CN110184518B - Rapidly-dissolved high-strength high-elongation magnesium alloy and preparation method thereof - Google Patents

Rapidly-dissolved high-strength high-elongation magnesium alloy and preparation method thereof Download PDF

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CN110184518B
CN110184518B CN201910335132.2A CN201910335132A CN110184518B CN 110184518 B CN110184518 B CN 110184518B CN 201910335132 A CN201910335132 A CN 201910335132A CN 110184518 B CN110184518 B CN 110184518B
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alloy
strength
magnesium alloy
elongation
pure
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CN110184518A (en
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胡毅
唐廷基
骆晓楠
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Beijing Yilian Technology Development Co ltd
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Beijing Yilian Technology Development Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/02Making alloys by melting
    • C22C1/03Making alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/06Alloys based on magnesium with a rare earth metal as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • EFIXED CONSTRUCTIONS
    • E21EARTH DRILLING; MINING
    • E21BEARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B33/00Sealing or packing boreholes or wells
    • E21B33/10Sealing or packing boreholes or wells in the borehole
    • E21B33/13Methods or devices for cementing, for plugging holes, crevices, or the like
    • E21B33/134Bridging plugs
    • EFIXED CONSTRUCTIONS
    • E21EARTH DRILLING; MINING
    • E21BEARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B43/00Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
    • E21B43/25Methods for stimulating production
    • E21B43/26Methods for stimulating production by forming crevices or fractures

Abstract

The invention provides a fast-dissolving high-strength high-elongation magnesium alloy and a preparation method thereof, wherein the fast-dissolving high-strength high-elongation magnesium alloy consists of the following elements in percentage by mass: 1.0-22.0% of Gd, 0.001-5.0% of Y, 0.001-10% of Al, 0.001-5.0% of Zn, 0.01-1.0% of Zr, 0.0001-1.0% of Sc, 0.01-10.0% of Cu, 0.01-3.0% of Li, 0.01-3.0% of Ni, 0.01-3.0% of Ga, 0.01-3.0% of In and the balance of Mg and impurity elements, wherein the total amount of Li, Ni, Ga and In is 0.1-6.0%. The rapidly-dissolved high-strength high-elongation magnesium alloy can be rapidly reacted with a water-soluble medium for dissolution, has the mechanical strength properties of high strength and high elongation, and can meet the application requirements of various industrial fields.

Description

Rapidly-dissolved high-strength high-elongation magnesium alloy and preparation method thereof
Technical Field
The invention belongs to the technical field of metal material processing, and particularly relates to a fast-dissolving high-strength high-elongation magnesium alloy and a preparation method thereof.
Background
In some special construction fields, such as oil and natural gas exploitation processes, a large number of underground exploitation tools, such as fracturing balls and bridge plugs, need to be used, the tools need to have mechanical properties meeting application functions of the tools, secondly, in order to improve the speed of engineering progress, the tools need to be rapidly dissolved after failure, recycling is not needed, and meanwhile, resource waste during tool recycling can be avoided.
The magnesium alloy is an alloy formed by adding other elements into magnesium as a base, and is characterized by small density, high specific strength, good heat dissipation, good shock absorption, easy machining, good organic matter and alkali corrosion resistance, active chemical properties in the existing metal materials, and the most common alloy material in the industrial field requiring structural materials and having degradation capability. Although the magnesium alloy has active chemical properties, the reaction speed of magnesium and water, water-oil mixture and other water-soluble media is very weak at normal temperature, and the reason is that magnesium hydroxide generated by the reaction prevents further reaction, and the reaction speed is not obviously improved even if the water-soluble media is heated to boil. In a certain temperature range, the reaction rate of the conventional magnesium alloy and a medium is low, and the conventional magnesium alloy is insensitive to temperature change, so that the requirement of industrial application cannot be met. In order to improve the dissolution rate of the magnesium alloy, some elements are usually added into the alloy to reduce the continuity of the magnesium hydroxide product and improve the reaction rate, however, the addition of the alloy elements can cause solid solution strengthening and second phase dispersion strengthening of the alloy, the increase of the second phase can also cause the reduction of the elongation of the alloy to different degrees, the mechanical strength performance of the alloy material is sacrificed, and the reliability of the alloy material applied to related fields is poor.
Disclosure of Invention
The invention aims to provide a fast-dissolving high-strength high-elongation magnesium alloy and a preparation method thereof, wherein the alloy can be fast dissolved by reacting with an aqueous medium, and has the mechanical strength properties of high strength and high elongation.
