Zn6Y9(ii) a Preparing an LPSO alloy ingot by a conventional magnesium alloy smelting method, and processing the LPSO alloy ingot into fine scraps to obtain LPSO pre-alloy powder;
(2) mechanical alloying oxygen doping treatment: carrying out mechanical alloying oxygen doping treatment on the LPSO prealloy powder prepared in the step (1) by an air oxidation method or a magnesium oxide decomposition method to obtain magnesium alloy precursor powder with oxygen solid solution;
(3) sintering and forming: and (3) drying the magnesium alloy precursor powder dissolved with oxygen prepared in the step (2), performing cold press molding, and sintering and molding the cold-pressed blank to obtain the primary nano dispersed phase modified LPSO structural alloy.
Further, in the step (1), the fine scraps need to be processed on the LPSO alloy ingot through a turning or milling process under the protection of argon, and the size of the fine scraps is controlled to be 0.5-1 mm.
Further, in the step (2), the mechanical alloying oxygen-doping treatment of the LPSO prealloying powder by the air oxidation method comprises the following steps: cleaning and drying the prealloying powder, then filling the prealloying powder into a ball milling tank in the air, and carrying out mechanical alloying reaction under the condition of set mechanical alloying parameters. The mechanical alloying parameter conditions are as follows: the ball material ratio is 2: 1-5: 1, and the rotation speed is 500-; stopping the ball mill for 0.5h and scraping once, wherein the total ball milling time is 3-5 h, and the total time of stopping and scraping is not counted.
Furthermore, the cleaning refers to ultrasonic cleaning in alcohol, and the drying is performed in a vacuum/argon protective atmosphere. The cleaning of the prealloying powder is to wash away the pollution such as oil stain and the like introduced in the chip making process; the drying process is carried out under vacuum/argon atmosphere in order to avoid the introduction of uncontrolled oxygen when heating in air.
The shutdown scraping is to prevent the pre-alloyed powder from generating excessive cold welding in the mechanical alloying process. Because LPSO has better plasticity, cold welding and adhesion are easy to occur in the mechanical alloying process, the cold welding cannot be prevented by adding ball-milling aids such as alcohol, normal hexane and the like, and the machine is stopped and scraped within 0.5 h; on the other hand, the shutdown scraping supplements oxygen consumed in the mechanical alloying process.
Further, the above-mentioned shutdown scraping is performed in an air or argon environment, the number of times of scraping in the air is determined by the oxygen doping amount required by the material, the oxygen doping amount is actually determined according to the specific requirements on the material performance, and the rest of scraping processes are performed in the argon environment provided by the glove box.
After the material scraping in the air is finished, the ball milling tank is sealed, which is equivalent to supplementing oxygen consumed in the mechanical alloying process. The amount of oxygen replenished after each scraping in air was 21% of the volume of the milling jar (i.e., the volume fraction of oxygen in air), which allows quantitative control of the amount of oxygen incorporation to some extent.
Further, in the step (2), the process of performing mechanical alloying oxygen-doping treatment on the LPSO prealloy powder by a magnesium oxide decomposition method comprises the following steps: cleaning and drying the pre-alloyed powder, weighing MgO powder with a certain mass, putting the pre-alloyed powder and the MgO powder into a ball-milling tank in a protective atmosphere according to a certain proportion, sealing, and carrying out mechanical alloying reaction under the condition of set mechanical alloying parameters. The mechanical alloying parameter conditions are as follows: the ball material ratio is 5: 1-10: 1, and the rotation speed is 500-; stopping the ball mill for 0.5h and scraping once per ball mill, wherein the total ball milling time is 3-5 h, and the total time is not counted in the stopping and scraping time; the shutdown scraping process is carried out in an argon atmosphere provided by a glove box.
Further, the oxygen doping amount of the LPSO prealloy powder is determined by the certain proportion, and the oxygen doping amount determines the number density of the primary nano dispersed phase, so that the mechanical property and the thermal stability of the material are determined. Quantitative control of the oxygen incorporation amount can be achieved by controlling the proportion fraction of the MgO powder.
