CN112301261A - Preparation method of ultrafine crystal or nanocrystalline magnesium-zinc alloy - Google Patents
Preparation method of ultrafine crystal or nanocrystalline magnesium-zinc alloy Download PDFInfo
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- CN112301261A CN112301261A CN202011048074.4A CN202011048074A CN112301261A CN 112301261 A CN112301261 A CN 112301261A CN 202011048074 A CN202011048074 A CN 202011048074A CN 112301261 A CN112301261 A CN 112301261A
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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
- C22C23/04—Alloys based on magnesium with zinc or cadmium 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
- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2200/00—Crystalline structure
- C22C2200/04—Nanocrystalline
Abstract
The invention provides a preparation method of ultrafine crystal or nano crystal magnesium-zinc alloy, which comprises the following steps: preparing a magnesium-zinc alloy casting blank, wherein the magnesium-zinc alloy casting blank comprises the following elements in percentage by weight: 1.5 to 2.5 percent of Zn, and the balance of Mg; and carrying out solution treatment on the magnesium-zinc alloy casting blank, rolling the magnesium-zinc alloy casting blank subjected to solution treatment, and rolling to obtain the magnesium-zinc alloy with ultrafine grain or nanocrystalline grain size. The invention can effectively refine the crystal grains of the magnesium-zinc alloy to a nanometer size, so that the alloy has high strength and good corrosion resistance.
Description
Technical Field
The invention relates to the field of magnesium alloy material processing, in particular to a preparation method of ultrafine grain or nanocrystalline magnesium-zinc alloy.
Background
Magnesium and magnesium alloy have low density, high specific strength, easy recovery and utilization, and are known as green engineering materials in 21 st century. In addition, magnesium can be spontaneously corroded and degraded in the human body environment, has excellent biocompatibility, and is the most representative biomedical degradable metal material at present. In both industrial applications and biomedical applications, it has been sought to improve the strength of magnesium alloys, reduce the types of alloying elements (particularly, rare earth elements), and reduce the alloy cost. In addition, for the biomedical magnesium alloy, the addition of harmful elements such as Al, rare earth and the like is avoided as much as possible; reducing the generation of precipitated phases in the alloy to avoid accelerating the corrosion degradation rate. Due to the reasons, the grain size of the magnesium alloy is refined, the strength of the alloy can be obviously improved, the corrosion resistance is improved, the biocompatibility and the safety are not influenced, and the dependence on alloy elements is reduced.
The Chinese patent with the application number of 201610913369.0 discloses a preparation method of an anisotropic biomedical directional solidification magnesium-zinc alloy material, which combines a directional solidification technology and an orientation analysis technology to realize the preparation of the biomedical magnesium-zinc alloy material meeting the anisotropic requirement; firstly, preparing pure magnesium and pure zinc according to component requirements, smelting magnesium-zinc alloy in a resistance furnace, directly casting the mixture into a bar or preparing the bar by cutting the bar from a cast ingot, then preparing the magnesium alloy with growth orientation, obvious mechanical property and corrosion performance anisotropy on directional solidification equipment, and then performing magnesium alloy cutting processing with different orientations according to the performance required by the biomedical material; wherein the smelting temperature is 720-750 ℃, the directional solidification heating temperature is 720-820 ℃, and the directional solidification temperature gradient is 5-15 ℃/mm; the drawing speed of the directional solidification is 20 to 200 μm/s. The alloy aims at biomedical use, the Zn content is 1-5 wt.%, and the microstructure is a directional solidification structure. However, the above patents have the following disadvantages: the grain size is difficult to reach the submicron level, and especially a nanocrystalline structure cannot be prepared to obtain high strength and excellent degradation performance.
At present, no relevant report is provided for preparing the nanocrystalline magnesium alloy by the conventional processing technology. For the preparation of the superfine crystal magnesium alloy, on one hand, the preparation processes such as equal channel angular extrusion, high-pressure torsion and the like are complex, and the size of the material is greatly limited. On the other hand, most of the alloys are rare earth alloys having complicated compositions. Therefore, from both industrial application and biomedical field, it is urgently needed to prepare ultra-fine crystal and even nanocrystalline magnesium alloy in less processing passes and in non-rare earth magnesium alloy with simple components by only using a conventional processing technology, so as to obtain excellent mechanical property, degradation property and biocompatibility.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of ultrafine grain or nano-grain magnesium-zinc alloy.