In order to solve the problems, the invention provides a fast-dissolving high-strength high-elongation magnesium alloy, which consists of the following elements in percentage by mass: 1.0-22.0% of Gd, 0.001-5.0% of Y, 0.001-10% of Al, 0.001-5.0% of Zn0.01-1.0% of Zr, 0.0001-1.0% of Sc, 0.01-10.0% of Cu, 0.01-3.0% of Li, 0.01-3.0% of Ni, 0.01-3.0% of Ga, 0.01-3.0% of In and the balance of Mg and impurity elements, wherein the total amount of Li, Ni, Ga and In is 0.1-6.0%.
Wherein, the impurity element refers to an inevitable impurity element introduced from a raw material for preparing the alloy during the process of preparing the alloy, i.e., a metal or a non-metal element which is present in the metal but is not intentionally added or retained, and preferably, the mass percentage of the inevitable impurity element is 0% to 0.15%.
Cu, Li, Ni, Ga and In are mixed reaction promoting elements, the elements and magnesium form new crystal phases In the smelting process, and the crystal phases can destroy the continuity of generated magnesium hydroxide In the reaction process of magnesium and a water-soluble medium, so that the obstruction of magnesium hydroxide on the contact of magnesium and the water-soluble medium is reduced, the reaction of magnesium and water and other media is promoted, and the reaction rate of magnesium and the water-soluble medium is improved; in addition, Cu, Li, Ni, Ga and In are matched with each other, and are added according to the proportion, so that the intragranular segregation of the magnesium alloy can be eliminated to the maximum extent, crystal grains are refined, and the elongation is improved; cu, Li, Ni, Ga and In can promote the precipitation strengthening of Gd and Zn elements In the subsequent heat treatment process, and further improve the strength of the alloy.
Wherein Gd and Y can form solid solution with Mg in the smelting process, the strength of the obtained alloy can be obviously improved through the solid solution or aging strengthening effect, the solid solubility of Gd, Y and Mg is high, Gd can be dissolved into the magnesium alloy at higher solid solubility, and the solid solubility is obviously reduced along with the reduction of temperature, so that the strength and other properties of the alloy can be greatly improved through solid solution strengthening or aging strengthening. Y acts similarly to Gd. Meanwhile, a small amount of Y can be added to refine crystal grains and improve the mechanical property of the alloy. Because the maximum solid solubility of Gd and Y in the magnesium alloy is 23.5 percent and 12.6 percent respectively, the Gd and the Y are added in proper amount to ensure that the Gd and the Y and Mg can respectively form solid solutions with single lattice structures, thereby achieving the high strength and the high elongation of the magnesium alloy. Gd. Y can also improve the stability of the melt in the smelting process, improve the stability of an oxide film and reduce the burning loss of other elements.
Zr and Sc elements can obviously refine cast ingot grains of the material, and the refined grains can improve the strength and the plasticity of the magnesium alloy formed part according to the Hall Peltier formula; in addition, the refinement of the cast ingot crystal grains can also promote the dispersion uniformity of mixed reaction promoting elements of Li, Ni, Ga and In the alloy, further improve the reaction rate of magnesium and a water-soluble medium, and also promote the dispersion uniformity of Gd and Y In the alloy, so that the elements Gd and Y In the alloy are dispersed more uniformly, and further improve the high strength and the high elongation of the magnesium alloy. Wherein, the price of Sc is expensive, while the grain refining function of Zr is not as good as that of Sc, but the price is cheap, and the two are added into the raw materials according to the mass percentage, so that the best grain refining effect can be obtained and the material cost is greatly reduced.
In the technical scheme, preferably, the rapidly-dissolved high-strength high-elongation magnesium alloy consists of the following elements in percentage by mass: 1.5 to 14.5 percent of Gd, 0.5 to 2.0 percent of Y, 0.1 to 2.0 percent of Al, 0.1 to 1.0 percent of Zn, 0.2 to 0.5 percent of ZrC, 0.001 to 0.02 percent of Sc, 0.1 to 2.0 percent of Cu, 0.01 to 1.0 percent of Li, 0.01 to 1.0 percent of Ni, 0.01 to 1.0 percent of Ga, 0.01 to 1.0 percent of In, and the balance of Mg and impurity elements, wherein the total amount of Li, Ni, Ga and In is 0.5 to 2.0 percent.