Further, in the step (3), the sintering molding adopts the processes of common hot pressing sintering, spark plasma sintering or hot isostatic pressing and the like, and the main purpose is to sinter the precursor powder into a compact block body, so that the LPSO structure and the nanometer yttrium oxide dispersed phase are dynamically precipitated in situ in the sintering process of the alloy. The sintering temperature is 350-450 ℃, the sintering pressure is 20-150 MPa, and the sintering time is 5-120 min.
By adopting different sintering forming methods, the precipitation kinetics of the LPSO structure and the nano yttrium oxide dispersed phase can be changed to a certain extent, but the thermodynamic formation mechanism of the LPSO structure and the nano yttrium oxide dispersed phase is not changed essentially.
The present invention mechanically alloys LPSO pre-alloyed powder by an air oxidation process or a magnesium oxide decomposition process to introduce oxygen into the material. Through huge energy input in the mechanical alloying process, oxygen in the air is forced to be dissolved in crystal lattices of the LPSO pre-alloyed powder through a solid-gas reaction mechanism or oxygen generated by decomposing magnesium oxide through a solid-solid reaction mechanism, and the magnesium alloy precursor powder with oxygen dissolved in a solid solution is prepared. And sintering and molding the precursor powder to precipitate a large amount of fine oxide nano disperse phase in situ in the LPSO structure to obtain the primary nano disperse phase modified LPSO structure.
The incorporation of oxygen changes the thermodynamic state of the material due to the higher affinity of yttrium and oxygen in the alloy. During the powder sintering process, when the LPSO structure is formed again, a part of yttrium element in the alloy can be combined with solid-solution oxygen element to generate a nano yttrium oxide dispersed phase, and the nano yttrium oxide dispersed phase is precipitated in situ in the LPSO and on a grain boundary. The nano dispersed phase precipitated in LPSO can effectively block basal plane dislocation glide, thereby further improving the heat resistance and reducing the anisotropy. Meanwhile, the growth of LPSO grains is inhibited by the action of kinetic pinning of the nano dispersed phase precipitated on the grain boundary, so that the modified LPSO structure keeps high thermal stability, and the grain size is stabilized at 200 nm.
Compared with the prior art, the invention has the following advantages:
1. the invention introduces nano disperse phase into LPSO structure to realize the modification of non-heat-treatable LPSO structure. The introduced nano dispersed phase is essentially oxide ceramic particles with ultrahigh melting point, does not grow up at high temperature and has excellent thermal stability; meanwhile, the steel plate has small size, dispersed distribution, high number density and obvious strengthening effect; in addition, a determined crystallographic relation exists between the nano dispersed phase introduced by an in-situ precipitation mode and the LPSO substrate, so that the nano dispersed phase has tight interface combination, and the problems of weak binding force and low strengthening and toughening effects between nano ceramic particles and the substrate added in the traditional powder metallurgy process are solved.
2. The high-energy ball milling process adopted by the invention effectively refines the grain size of LPSO, and then the dynamic pinning effect of the nano dispersed phase precipitated in situ is utilized to obviously inhibit the growth of LPSO grains, so that the modified LPSO structure keeps high thermal stability. The LPSO structure with the grain size of about 200nm prepared by the invention basically does not grow crystal grains and does not reduce the performance after being annealed for 100 hours at the high temperature of below 400 ℃.
3. The modified LPSO structure can be prepared by mechanical alloying and conventional powder sintering method. The preparation process is simple, the requirement on equipment environment is low, and the prepared material has excellent mechanical property and good application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a transmission electron micrograph of a native nanodispersed phase modified LPSO structure prepared in example 2 of the present invention.
Fig. 2 is an electron diffraction photograph of the native nanodispersed phase modified LPSO structure prepared in example 2 of the present invention.
Fig. 3 is a scanning transmission electron microscope dark field phase photograph of the native nanodispersed phase modified LPSO structure prepared in example 2 of the present invention.
Fig. 4 is a high resolution electron micrograph of the native nanodispersed phase modified LPSO structure prepared in example 2 of the present invention.
