CN117778838A - High-performance Si-containing magnesium alloy and preparation method thereof - Google Patents
High-performance Si-containing magnesium alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-performance Si-containing magnesium alloy and a preparation method thereof. The weight percentages of the components are as follows: si:0.2-3.5%, ca:0.05-1.2% of magnesium, additive elements and unavoidable impurities, wherein the additive elements are at least one of Mn, zn and Al, and the addition amounts are as follows in percentage: mn:0-1.1%, zn:0-1.1%, al:0-2.5%. The preparation method comprises the following steps: smelting, casting, heat treatment and plastic working. The alloy disclosed by the invention has good plastic processability, excellent mechanical properties, good heat conduction performance and excellent discharge performance, and can be used in the fields of high-quality lightweight structural parts, lightweight heat conduction parts, degradable biomedical materials, magnesium-air battery anode materials and the like.
Description
Technical Field
The invention relates to the field of metal materials and processing thereof, in particular to a preparation method of a high-performance Si-containing magnesium alloy.
Background
The magnesium alloy is the lightest metal material for engineering structures at present, has the advantages of higher specific strength and specific rigidity, good anti-magnetic interference property, excellent damping and shock absorption performance, higher thermal conductivity, easy recycling and the like, can be used for light-weight parts in the fields of vehicles, communication equipment and consumer electronics, can also be used for functional materials required in the fields of biomedical and battery and the like, and is considered as one of the new materials with the most development prospect in the 21 st century.
However, at present, only the performance of one or two aspects of magnesium alloy is generally concerned in the aspects of research and technical development of domestic and foreign magnesium alloy, and in practical application, on one hand, the service environment generally requires the alloy to have excellent comprehensive performance in many aspects; on the other hand, the component system alloy has various comprehensive properties, can meet the requirements of more diversified service environments, can be used for processing and preparing various different parts by the same material system, and is beneficial to simplifying the production and preparation flow and recycling. Patent CN111254333a discloses a wrought magnesium alloy and a preparation method thereof, wherein the wrought magnesium alloy comprises the following components in percentage by mass: 2.8 to 4.8 percent of Sn, 0.8 to 2.2 percent of Zn, 0.3 to 1.0 percent of Zr, 0.2 to 2.2 percent of RE (rare earth metal), 0.05 to 0.15 percent of Mn, less than or equal to 0.2 percent of impurity content, and the balance of Mg, wherein the tensile strength at room temperature is 322 to 372MPa, the yield strength is 243 to 318MPa, and the elongation is 16.82 to 26.15 percent; the alloy has higher content of alloying elements, more noble Zr element and rare earth element, lower strength, higher yield strength of 320MPa and lower mechanical property. Meanwhile, the plastic processing performance and the heat conduction performance of the alloy are not related, and the range of the service environment which can be met is small, so that the wide application of the alloy is limited. Patent CN101709418 discloses a heat conductive alloy, which has a chemical composition of 1-6.5-wt% Zn, 0.2-2.5-wt% Si; the thermal conductivity is more than 120W/(m.K) at 20 ℃, the tensile strength is 265-380 MPa, and the yield strength is 210-355 MPa. The alloy has good heat conduction performance and certain mechanical property, but the processing performance and the discharge performance when being used as the anode material of the battery are undefined, and the range of the service environment which can be met is small, so that the wide application of the alloy is limited. Patent CN201410298397.7 discloses a heat-conducting magnesium alloy capable of being extruded efficiently and with low cost and high performance, and a preparation method thereof, wherein the heat-conducting magnesium alloy comprises the following chemical components in percentage by weight: 0.1-0.8wt.% Al, 0.1-0.6wt wt.% Ca, 0.1-0.6wt.% Mn, 0.05-0.4wt.% La, the balance Mg and unavoidable impurities. The room temperature heat conductivity coefficient of the product after extrusion is larger than 125W/(m.K) and the tensile yield strength is 180-230 MPa, the alloy has higher extrusion processing performance and heat conductivity, but the mechanical property is insufficient, and the discharge performance and the like are not clear when the alloy is used as a battery anode material.
Therefore, if the magnesium alloy with the multiple performances of good processability, excellent mechanical property, high heat conductivity coefficient, high discharge voltage and the like can be developed, the application of the magnesium alloy with integrated structure and function can be remarkably promoted, and the magnesium alloy has wide application prospect.
Disclosure of Invention
Aiming at the problems that most magnesium alloys in the prior art are poor in processability, low in mechanical property, low in thermal conductivity, insufficient in discharge performance, difficult to combine with the above performance, high in raw material cost and the like, the invention provides a preparation method of high-performance Si-containing magnesium alloy.
The technical scheme of the invention is as follows:
a preparation method of high-performance Si-containing magnesium alloy comprises the following components in percentage by mass: si:0.2-3.5%, ca:0.05-1.2% of magnesium, additive elements and unavoidable impurities, wherein the additive elements are at least one of Mn, zn and Al, and the addition amounts are as follows in percentage: mn:0-1.1%, zn:0-1.1%, al:0-2.5%.