In the technical scheme, preferably, the rapidly-dissolved high-strength high-elongation magnesium alloy consists of the following elements in percentage by mass: 2.5% of Gd, 1.0% of Y, 1.0% of Al, 0.5% of Zn, 0.4% of Zr, 0.01% of Sc, 1.5% of Cu, 0.25% of Li0, 0.25% of Ni, 0.25% of Ga, 0.25% of In, and the balance of Mg and impurity elements.
Another object of the present invention is to provide a method for preparing the above rapidly dissolving high strength high elongation magnesium alloy, comprising the steps of:
s1, taking raw materials according to selected mass percentage;
s2, mixing the raw materials in the step S1, and then carrying out smelting, refining and covering to obtain a melt;
s3, casting the melt in the step S2 to obtain a cast ingot;
s4, homogenizing the cast ingot in the step S3, and then carrying out forming treatment to obtain a formed piece;
and S5, performing aging strengthening treatment on the formed part in the step S4 to obtain the rapidly-dissolved high-strength high-elongation magnesium alloy.
Preferably, step S1 specifically includes: taking pure Mg, pure Al, pure Zn, pure Ga, pure In, Mg-Gd intermediate alloy, Mg-Y intermediate alloy, Mg-Zr intermediate alloy, Mg-Sc intermediate alloy, Mg-Cu intermediate alloy, Mg-Li intermediate alloy and Mg-Ni intermediate alloy according to the selected mass percentage. The intermediate alloy can be selected from any commercially available intermediate alloy with any proportion, for example, Mg-Li intermediate alloy can be Mg-20% Li intermediate alloy, and Mg-Zr intermediate alloy can be Mg-30% Zr intermediate alloy.
Among them, it is preferable that the method further includes preheating the raw materials except for pure Ga before step S2, that is, further performing step S2a before step S2, where step S2a specifically is: preheating the pure Mg, the pure Al, the pure Zn, the pure In, the Mg-Gd intermediate alloy, the Mg-Y intermediate alloy, the Mg-Zr intermediate alloy, the Mg-Sc intermediate alloy, the Mg-Cu intermediate alloy, the Mg-Li intermediate alloy and the Mg-Ni intermediate alloy In the step S1 at the temperature of 100 ℃ and 300 ℃ for 5-12 h.
Preferably, step S2 specifically includes: mixing the raw materials, heating at 720-780 ℃, smelting for 30-60min, refining for 20-40min, and then covering with a covering agent.
The refining process may be carried out by adding a refining agent or by blowing a gas such as Ar into a refining furnace. Preferably, a refining agent is added in the refining process, the refining agent can be any commercially available magnesium alloy refining agent, and preferably, the refining agent can be a first refining agent which comprises the following components in parts by mass: MgCl224-30 parts of KCl20-26 parts of BaCl228-31 parts of CaF213-15 parts of NaCl, 1-7 parts of CaCl21-7 parts of insoluble substances, less than or equal to 1.5 parts of MgO, less than or equal to 1.5 parts of water and less than or equal to 2 parts of water; the refining agent can also be selected from a second refining agent, and the second refining agent comprises the following components in parts by mass: KCl54-56 parts and BaCl214-16 parts of CaF23 to 5 portions of CaCl227-29 parts of insoluble substances, less than or equal to 1.5 parts of MgO, less than or equal to 1.5 parts of water.
The covering agent can be any conventional commercially available magnesium alloy covering agent, and preferably consists of the following components in percentage by mass: MgCl235-41 parts of KCl, 25-29 parts of NaCl, 24-28 parts of CaCl26-10 parts of insoluble substances, less than or equal to 1.5 parts of MgO, and H2O is less than or equal to 2 parts.
Among them, it is preferable that the casting temperature when the melt is used for casting in step S3 is 670-750 ℃.
Preferably, the homogenization treatment in step S4 is specifically: keeping the ingot at 370-540 ℃ for 1-48 h; the molding treatment can be forging molding, extrusion molding or casting molding; the processing temperature in the molding process in step S4 is 300-450 ℃.
Preferably, the aging strengthening treatment in step S5 is specifically: and keeping the formed piece at the temperature of 25-250 ℃ for 20-1500 h.