Fig. 5 is a transmission electron micrograph of the primary nanodispersed phase modified LPSO structure prepared in example 3 of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. Any specific values in all examples shown and discussed herein are to be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
The invention provides a method for modifying LPSO structure in magnesium alloy by primary nano disperse phase, which comprises the following steps of firstly, selecting a molecular formula of Mg85Zn6Y9The chemical composition of the LPSO is Mg: 63.40 wt%; zn: 12.04 wt%; y: 24.56 wt% of LPSO alloy ingot prepared by a conventional magnesium alloy smelting method, and then processing the LPSO alloy ingot into fine scraps to obtain LPSO pre-alloy powder, wherein the fine scraps need to be processed on the LPSO alloy ingot by a turning or milling process under the protection of argon, and the size of the fine scraps is controlled to be 0.5-1 mm.
Then, carrying out mechanical alloying oxygen doping treatment on the LPSO prealloying powder to obtain magnesium alloy precursor powder with oxygen dissolved in a solid solution, wherein the mechanical alloying oxygen doping treatment is to carry out mechanical alloying oxygen doping treatment on the prepared LPSO prealloying powder by an air oxidation method or a magnesium oxide decomposition method to obtain magnesium alloy precursor powder with oxygen dissolved in a solid solution;
the process for carrying out mechanical alloying oxygen doping treatment on the LPSO prealloying powder by an air oxidation method comprises the following steps: cleaning and drying the prealloying powder, then filling the prealloying powder into a ball milling tank in the air, and carrying out mechanical alloying reaction under the condition of set mechanical alloying parameters. The cleaning is ultrasonic cleaning in alcohol, and the drying is carried out under the protection of vacuum/argon gas. The set mechanical alloying reaction parameters are as follows: the ball material ratio is 2: 1-5: 1, and the rotation speed is 500-; stopping the ball mill for 0.5h and scraping once per ball mill, wherein the total ball milling time is 3-5 h, and the total time is not counted in the stopping and scraping time; the shutdown scraping is carried out in an air or argon environment, the scraping frequency in the air is determined by the oxygen doping amount required by the material, and the rest scraping process is carried out in a glove box.
The process for carrying out mechanical alloying oxygen-doping treatment on the LPSO prealloy powder by a magnesium oxide decomposition method comprises the following steps: cleaning and drying the pre-alloyed powder, weighing MgO powder with a certain mass, putting the pre-alloyed powder and the MgO powder into a ball-milling tank in a protective atmosphere according to a certain proportion, sealing, and carrying out mechanical alloying reaction under the condition of set mechanical alloying parameters. The set mechanical alloying reaction parameters are as follows: the ball material ratio is 5: 1-10: 1, and the rotation speed is 500-; stopping the ball mill for 0.5h and scraping once per ball mill, wherein the total ball milling time is 3-5 h, and the total time is not counted in the stopping and scraping time; the shutdown scraping process is carried out in an argon atmosphere provided by a glove box.
And finally, drying the prepared magnesium alloy precursor powder with oxygen dissolved in solid solution, performing cold press molding, and sintering and molding the cold-pressed blank to obtain the primary nano dispersed phase modified LPSO structural alloy, wherein the sintering and molding adopt common hot press sintering, spark plasma sintering or hot isostatic pressing processes, the sintering temperature is 350-450 ℃, the sintering pressure is 20-150 MPa, and the sintering time is 5-120 min.
Example 1
The method for preparing the LPSO structure in the primary nano dispersed phase modified magnesium alloy comprises the following steps:
(1) preparation of LPSO prealloyed powder: the LPSO alloy ingot is prepared by a conventional magnesium alloy smelting method, and the whole process is carried out in CO2And SF6The method is carried out in a mixed gas atmosphere and mainly comprises the following steps: the weight ratio of Mg: zn: y63.4: 12.0: 24.6, batching; preheating a smelting furnace to 400-500 ℃, adding a pure magnesium ingot into a crucible of the smelting furnace, and then heating to 700-750 ℃; adding Zn and Mg-Y intermediate alloy after the magnesium ingot is melted, then raising the temperature of the furnace by 10-30 ℃, preserving the temperature for 10-15 min, and then mechanically stirring for 2-5 min; and adjusting the temperature of the smelting furnace to 700-720 ℃, preserving the heat for 10-15 min, pouring into a mold, and cooling to obtain the LPSO ingot. And then machining the LPSO alloy ingot into fine scraps with the size of 0.5-1 mm by a turning process under the protection of argon gas to obtain LPSO prealloying powder.