The first aspect of the invention provides a preparation method of an ultrafine grain or nano-grain magnesium-zinc alloy, which comprises the following steps:
preparing a magnesium-zinc alloy casting blank, wherein the magnesium-zinc alloy casting blank comprises the following elements in percentage by weight: 1.5 to 2.5 percent of Zn, and the balance of Mg;
rolling the magnesium-zinc alloy casting blank, wherein 2-3 passes of rolling are carried out at the set temperature of 300-400 ℃, the rolling speed is 10-14 m/min, the time for returning and preserving heat between each pass of rolling is 1-10min, the rolling reduction of each pass is 40-80%, and the accumulated rolling deformation is more than 85%;
rolling to form the magnesium-zinc alloy with ultra-fine grain or nano-grain structure.
Preferably, the magnesium-zinc alloy casting blank comprises the following elements in percentage by weight: 1.9 to 2.1 percent of Zn and the balance of Mg.
More preferably, the time of returning and holding the furnace between each pass of rolling is 5min-10 min.
Preferably, the magnesium-zinc alloy casting blank is rolled, wherein when 3 times of rolling are carried out, the rolling reduction of the 3 rd time of rolling is greater than that of the previous 2 times of rolling.
Preferably, the magnesium-zinc alloy casting blank is rolled, wherein when the set temperature is 300-350 ℃, 3-pass rolling is performed, wherein the deformation of the first 2 passes is more than 40%, and the deformation of the 3 rd pass is more than 50%; the time of returning and holding the furnace is 1-10min between each pass of rolling.
Preferably, the magnesium-zinc alloy casting blank is rolled, wherein when the set temperature is 350-400 ℃, 3-pass rolling is performed, wherein the deformation of the first 2-pass rolling is more than 50%, the deformation of the 3 rd-pass rolling is more than 60%, and the time for holding the temperature in the furnace returning process between every two-pass rolling is 1-10 min.
Preferably, before the rolling of the magnesium-zinc alloy casting blank, the method further comprises the step of performing solution treatment on the magnesium-zinc alloy casting blank. So that the magnesium-zinc alloy casting blank has more uniform texture.
Preferably, the magnesium-zinc alloy casting blank is subjected to solution treatment, wherein the temperature of the solution treatment is 300-400 ℃, and the heat preservation time is 0-12 h.
Preferably, the magnesium-zinc alloy casting blank is subjected to solution treatment, wherein the size parameters of the magnesium-zinc alloy casting blank are as follows: the length is 40mm-100mm, the width is 40mm-100mm, and the thickness is more than 20 mm.
More preferably, the magnesium-zinc alloy casting blank size parameters are as follows: 50mm long, 50mm wide and 25mm thick.
Preferably, the ultra-fine grain size is 100nm to 1000 nm.
Preferably, the nanocrystal size is 50nm to 100 nm.
The invention provides an ultrafine crystal or nano crystal magnesium-zinc alloy, which is prepared by the preparation method of the ultrafine crystal or nano crystal magnesium-zinc alloy.
The invention is different from the prior art in core improvement and principle: the invention controls the first-pass rolling parameters to ensure that the magnesium-zinc alloy material has full twin recrystallization behavior, preliminarily refines crystal grains and forms specific crystal orientation (the (0001) plane of the crystal grains is approximately parallel to the surface of the plate). By controlling the last pass rolling parameters, the magnesium-zinc alloy crystal grains after the preliminary refinement have very large Schmidt factors on a conical surface < c + a > slippage system, the conical surface < c + a > slippage is activated at the rolling temperature of 300-400 ℃, a large amount of recrystallization nucleation is formed, the crystal grains are inhibited from growing up through segregation of solute atoms Zn around the nanocrystalline grain boundary, and finally ultra-fine crystal or nanocrystalline tissues are formed.
Compared with the prior art, the invention has at least one of the following beneficial effects:
according to the method, the magnesium-zinc alloy casting blank alloy comprises magnesium and zinc, and the alloy does not contain noble elements such as rare earth and elements harmful to human bodies such as Al; magnesium element and zinc element are all nutrient elements and have excellent biocompatibility and safety; the method can prepare the magnesium-zinc alloy block plate containing the ultrafine crystal or nanocrystalline structure only by controlling the rolling process parameters, greatly simplifies the process steps compared with the traditional process, can be realized on the existing rolling mill equipment, and is convenient for batch production.