Compared with the prior art, the invention has the following beneficial effects:
1. the rapidly-dissolved high-strength high-elongation magnesium alloy provided by the embodiment of the invention obtains interaction among alloy elements which is beneficial to improving the alloy performance by regulating the alloy composition and reasonably selecting the content of each element, obtains the magnesium alloy which has high reaction rate with media such as water and the like, has high-strength and high-elongation mechanical strength properties, and can meet the application requirements of various industrial fields;
2. in the rapidly-dissolved magnesium alloy with high strength and high elongation percentage, Cu, Li, Ni, Ga and In are mixed reaction promoting elements, the elements and magnesium form new crystal phases In the smelting process, and the crystal phases can destroy the continuity of generated magnesium hydroxide In the reaction process of magnesium and a water-soluble medium, so that the barrier of magnesium hydroxide on the contact of magnesium and the water-soluble medium is reduced, the reaction of magnesium and water and other media is promoted, and the reaction rate of magnesium and the water-soluble medium is increased;
3. in the rapidly-dissolved high-strength high-elongation magnesium alloy provided by the embodiment of the invention, Gd and Y can form solid solutions with Mg in the smelting process, the strength of the obtained alloy can be obviously improved through the solid solution or aging strengthening effect, and because the maximum solid solubility of Gd and Y in the magnesium alloy is 23.5% and 12.6% respectively, the Gd and Y are added in proper amount to ensure that Gd and Y and Mg can form solid solutions with single lattice structures respectively, so that the high strength and the high elongation of the magnesium alloy are achieved;
4. in the rapidly-dissolved magnesium alloy with high strength and high elongation percentage, Zr and Sc elements can obviously refine cast ingot grains of the material, and the refined grains can improve the strength and the plasticity of a magnesium alloy formed part according to a Hall Peltier formula; in addition, the refinement of the cast ingot crystal grains can also promote the dispersion uniformity of mixed reaction promoting elements of Li, Ni, Ga and In the alloy, further improve the reaction rate of magnesium and a water-soluble medium, and also promote the dispersion uniformity of Gd and Y In the alloy, so that the elements Gd and Y In the alloy are dispersed more uniformly, and further improve the high strength and the high elongation of the magnesium alloy. Wherein, the price of Sc is expensive, while the grain refining function of Zr is not as good as that of Sc, but the price is cheap, and the two are added into the raw materials according to the mass percentage, so that the best grain refining effect can be obtained and the material cost is greatly reduced.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1
The rapidly-dissolving high-strength high-elongation magnesium alloy described in this embodiment is composed of the following elements by mass: gd 2.5%, Y1.0%, Al1.0%, Zn 0.5%, Zr 0.4%, Sc 0.01%, Cu 1.5%, Li 0.25%, Ni 0.25%, Ga 0.25%, In 0.25%, and the balance of Mg.
The preparation method of the rapidly-dissolved magnesium alloy with high strength and high elongation includes the following steps:
s1, weighing pure Mg, pure Al, pure Zn, pure Ga, pure In, Mg-Gd intermediate alloy, Mg-Y intermediate alloy, Mg-Zr intermediate alloy, Mg-Sc intermediate alloy, Mg-Cu intermediate alloy, Mg-Li intermediate alloy and Mg-Ni intermediate alloy according to selected mass percentage;
s2, preheating the raw materials except the pure Ga in the step S1 at 150 ℃ for 2 h;
s3, mixing all the raw materials, heating the mixed raw materials to 720 ℃ by using a crucible resistance furnace, melting for 30min, adding a first refining agent, refining for 30min, removing impurities in the melt, and then covering the refined materials by using a covering agent to obtain a melt;
s4, casting the melt at 680 ℃ to obtain a cast ingot;
s5, homogenizing the ingot, preserving the heat of the ingot at 420 ℃ for 24 hours, and then forging and forming the homogenized ingot at 350 ℃ to obtain a forging piece;
s6, performing aging strengthening treatment on the forged piece, and preserving heat of the forged piece at 150 ℃ for 32 hours to obtain the rapidly-dissolved high-strength high-elongation magnesium alloy.
The first refining agent comprises the following components in parts by mass: MgCl224-30 parts of KCl, 20-26 parts of BaCl228-31 parts of CaF213-15 parts of NaCl, 1-7 parts of CaCl21-7 parts, insoluble matter less than or equal to 1.5 parts, MgO less than or equal to 1.5 parts and water less than or equal to 2 parts.