(2) Mechanical alloying oxygen doping treatment: and carrying out mechanical alloying oxygen doping treatment on the prealloying powder by an air oxidation method. Ultrasonically cleaning the prealloy powder in alcohol for 10min, and then drying in a vacuum drying oven. The drying temperature is 150 ℃ and the time is 5 h. 5g of dried prealloyed powder is weighed, and the powder and 10g of grinding steel balls are put into a 50ml ball milling tank in the air and sealed for mechanical alloying. The parameters of mechanical alloying are that the ball-material ratio is 2:1, the rotating speed is 1000rpm, and the machine is stopped and scraped once every ball milling time is 0.5 h. The first stop is carried out and the scraping is carried out in the air, the ball milling tank is sealed after the scraping is finished, and the mechanical alloying is continuously carried out. And performing subsequent shutdown scraping operation in a glove box, wherein the total ball milling time is 3h, and the shutdown scraping time does not account for the total time, so as to obtain the oxygen-doped solid-solution magnesium alloy precursor powder with the oxygen content of 0.65 percent (mass fraction).
(3) Sintering and forming: and (3) drying the magnesium alloy precursor powder dissolved with oxygen prepared in the step (2) in a vacuum drying oven at the drying temperature of 100 ℃ for 2 hours. And (3) putting the dried powder into a die, and performing cold press molding at the molding pressure of 100 MPa. And then, performing SPS sintering molding on the cold-pressed blank at 350 ℃, 100MPa and 5min to obtain the primary nano dispersed phase modified LPSO structural alloy. The Vickers hardness value of the alloy at room temperature reaches 190HV, the compressive yield strength at room temperature is 785MPa, the compressive strain is 12 percent, and the compressive yield strength at 250 ℃ is 405 MPa.
Example 2
The method for preparing the LPSO structure in the primary nano dispersed phase modified magnesium alloy comprises the following steps:
(1) the first step of this example is the same as step (1) in example 1.
(2) Mechanical alloying oxygen doping treatment: and carrying out mechanical alloying oxygen doping treatment on the prealloying powder by an air oxidation method. Ultrasonically cleaning the prealloy powder in alcohol for 10min, and then drying in a vacuum drying oven. The drying temperature is 150 ℃ and the time is 5 h. 5g of dried prealloyed powder is weighed, and the powder and 10g of grinding steel balls are put into a 50ml ball milling tank in the air and sealed for mechanical alloying. The parameters of mechanical alloying are that the ball-material ratio is 2:1, the rotating speed is 1000rpm, and the machine is stopped and scraped once every ball milling time is 0.5 h. And stopping the machine for scraping in the air for the first three times, sealing the ball milling tank after the scraping is finished, and continuously performing mechanical alloying. And performing subsequent shutdown scraping operation in a glove box, wherein the total ball milling time is 3h, and the shutdown scraping time does not account for the total time, so as to obtain the oxygen-doped solid-solution magnesium alloy precursor powder with the oxygen content of 1.5 percent (mass fraction).
(3) Sintering and forming: and (3) drying the magnesium alloy precursor powder dissolved with oxygen prepared in the step (2) in a vacuum drying oven at the drying temperature of 100 ℃ for 2 hours. And (3) putting the dried powder into a die, and performing cold press molding at the molding pressure of 150 MPa. And then, performing SPS sintering molding on the cold-pressed blank at the sintering temperature of 400 ℃, the sintering pressure of 120MPa and the sintering time of 5min to obtain the primary nano dispersed phase modified LPSO structural alloy. The Vickers hardness value at room temperature of the alloy reaches 215HV, the compressive yield strength at room temperature is 855MPa, the compressive strain is 9 percent, and the compressive yield strength at 250 ℃ is 455 MPa. After the alloy is annealed for 100 hours at the high temperature of 400 ℃ for a long time, the LPSO crystal grains are not grown basically, and the Vickers hardness value at room temperature is still as high as 203 HV.