The product prepared by the method has high strength due to fine crystal grains, has better corrosion resistance due to no precipitated phase, and has excellent biocompatibility and safety due to the fact that alloy components are designed to be full nutrient elements. Has good biomedical and industrial application prospect.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a flow chart of the operation steps of a method for preparing an ultra-fine grain or nano-grain magnesium-zinc alloy according to a preferred embodiment of the present invention;
FIG. 2 is a transmission electron microscope image of a nanocrystalline Mg-Zn alloy prepared in example 1 of the present invention;
FIG. 3 is a transmission electron microscope image of an ultra-fine grained magnesium-zinc alloy prepared in example 2 of the present invention;
FIG. 4 is a transmission electron microscope image of a nanocrystalline Mg-Zn alloy prepared in example 3 of the present invention;
FIG. 5 is a transmission electron microscope image of an ultra-fine grained magnesium-zinc alloy prepared in example 4 of the present invention;
FIG. 6 is a transmission electron microscope image of an ultra-fine grained magnesium-zinc alloy prepared in example 5 of the present invention;
FIG. 7 is a transmission electron microscope image of an ultra-fine grained magnesium-zinc alloy prepared in example 6 of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment provides a preparation method of an ultrafine grain or nanocrystalline magnesium-zinc alloy, which is shown in fig. 1 and includes the following steps:
preparing a magnesium-zinc alloy casting blank containing 2 weight percent of Zn and the balance of Mg, wherein the size of the casting blank is 50 (length) multiplied by 50 (width) multiplied by 22 (thickness).
The magnesium-zinc alloy casting blank is rolled for 3 times at the set temperature of 400 ℃, the rolling speed is 14m/min, the time of returning to the furnace and keeping the temperature between each time of rolling is 2min, the rolling reduction of the 1 st and 2 nd times of rolling is 50%, the rolling reduction of the third time of rolling is 65%, and the cumulative rolling deformation is 91%.
Rolling to obtain the nanocrystalline magnesium-zinc alloy.
Referring to fig. 2, as can be seen from a transmission electron microscope image of the magnesium-zinc alloy prepared above, a nanocrystalline magnesium-zinc alloy with a grain size of about 70nm-80nm can be obtained by the preparation method; the nano-crystalline magnesium-zinc alloy is obtained by mechanical test, and has the yield strength of 210MPa and the tensile strength of 240 MPa; the average corrosion rate of the nanocrystalline magnesium-zinc alloy measured by soaking the nanocrystalline magnesium-zinc alloy in simulated body fluid (m-SBF) for one week is 1mg/cm2Day; biological experiments show that the cytotoxicity of the nanocrystalline magnesium-zinc alloy is 0 grade, and the average degradation rate of the nanocrystalline magnesium-zinc alloy in a new Zealand white rat subcutaneously implanted for three months is 0.2 mm/year.
Example 2
The embodiment provides a preparation method of an ultrafine crystal or nano crystal magnesium-zinc alloy, which comprises the following steps:
preparing a magnesium-zinc alloy casting blank containing 2.1 weight percent of Zn and the balance of Mg, wherein the size of the casting blank is 60 (length) multiplied by 50 (width) multiplied by 25 (thickness).
Carrying out solution treatment on the magnesium-zinc alloy casting blank at 300 ℃ for 4 h.
And (3) carrying out 3-pass rolling on the magnesium-zinc alloy casting blank subjected to the solution treatment at the set temperature of 300 ℃, wherein the rolling speed is 12m/min, the time for holding the furnace back between each pass of rolling is 8min, the rolling reduction of each pass is 55%, and the cumulative rolling deformation is 90%.
Rolling to obtain the superfine crystal magnesium-zinc alloy.
Referring to fig. 3, it can be seen from the transmission electron microscope image of the prepared magnesium-zinc alloy that the ultrafine crystal magnesium-zinc alloy with the grain size of about 200nm-300nm can be obtained by the preparation method; the yield strength of the superfine crystal magnesium-zinc alloy is 250MPa, and the tensile strength is 270 MPa; the average corrosion rate of the ultra-fine crystal magnesium-zinc alloy measured by soaking the ultra-fine crystal magnesium-zinc alloy in simulated body fluid (m-SBF) for one week is 1.2mg/cm2Day; biological experiments show that the cytotoxicity of the ultra-fine crystal magnesium-zinc alloy is 0 grade, and the average degradation rate is 0.25 mm/year within three months after the ultra-fine crystal magnesium-zinc alloy is subcutaneously implanted into New Zealand white rats.
Example 3
The embodiment provides a preparation method of an ultrafine crystal or nano crystal magnesium-zinc alloy, which comprises the following steps:
preparing a magnesium-zinc alloy casting blank containing 2.2 weight percent of Zn and the balance of Mg, wherein the size of the casting blank is 60 (length) multiplied by 40 (width) multiplied by 25 (thickness).
Carrying out solution treatment on the magnesium-zinc alloy casting blank at 350 ℃ for 2 h.