Wherein, the covering agent comprises the following components in percentage by mass: MgCl235-41 parts of KCl, 25-29 parts of NaCl24-28 parts of CaCl26-10 parts of insoluble substances, less than or equal to 1.5 parts of MgO, and H2O is less than or equal to 2 parts.
Example 2
The rapidly-dissolving high-strength high-elongation magnesium alloy described in this embodiment is composed of the following elements by mass: 1.5% of Gd, 0.5% of Y, 0.1% of Al, 0.1% of Zn, 0.2% of Zr, 0.001% of Sc, 0.1% of Cu, 0.01% of Li, 0.01% of Ni, 0.01% of Ga, 0.01% of In and the balance of Mg.
The method of making the rapidly dissolving, high strength, high elongation magnesium alloy described in this example is the same as in example 1.
Example 3
The rapidly-dissolving high-strength high-elongation magnesium alloy described in this embodiment is composed of the following elements by mass: 14.5% of Gd, 2.0% of Y, 2.0% of Al, 1.0% of Zn, 0.5% of Zr, 0.02% of Sc, 2.0% of Cu, 0.5% of Li, 0.5% of Ni, 0.5% of Ga, 0.5% of In and the balance of Mg.
The method of making the rapidly dissolving, high strength, high elongation magnesium alloy described in this example is the same as in example 1.
Example 4
The rapidly-dissolving high-strength high-elongation magnesium alloy described in this embodiment is composed of the following elements by mass: 8.0% of Gd, 1.2% of Y, 1.2% of Al, 0.5% of Zn, 0.3% of Zr, 0.008% of Sc, 1.3% of Cu, 0.25% of Li, 0.25% of Ni, 0.25% of Ga, 0.25% of In and the balance of Mg.
The method of making the rapidly dissolving, high strength, high elongation magnesium alloy described in this example is the same as in example 1.
Example 5
The rapidly-dissolving high-strength high-elongation magnesium alloy described in this embodiment is composed of the following elements by mass: 1.0% of Gd, 0.001% of Y, 0.001% of Al, 0.001% of Zn, 0.01% of Zr, 0.0001% of Sc, 0.01% of Cu, 0.01% of Li, 0.01% of Ni, 0.01% of Ga, 0.01% of In and the balance of Mg.
Example 6
The rapidly-dissolving high-strength high-elongation magnesium alloy described in this embodiment is composed of the following elements by mass: 12% of Gd, 4.0% of Y, 1.0% of Al, 2.5% of Zn, 0.5% of Zr, 0.005% of Sc, 0.8% of Cu, 0.4% of each of Li, Ni, Ga and In, and the balance of Mg.
The preparation method of the rapidly-dissolved magnesium alloy with high strength and high elongation includes the following steps:
s1, weighing pure Mg, pure Al, pure Zn, pure Ga, pure In, Mg-Gd intermediate alloy, Mg-Y intermediate alloy, Mg-Zr intermediate alloy, Mg-Sc intermediate alloy, Mg-Cu intermediate alloy, Mg-Li intermediate alloy and Mg-Ni intermediate alloy according to selected mass percentage;
s2, preheating the raw materials except the pure Ga in the step S1 at 120 ℃ for 4 h;
s3, mixing all the raw materials, heating the mixed raw materials to 780 ℃ by using a crucible resistance furnace, smelting for 50min, adding a first refining agent, refining for 30min, removing impurities in the melt, and then covering the refined material by using a covering agent to obtain a melt;
s4, casting the melt at 670 ℃ to obtain a cast ingot;
s5, homogenizing the cast ingot, preserving the heat of the cast ingot at 520 ℃ for 24 hours, and then forging and forming the homogenized cast ingot at 400 ℃ to obtain a forging piece;
s6, performing aging strengthening treatment on the forged piece, and preserving heat of the forged piece at 175 ℃ for 64h to obtain the rapidly-dissolved high-strength high-elongation magnesium alloy.
Example 7
The rapidly-dissolving high-strength high-elongation magnesium alloy described in this embodiment is composed of the following elements by mass: 6.0% of Gd, 2.0% of Y, 1.5% of Al, 2.5% of Zn, 0.5% of Zr, 0.01% of Sc, 1.8% of Cu, 0.2% of Li, 0.6% of Ni0.3% of Ga, 0.4% of In and the balance of Mg.