As shown in fig. 1, is a transmission electron micrograph of the primary nanodispersed phase modified LPSO structure prepared in example 2. It can be seen that the LPSO crystal grain size is fine, with an average crystal grain size of 200nm, in equiaxed morphology. The electron diffraction analysis of FIG. 2 shows that the structure type is 18R-LPSO, which is a sub-type of LPSO with good heat resistance. As can be seen from fig. 3, a large number of finely dispersed white particles are present both inside LPSO grains and on grain boundaries, and energy spectrum analysis indicates that these white particles are yttria nanophase. The particle size distribution is 3-20 nm, and the number density is 3.6 x 1022m-3. FIG. 4 shows that the fine nano-dispersed phase precipitated in situ inside the LPSO structure has a definite crystallographic relationship with the matrix. The primary nano phase is firmly combined with the matrix, and the generation of interface defects is avoided.
Example 3
The method for preparing the LPSO structure in the primary nano dispersed phase modified magnesium alloy comprises the following steps:
(1) the first step of this example is the same as step (1) in example 1.
(2) Mechanical alloying oxygen doping treatment: the prealloyed powder is subjected to mechanical alloying oxygen doping treatment by a magnesium oxide decomposition method. Ultrasonically cleaning the prealloy powder in alcohol for 10min, and then drying in a vacuum drying oven. The drying temperature is 150 ℃ and the time is 5 h. 5g of mixture powder was prepared in a proportion of 5% by mass of MgO. The alloy powder includes 4.75g of LPSO prealloying powder and 0.25g of MgO powder. The prepared mixture powder was put into a 50ml ball mill pot together with 10g of a milling steel ball in a glove box and sealed, and subjected to mechanical alloying. The mechanical alloying parameters are that the ball-material ratio is 5:1, the rotating speed is 1000rpm, the machine stops and scrapes materials once in a glove box after each ball milling for 0.5h, the total ball milling time is 5h, and the total time of the machine stops and scrapes materials is not counted. Obtaining the precursor powder of the magnesium alloy with oxygen doping amount of 2 percent (mass fraction) and oxygen solid solution.
(3) Sintering and forming: and (3) drying the magnesium alloy precursor powder dissolved with oxygen prepared in the step (2) in a vacuum drying oven at the drying temperature of 100 ℃ for 2 hours. And (3) putting the dried powder into a die, and performing cold press molding at the molding pressure of 250 MPa. And then carrying out common hot-pressing sintering molding on the cold-pressed blank, wherein the sintering temperature is 450 ℃, the sintering pressure is 150MPa, and the sintering time is 60min, so as to obtain the primary nano dispersed phase modified LPSO structural alloy. The Vickers hardness value of the alloy at room temperature reaches 235HV, the compressive yield strength at room temperature is 895MPa, the compressive strain is 7.5 percent, and the compressive yield strength at 250 ℃ is 485 MPa. After the alloy is annealed for 100 hours at the high temperature of 400 ℃ for a long time, the LPSO crystal grains are basically not grown, and the Vickers hardness value at room temperature is still as high as 213 HV.
As shown in fig. 5, is a transmission electron micrograph of the primary nanodispersed phase modified LPSO structure prepared in example 3. It can be seen that the LPSO has a fine grain size, an average grain size of 187nm, a large number of black nano dispersed phase particles in the grain and on the grain boundary, a particle size distribution of 3 to 22nm, and a number density of 5.2 x 1022m-3。
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for modifying LPSO structure in magnesium alloy by primary nanometer disperse phase is characterized in that LPSO with preset components is selected, and is processed into LPSO prealloy powder after an alloy ingot is prepared by smelting; carrying out mechanical alloying oxygen doping treatment on the LPSO prealloying powder to obtain magnesium alloy precursor powder with oxygen dissolved in solid solution; and (2) cold-press molding and sintering the magnesium alloy precursor powder dissolved with oxygen, and introducing a nanometer disperse phase with a super-high melting point into the LPSO structure in situ while preparing superfine LPSO grains to obtain the primary nanometer disperse phase modified LPSO structure alloy.