And (3) carrying out 3-pass rolling on the magnesium-zinc alloy casting blank subjected to the solution treatment at the set temperature of 350 ℃, wherein the rolling speed is 10m/min, the time for holding the furnace back between each pass of rolling is 5min, the rolling reduction of each pass of rolling is 60%, and the cumulative rolling deformation is 93%.
Rolling to obtain the nanocrystalline magnesium-zinc alloy.
Referring to fig. 4, as can be seen from a transmission electron microscope image of the magnesium-zinc alloy prepared above, a nanocrystalline magnesium-zinc alloy with a grain size of about 20nm to 30nm can be obtained by the preparation method; the yield strength of the superfine crystal magnesium-zinc alloy is 240MPa, and the tensile strength is 273 MPa; the average corrosion rate of the nanocrystalline magnesium-zinc alloy measured by soaking the nanocrystalline magnesium-zinc alloy in simulated body fluid (m-SBF) for one week is 1.1mg/cm2Day; biological experiments show that the cytotoxicity of the nanocrystalline magnesium-zinc alloy is 0 grade.
Example 4
The embodiment provides a preparation method of an ultrafine crystal or nano crystal magnesium-zinc alloy, which comprises the following steps:
preparing a magnesium-zinc alloy casting blank containing 1.9 wt% of Zn and the balance of Mg, wherein the size of the casting blank is 100 (length) multiplied by 60 (width) multiplied by 25 (thickness).
Carrying out solution treatment on the magnesium-zinc alloy casting blank for 2h at 400 ℃.
And (3) carrying out 2-pass rolling on the magnesium-zinc alloy casting blank subjected to the solution treatment at the set temperature of 400 ℃, wherein the rolling speed is 14m/min, the time for holding the temperature of the furnace back between each pass of rolling is 2min, the rolling reduction of each pass of rolling is 70%, and the cumulative rolling deformation is 91%.
Rolling to obtain the superfine crystal magnesium-zinc alloy.
Referring to FIG. 5, it can be seen from a transmission electron microscope image of the prepared magnesium-zinc alloy that an ultra-fine crystal magnesium-zinc alloy with a grain size of about 200nm to 300nm can be obtained by the above preparation method; the yield strength of the superfine crystal magnesium-zinc alloy is 200MPa, and the tensile strength is 240 MPa; the average corrosion rate of the ultra-fine crystal magnesium-zinc alloy measured by soaking the ultra-fine crystal magnesium-zinc alloy in simulated body fluid (m-SBF) for one week is 1.3mg/cm2Day; biological experiments show that the cytotoxicity of the ultra-fine crystal magnesium-zinc alloy is 0 grade.
Example 5
The embodiment provides a preparation method of an ultrafine crystal or nano crystal magnesium-zinc alloy, which comprises the following steps:
preparing a magnesium-zinc alloy casting blank containing 1.5 weight percent of Zn and the balance of Mg, wherein the size of the casting blank is 100 (length) multiplied by 60 (width) multiplied by 20 (thickness).
The magnesium-zinc alloy casting blank is rolled for 2 times at the set temperature of 400 ℃, the rolling speed is 14m/min, the time of furnace returning and heat preservation between each rolling is 5min, the rolling reduction of each rolling is 62%, and the cumulative rolling deformation is 85%.
Rolling to obtain the superfine crystal magnesium-zinc alloy.
Referring to fig. 6, as can be seen from a transmission electron microscope image of the prepared magnesium-zinc alloy, an ultra-fine crystal magnesium-zinc alloy with a grain size of about 700nm to 900nm can be obtained by the preparation method; the yield strength of the ultra-fine crystal magnesium-zinc alloy is 170MPa, and the tensile strength is 230 MPa; immersing ultra-fine crystal magnesium-zinc alloy by simulated body fluid (m-SBF)The average corrosion rate measured in one week of soaking was 1.4mg/cm2Day; biological experiments show that the cytotoxicity of the ultra-fine crystal magnesium-zinc alloy is 0 grade.
Example 6
The embodiment provides a preparation method of an ultrafine crystal or nano crystal magnesium-zinc alloy, which comprises the following steps:
preparing a magnesium-zinc alloy casting blank containing 2.5 weight percent of Zn and the balance of Mg. The size of the cast slab is 40 (length) × 40 (width) × 20 (thickness) mm.
Carrying out solution treatment on the magnesium-zinc alloy casting blank for 4h at 320 ℃.