The preparation method of the rapidly-dissolved magnesium alloy with high strength and high elongation includes the following steps:
s1, weighing pure Mg, pure Al, pure Zn, pure Ga, pure In, Mg-Gd intermediate alloy, Mg-Y intermediate alloy, Mg-Zr intermediate alloy, Mg-Sc intermediate alloy, Mg-Cu intermediate alloy, Mg-Li intermediate alloy and Mg-Ni intermediate alloy according to selected mass percentage;
s2, preheating the raw materials except the pure Ga in the step S1 at 100 ℃ for 5 h;
s3, mixing all the raw materials, heating the mixed raw materials to 760 ℃ by using a crucible resistance furnace, melting for 40min, adding a second refining agent, refining for 25min, removing impurities in the melt, and then covering the refined materials by using a covering agent to obtain a melt;
s4, casting the melt at 690 ℃ to obtain a cast ingot;
s5, homogenizing the cast ingot, preserving the heat of the cast ingot at 460 ℃ for 12 hours, and then forging and forming the homogenized cast ingot at 400 ℃ to obtain a forging piece;
s6, performing aging strengthening treatment on the forged piece, and preserving heat of the forged piece at 175 ℃ for 64h to obtain the rapidly-dissolved high-strength high-elongation magnesium alloy.
The second refining agent comprises the following components in parts by mass: KCl54-56 parts and BaCl214-16 parts of CaF23 to 5 portions of CaCl227-29 parts of insoluble substances, less than or equal to 1.5 parts of MgO, less than or equal to 1.5 parts of water.
Example 8
The rapidly-dissolving high-strength high-elongation magnesium alloy described in this embodiment is composed of the following elements by mass: 1.5% of Gd, 4.0% of Y, 8.0% of Al, 1.2% of Zn, 0.4% of Zr, 0.01% of Sc, 7.5% of Cu, 1.5% of Li, 0.8% of Ni0.1% of Ga, 0.4% of In and the balance of Mg.
The preparation method of the rapidly-dissolved magnesium alloy with high strength and high elongation includes the following steps:
s1, weighing pure Mg, pure Al, pure Zn, pure Ga, pure In, Mg-Gd intermediate alloy, Mg-Y intermediate alloy, Mg-Zr intermediate alloy, Mg-Sc intermediate alloy, Mg-Cu intermediate alloy, Mg-Li intermediate alloy and Mg-Ni intermediate alloy according to selected mass percentage;
s2, preheating the raw materials except the pure Ga in the step S1 at 100 ℃ for 6 h;
s3, mixing all the raw materials, heating the mixed raw materials to 740 ℃ by using a crucible resistance furnace, smelting for 60min, adding a second refining agent, refining for 30min, removing impurities in the melt, and then covering the refined material by using a covering agent to obtain a melt;
s4, casting the melt at 680 ℃ to obtain a cast ingot;
s5, homogenizing the cast ingot, preserving the heat of the cast ingot at 400 ℃ for 48 hours, and then forging and forming the homogenized cast ingot at 380 ℃ to obtain a forging piece;
s6, performing aging strengthening treatment on the forged piece, and preserving heat of the forged piece at 120 ℃ for 64h to obtain the rapidly-dissolved high-strength high-elongation magnesium alloy.
Comparative example 1
The magnesium alloy of the comparative example consists of the following elements in percentage by mass:
gd 2.5%, Y1.0%, Al 1.0%, Zn 0.5%, Zr 0.4%, Sc 0.01%, and the balance of Mg. The preparation method of the magnesium alloy is the same as that of example 1.
Comparative example 2
The magnesium alloy of the comparative example consists of the following elements in percentage by mass:
gd 2.5%, Y1.0%, Al 1.0%, Zn 0.5%, Zr 0.4%, Sc 0.01%, Cu 10.5%, Li, Ni, Ga, In each 3.1%, and the balance Mg, and the magnesium alloy was prepared In the same manner as In example 1
Comparative example 3
The magnesium alloy of the comparative example consists of the following elements in percentage by mass:
2.5% of Gd, 1.0% of Y, 1.0% of Al, 0.5% of Zn, 0.4% of Zr, 0.01% of Sc, 0.1% of Si, 0.1% of Cu0.1%, 0.1% of Fe, 0.1% of Ni, 0.1% of Ga, 0.1% of In and the balance of Mg.
Comparative example 4
The magnesium alloy of the comparative example consists of the following elements in percentage by mass:
2.5 percent of Sr, 1.0 percent of La, 1.0 percent of Al, 0.5 percent of Zn, 0.4 percent of Zr, 0.01 percent of Sc, 1.5 percent of Cu, 0.25 percent of Li0, 0.25 percent of Ni, 0.25 percent of Ga, 0.25 percent of In and the balance of Mg.