2. The method of claim 1, wherein the molecular formula of LPSO is Mg85Zn6Y9The chemical composition is Mg: 63.40 wt%; zn: 12.04 wt%; y: 24.56 wt%; the LPSO alloy ingot is prepared by a conventional magnesium alloy smelting method, and then the LPSO alloy ingot is processed into fine scraps to obtain LPSO pre-alloy powder.
3. The method for modifying LPSO structure in magnesium alloy according to claim 1, wherein the mechanical alloying oxygen-doping treatment is to perform oxygen-doping treatment on the prepared LPSO pre-alloyed powder by air oxidation or magnesium oxide decomposition to obtain magnesium alloy precursor powder with oxygen solid solution.
4. The method for preparing the LPSO structure in the primary nano disperse phase modified magnesium alloy according to claim 1, wherein the prepared magnesium alloy precursor powder with oxygen dissolved in solid solution is dried and then subjected to cold press molding, and then the cold press blank is subjected to sintering molding to obtain the primary nano disperse phase modified LPSO structure alloy, wherein the sintering molding adopts common hot press sintering, spark plasma sintering or hot isostatic pressing process, the sintering temperature is 350-450 ℃, the sintering pressure is 20-150 MPa, and the sintering time is 5-120 min.
5. The method for preparing LPSO structure in primary nano dispersed phase modified magnesium alloy according to claim 2, wherein the fine debris is processed into LPSO alloy ingot by turning or milling process under argon protection, and the size of the fine debris is controlled to be 0.5-1 mm.
6. The method for modifying LPSO structure in magnesium alloy according to claim 3, wherein the mechanical alloying oxygen-doped process of LPSO pre-alloy powder by air oxidation comprises the following steps: cleaning and drying the prealloying powder, then filling the prealloying powder into a ball milling tank in the air, and carrying out mechanical alloying reaction under the condition of set mechanical alloying parameters.
7. The method for modifying LPSO structure in magnesium alloy according to claim 6, wherein the cleaning is ultrasonic cleaning in alcohol, and the drying is performed under vacuum/argon protection.
8. The method of LPSO structure in primary nanodispersed modified magnesium alloy as claimed in claim 6, wherein the mechanical alloying parameters are as follows: the ball material ratio is 2: 1-5: 1, and the rotation speed is 500-; stopping the ball mill for 0.5h and scraping once per ball mill, wherein the total ball milling time is 3-5 h, and the total time is not counted in the stopping and scraping time; the shutdown scraping is carried out in an air or argon environment, the scraping frequency in the air is determined by the oxygen doping amount required by the material, and the rest scraping process is carried out in a glove box.
9. The method for modifying LPSO structure in magnesium alloy according to claim 3, wherein the mechanical alloying oxygen-doped treatment of LPSO pre-alloy powder by magnesium oxide decomposition method comprises: cleaning and drying the pre-alloyed powder, weighing 0.25g of MgO powder, preparing 5g of mixture powder according to the proportion that the MgO accounts for 5 percent by mass, putting the pre-alloyed powder and the MgO powder into a ball-milling tank in protective atmosphere and sealing, wherein 4.75g of the pre-alloyed powder is subjected to mechanical alloying reaction under the condition of set mechanical alloying parameters.
10. The method of LPSO structure in primary nanodispersed phase modified magnesium alloy as claimed in claim 9, wherein the mechanical alloying parameters are as follows: the ball material ratio is 5: 1-10: 1, and the rotation speed is 500-; stopping the ball mill for 0.5h and scraping once per ball mill, wherein the total ball milling time is 3-5 h, and the total time is not counted in the stopping and scraping time; the shutdown scraping process is carried out in an argon atmosphere provided by a glove box.
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