And (3) carrying out 3-pass rolling on the magnesium-zinc alloy casting blank subjected to the solution treatment at the set temperature of 320 ℃, wherein the rolling speed is 10m/min, the time for holding the furnace back between each pass of rolling is 10min, the rolling reduction of each pass of rolling is 60%, and the cumulative rolling deformation is 93%.
Rolling to obtain the superfine crystal magnesium-zinc alloy.
Referring to FIG. 7, it can be seen from a transmission electron microscope image of the prepared magnesium-zinc alloy that an ultra-fine crystal magnesium-zinc alloy with a grain size of about 200nm to 300nm can be obtained by the above preparation method; the yield strength of the ultra-fine crystal magnesium-zinc alloy is 180MPa, and the tensile strength is 237 MPa; the average corrosion rate of the ultra-fine crystal magnesium-zinc alloy measured by soaking the ultra-fine crystal magnesium-zinc alloy in simulated body fluid (m-SBF) for one week is 1.4mg/cm2Day; biological experiments show that the cytotoxicity of the ultra-fine crystal magnesium-zinc alloy is 0 grade.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. A preparation method of ultra-fine grain or nano-grain magnesium-zinc alloy is characterized by comprising the following steps:
preparing a magnesium-zinc alloy casting blank, wherein the magnesium-zinc alloy casting blank comprises the following elements in percentage by weight: 1.5 to 2.5 percent of Zn, and the balance of Mg;
rolling the magnesium-zinc alloy casting blank, wherein 2-3 passes of rolling are carried out at the set temperature of 300-400 ℃, the rolling speed is 10-14 m/min, the time for returning and preserving heat between each pass of rolling is 1-10min, the rolling reduction of each pass is 40-80%, and the accumulated rolling deformation is more than 85%;
rolling to form the magnesium-zinc alloy with ultra-fine grain or nano-grain structure.
2. The method for preparing ultra-fine grain or nano-grain magnesium-zinc alloy according to claim 1, wherein the magnesium-zinc alloy casting blank comprises the following elements in percentage by weight: 1.9 to 2.1 percent of Zn and the balance of Mg.
3. The method of claim 1, wherein the ultra-fine grain or nano-grain magnesium-zinc alloy is prepared by the method,
and rolling the magnesium-zinc alloy casting blank, wherein when 3 times of rolling are carried out, the rolling reduction of the 3 rd time of rolling is greater than that of the previous 2 times of rolling.
4. The method of claim 1, wherein the ultra-fine grain or nano-grain magnesium-zinc alloy is prepared by the method,
rolling the magnesium-zinc alloy casting blank, wherein when the set temperature is 300-350 ℃, 3-pass rolling is carried out, wherein the deformation of the first 2 passes is more than 40%, and the deformation of the 3 rd pass is more than 50%; the time of returning and holding the furnace is 1-10min between each pass of rolling.
5. The method of claim 1, wherein the ultra-fine grain or nano-grain magnesium-zinc alloy is prepared by the method,
rolling the magnesium-zinc alloy casting blank, wherein when the set temperature is 350-400 ℃, 3-pass rolling is carried out, wherein the deformation of the first 2 passes is more than 50%, and the deformation of the 3 rd pass is more than 60%; the time of returning and holding the furnace is 1-10min between each pass of rolling.
6. The method of claim 1, further comprising subjecting the billet to solution treatment before rolling the billet.
7. The method for preparing ultra-fine grain or nano grain magnesium-zinc alloy as claimed in claim 6, wherein the magnesium-zinc alloy ingot blank is subjected to solution treatment at the temperature of 300-400 ℃ for 0-12 h.
8. The method for preparing an ultra-fine grained or nano-grained magnesium-zinc alloy according to any one of claims 1 to 7, characterized in that: the size of the superfine crystal is 100nm-1000 nm.
9. The method for preparing an ultra-fine grained or nano-grained magnesium-zinc alloy according to any one of claims 1 to 7, characterized in that: the size of the nano crystal is 50nm-100 nm.
10. An ultra-fine grain or nano-grain magnesium-zinc alloy, which is characterized in that: prepared by the process of any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114602993A (en) * | 2022-03-14 | 2022-06-10 | 常熟致圆微管技术有限公司 | Preparation method of biodegradable medical metal magnesium and magnesium alloy foil |
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| CN106995908A (en) * | 2016-01-22 | 2017-08-01 | 中国科学院金属研究所 | A kind of efficient rolling method of weak non-textured magnesium alloy plate |
| CN109504884A (en) * | 2019-01-10 | 2019-03-22 | 吉林大学 | Polynary a small amount of high-strength plasticity magnesium alloy and its heavy reduction short flow process |
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