Comparative example 5
The magnesium alloy of the comparative example consists of the following elements in percentage by mass:
25.0% of Gd, 6.0% of Y, 1.0% of Al, 2.5% of Zn, 0.5% of Zr, 0.005% of Sc, 0.8% of Cu, 0.4% of each of Li, Ni, Ga and In, and the balance of Mg.
Comparative example 6
The magnesium alloy of the comparative example consists of the following elements in percentage by mass:
1.0% of Y, 1.0% of Al, 0.5% of Zn, 1.5% of Cu, 0.25% of each of Li, Ni, Ga and In, and the balance of Mg.
Comparative example 7
The magnesium alloy of the comparative example consists of the following elements in percentage by mass:
2.5% of Gd, 1.0% of Y, 1.0% of Al, 0.5% of Zn, 0.4% of Zr, 1.5% of Cu, 0.25% of each of Li, Ni, Ga and In, and the balance of Mg.
Comparative example 8
The magnesium alloy composition of this comparative example was the same as the rapidly dissolving, high strength, high elongation magnesium alloy composition of example 1, except for the preparation method, in which the ingot obtained was not homogenized during the preparation of the magnesium alloy of this comparative example.
Comparative example 9
The magnesium alloy composition of this comparative example was the same as the rapidly dissolving, high strength, high elongation magnesium alloy composition of example 1, except for the preparation method, in which the magnesium alloy was prepared without subjecting the resulting forging to aging strengthening treatment.
Comparative example 10
The magnesium alloy composition of the present comparative example was the same as the rapidly-dissolving, high-strength, high-elongation magnesium alloy composition of example 1, except for the preparation method, in which the ingot after the homogenization treatment was directly subjected to the aging strengthening treatment without being subjected to the forming treatment in the magnesium alloy preparation process of the present comparative example.
And (3) performing mechanical property test and dissolution property test on the rapidly-dissolved high-strength high-elongation magnesium alloy in the embodiment and the magnesium alloy in the comparative example, wherein the mechanical property test method is executed according to GB T228.1-2010, and the dissolution property test conditions are as follows: will be provided withThe sample (2) was placed in a 3% KCl aqueous solution at 93 ℃ and the weight dissolved per hour was measured. The dissolution rate was: weight dissolved/(sample surface area × time). The mechanical properties and dissolution performance indexes of the rapidly-dissolving high-strength high-elongation magnesium alloy of the embodiment are shown in table 1.
TABLE 1 magnesium alloy room-temperature mechanical properties and high-temperature dissolution rates
The mechanical property test results show that the tensile strength of the rapidly-dissolved high-strength high-elongation magnesium alloy is more than or equal to 220MPa, the yield strength is more than or equal to 150MPa, and the elongation is more than or equal to 16 percent; the dissolution rate in 3% KCl solution at 93 deg.C is 40-100mg·cm-2h-1
The dissolution rate of the rapidly dissolving, high strength, high elongation magnesium alloy of the present invention in an aqueous medium is significantly higher than the magnesium alloy of comparative example 1, compared to the magnesium alloy of comparative example 1.
In the magnesium alloy of comparative example 2, the content of the mixing reaction promoting element is out of the content range of the present invention, and the dissolution rate in an aqueous medium is higher than that of the present invention, but the mechanical properties of the magnesium alloy of comparative example 2 are far inferior to those of the magnesium alloy of the present invention.
In the magnesium alloy of comparative example 3, the other components are the same as those In example 1 of the present invention, but the mixing reaction promoting elements are not selected from Cu, Li, Ni, Ga, In of the present invention, and the material elongation is far lower than that of the rapidly-dissolving high-strength high-elongation magnesium alloy of the present invention although the dissolution rate In an aqueous medium is similar to that of the present invention.
The magnesium alloy of comparative example 4 has the same other components as those of example 1 of the present invention, but does not contain two rare earth elements of Gd and Y, and contains two rare earth elements of Sr and La, and the mechanical properties thereof are significantly inferior to those of the rapidly soluble high-strength high-elongation magnesium alloy of example 1 of the present invention.
The magnesium alloy of comparative example 5 has the same other components as those of example 6 of the present invention, but the contents of Gd and Y are out of the range of the present invention, and the mechanical properties thereof are significantly inferior to those of the rapidly-dissolving high-strength high-elongation magnesium alloy of example 6 of the present invention.