The invention also provides a preparation method of the high-performance Si-containing magnesium alloy, which is characterized by comprising the following steps:
(1) Smelting: cleaning a magnesium alloy smelting furnace and a crucible, heating to 400-500 ℃ and preheating for 0.3-2 hours, adding pure magnesium under the protection of protective gas or covering agent, and heating and melting at 730-800 ℃; then adding Mg-Si intermediate alloy and Mg-Ca intermediate alloy, after the intermediate alloy and the Mg-Si intermediate alloy are completely melted, sequentially adding at least one of pure Zn, pure Al and Mg-Mn intermediate alloy, after the intermediate alloy and the Mg-Si intermediate alloy are melted, uniformly stirring, then refining, degassing and deslagging, and standing for 5-100min to obtain alloy melt;
(2) Pouring: regulating the temperature of the melt to 665-700 ℃ and Ar and SF 6 Or SF 6 With CO 2 Under the protection of mixed gas, casting the magnesium alloy melt which is evenly smelted by adopting a sand casting, metal mold casting or semi-continuous casting mode to obtain an as-cast alloy ingot;
(3) And (3) heat treatment: carrying out heat treatment on the alloy cast ingot prepared in the step (2) in a heat treatment furnace, wherein the heat treatment temperature is 160-550 ℃ and the time is 0.5-48 hours, and then cooling to room temperature in an air cooling or water cooling mode;
(4) Plastic working: cutting the blank after heat treatment into corresponding specifications, removing surface oxide skin, heating to deformation temperature, placing into a deformation mold for deformation processing, wherein the deformation temperature is 180-520 ℃ and the strain rate is 0.001s -1 -20s -1 And the strain amount is more than 0.8, and the blank after thermal deformation is directly cooled to room temperature to obtain the magnesium alloy material.
Preferably, the shielding gas in step (1) is: ar and SF 6 Or SF 6 With CO 2 Or Ar,SF 6 、CO 2 And (3) mixing the three gases.
Preferably, the covering agent in the step (1) is RJ-5.
Preferably, the Mg-Si master alloy in the step (1) is a Mg-7Si master alloy, the Mg-Mn master alloy is a Mg-5Mn master alloy, and the Mg-Ca master alloy is a Mg-20Ca master alloy.
Preferably, the refining in the step (1) is refining by adding a refining agent or blowing argon gas or a combination thereof.
Preferably, the heat treatment in the step (3) is a single-stage heat treatment or a double-stage heat treatment, wherein the single-stage heat treatment is performed at a constant temperature between 160 ℃ and 410 ℃ for 0.5 to 20 hours, then cooling is performed, and the double-stage heat treatment is performed at a constant temperature between 400 ℃ and 430 ℃ for 5 to 24 hours, then the temperature is raised to a temperature between 450 ℃ and 550 ℃ for 1 to 24 hours.
Preferably, the plastic working in the step (4) is forging, rolling or extrusion, wherein the deformation speed of the extrusion is 0.1-50m/min, and the extrusion ratio is 5-100: and 1, directly cooling the blank after thermal deformation to room temperature at the extrusion temperature of 230-500 ℃ to obtain the magnesium alloy material.
Preferably, the mould of step (4) is a mould for forming a plate, rod, tube, wire or profile.
The invention has the substantial characteristics that:
the magnesium alloy of the invention belongs to a new magnesium alloy with excellent plastic processing property, mechanical property, heat conduction property and discharge property, si is taken as main alloying element, si can generate high melting point Mg with magnesium in the alloy in situ 2 The Si phase (the melting point is 1085 ℃) has a melting point higher than that of most magnesium-containing compounds, high thermal stability and high Mg-Si alloy eutectic point temperature (637.6 ℃), so that the alloy can be ensured not to be cracked due to melting of an alloy matrix or a second phase caused by actual temperature rise when the alloy is plastically deformed under the condition of high strain rate; the other key is that trace Ca element and Mn, zn, al and other additive elements are modified and smelted and poured at the same temperatureCan make Mg 2 The Si phase is obviously refined, thereby avoiding the occurrence of coarse blocky or even dendritic Mg 2 The Si phase avoids the splitting effect on the matrix, combines with the improvement of the capacity of the involution Jin Bianxing of a small amount of solid solution elements, and endows the alloy with good plastic workability. During plastic deformation, mg after refinement 2 The phase boundary between the Si phase and the matrix can provide more dynamic recrystallization nucleation sites, promote dynamic recrystallization in a particle excitation nucleation and mode, and pin the movement of a recrystallization grain boundary to inhibit the growth of recrystallization grains. In addition, trace Ca element can form nano precipitated phase in the matrix, and can effectively pin grain boundary movement. The above structural factors present in the alloy can significantly inhibit the growth of recrystallized grains, thereby achieving a fine recrystallized grain structure even when formed under high strain rate conditions (e.g., high-speed extrusion). On the other hand, when the alloy is subjected to external force, second phase particles and nano precipitated phases are dispersed in the matrix, so that dislocation movement can be blocked, and the mechanical properties of the alloy are synergistically improved together with fine grain strengthening effect. The alloying element in the alloy is mainly in the form of fine second phase particles, so that the heat conduction performance of the magnesium matrix is not excessively weakened while the active effects of re-refining and re-crystallizing grains and improving the mechanical performance of the alloy are exerted, and the alloy also has good heat conduction performance. In addition, as at least one of trace Si element, ca element and proper amount of additive elements (Mn, zn and Al) in the alloy are dissolved in the matrix in a solid manner, the discharge activity of the alloy is improved under the synergistic effect, so that the alloy has high discharge voltage when being used as an anode material of a magnesium air battery. Therefore, the alloy of the invention has excellent plastic processing performance, good mechanical property, high heat conductivity and high discharge performance.