In the magnesium alloys of comparative examples 6 and 7, other components were the same as those in inventive example 1, but Gd, Sc, and Zr were not contained; sc, the mechanical properties of which are significantly worse than those of the fast dissolving high strength high elongation magnesium alloy of the embodiment 1 of the present invention.
The magnesium alloys of comparative examples 8, 9 and 10 have the same composition as the alloy of example 1, but the mechanical properties of the magnesium alloy are significantly inferior to those of the rapidly-dissolving high-strength high-elongation magnesium alloy of example 1 of the present invention, because the preparation method does not include the homogenization treatment, the aging strengthening treatment and the forming treatment.
The rapidly-dissolved magnesium alloy with high strength and high elongation percentage comprises 1.5-14.5% of Gd, 0.5-2.0% of Y, 0.1-2.0% of Al, 0.1-1.0% of Zn, 0.2-0.5% of Zr, 0.001-0.02% of Sc, 0.1-2.0% of Cu0.01-1.0% of Li, 0.01-1.0% of Ni, 0.01-1.0% of Ga, 0.01-1.0% of In, and the balance of Mg, and has better comprehensive performance of mechanical property and dissolution property, and is a preferred scheme; wherein Gd 2.5%, Y1.0%, Al1.0%, Zn 0.5%, Zr 0.4%, Sc 0.01%, Cu 1.5%, Li 0.25%, Ni 0.25%, Ga 0.25%, In0.25%, and the balance of Mg, the scheme is the most preferable scheme.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (5)

1. A fast-dissolving high-strength high-elongation magnesium alloy is characterized by comprising the following elements in percentage by mass: 2.5% of Gd, 1.0% of Y, 1.0% of Al, 0.5% of Zn, 0.4% of Zr, 0.01% of Sc, 1.5% of Cu, 0.25% of Li, 0.25% of Ni, 0.25% of Ga, 0.25% of In, and the balance of Mg and impurity elements;
the preparation method of the rapidly-dissolved magnesium alloy with high strength and high elongation comprises the following steps:
s1, taking raw materials according to selected mass percentage;
s2, mixing the raw materials in the step S1, and then carrying out smelting, refining and covering to obtain a melt;
s3, casting the melt in the step S2 to obtain a cast ingot;
s4, homogenizing the ingot casting in the step S3 at the temperature of 370-540 ℃ for 1-48h, and then carrying out forming treatment to obtain a formed part;
s5, performing aging strengthening treatment on the formed piece in the step S4 at 25-250 ℃ for 20-1500h to obtain the rapidly-dissolved high-strength high-elongation magnesium alloy.
2. The rapidly dissolving, high strength, high elongation magnesium alloy of claim 1 wherein step S1 is specifically: taking pure Mg, pure Al, pure Zn, pure Ga, pure In, Mg-Gd intermediate alloy, Mg-Y intermediate alloy, Mg-Zr intermediate alloy, Mg-Sc intermediate alloy, Mg-Cu intermediate alloy, Mg-Li intermediate alloy and Mg-Ni intermediate alloy according to the selected mass percentage.
3. The rapidly dissolving, high strength, high elongation magnesium alloy of claim 2 further comprising, prior to step S2, step S2a, wherein step S2a is specifically: preheating the pure Mg, the pure Al, the pure Zn, the pure In, the Mg-Gd intermediate alloy, the Mg-Y intermediate alloy, the Mg-Zr intermediate alloy, the Mg-Sc intermediate alloy, the Mg-Cu intermediate alloy, the Mg-Li intermediate alloy and the Mg-Ni intermediate alloy In the step S1 at the temperature of 100-300 ℃ for 5-12 h.
4. The rapidly dissolving, high strength, high elongation magnesium alloy of claim 1 wherein step S2 is specifically: mixing the raw materials, heating at 720-780 ℃, smelting for 30-60min, refining for 20-40min, and then covering by using a covering agent.
5. The rapidly dissolving, high strength, high elongation magnesium alloy of claim 4 wherein the covering agent is comprised of the following components in parts by mass: MgCl235-41 parts of KCl, 25-29 parts of NaCl, 24-28 parts of CaCl26-10 parts of insoluble substances, less than or equal to 1.5 parts of MgO, and H2O is less than or equal to 2 parts.
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