Compared with the prior art, the invention has the beneficial effects that:
1) The Mg-Si based alloy has excellent plastic processing performance, can be subjected to plastic deformation processing such as forging, rolling, extrusion and the like in a wider temperature range, and has a wide plastic processing process window, wherein the highest extrusion speed can reach 50m/min during extrusion processing, and the maximum extrusion ratio can reach 100:1.
2) The extruded material prepared by the invention has fine grains and excellent mechanical properties. Even the alloy obtained under the high-speed deformation condition has the grain size of most below 40 mu m, and can lead the alloy to have good mechanical property, the tensile strength of 310-470 MPa and the elongation of more than 11 percent by combining the strengthening effect of the micro-nano double-scale second phase in the alloy and the solid solution strengthening effect of solid solution atoms. The alloy has the yield strength of 270MPa or more and the elongation of 10% or more under the high-speed extrusion condition of 50m/min, and shows excellent plastic processing performance and toughness performance.
3) The alloy has excellent heat conducting performance, and the heat conductivity of the alloy can reach more than 100W/m.K.
4) After the alloy is assembled into the metal-air battery, the discharge voltage is high, the highest discharge voltage of a single battery can reach more than 1.7V under the condition of full battery discharge test, the discharge voltage of the existing single-group magnesium-air battery is generally lower than 1.5V, and the discharge voltage of the metal-air battery assembled by the alloy is in the front of the magnesium-air battery and can be used as a high-quality magnesium-air battery anode material.
5) The magnesium alloy blank has simple preparation process, and introduces tiny Mg into magnesium 2 The method of Si phase element adopts Mg-Si intermediate alloy mode to introduce Si element, and then trace Ca element, mn, zn, al and other additive elements are modified and the smelting and casting temperature is regulated so as to ensure that Mg 2 Si phase is obviously refined, and the defect that fine dispersion distribution Mg is difficult to introduce into magnesium alloy is overcome 2 The technical problem of Si phase is that the existing smelting and extrusion equipment can be prepared without additional improvement, and the requirement on equipment is low.
6) The alloy disclosed by the invention can obtain good mechanical properties without heat treatment after deformation processing, so that the production process is simplified, the energy consumption and the production cost are reduced, and the processing efficiency is improved.
7) The alloy of the invention has low price of raw materials and low material cost, and is convenient for mass application in civil fields such as automobiles, high-speed rails, airplanes and the like.
8) The related elements in the alloy have no harmful effect on the whole human body, and partial elements have beneficial effects of promoting bone tissue growth and the like, and are also expected to be used as biomedical materials due to good mechanical properties.
Drawings
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further illustrated with reference to the accompanying drawings.
FIG. 1 is an extruded microstructure of example 2 alloy at an extrusion speed of 2 m/min;
FIG. 2 is a typical tensile stress strain curve for the alloy of example 2 at an extrusion speed of 40 m/min;
FIG. 3 is an extruded microstructure of example 3 alloy extrusion speed 40 m/min;
FIG. 4 is an extruded microstructure of example 4 alloy at an extrusion speed of 25 m/min;
FIG. 5 is an extruded microstructure of the alloy of example 5 at an extrusion speed of 50 m/min;
FIG. 6 shows the microstructure of the alloy of example 6 in an extruded state at an extrusion speed of 4 m/min.
Detailed Description
The technical scheme of the invention is described in detail by the following specific examples, which are all implemented on the premise of the technical scheme of the invention, and detailed implementation modes and specific operation processes are given, but the protection scope of the invention is not limited to the following examples.
Example 1
Mg-1.8Si-0.4Ca (wt%) is designed and selected, and the preparation method comprises the following steps:
(1) Smelting: cleaning a smelting furnace, heating to 450 ℃, putting a magnesium ingot preheated to 150 ℃ into a crucible of the smelting furnace for heating, and introducing Ar with the flow ratio of: SF (sulfur hexafluoride) 6 Mixed gas protection of =100:1 prevents combustion; heating furnace temperature to 760 ℃ at a heating rate of 10 ℃/min, adding Mg-7Si intermediate alloy preheated to about 150 ℃ after magnesium ingot is completely melted, adding Mg-30Ca intermediate alloy after melting, mechanically stirring for 2 minutes after full melting to make melt uniform, adjusting furnace temperature to 720 ℃, blowing argon for refining and degassing treatment, skimming surface scum, preserving heat and standing for 20 minutesObtaining a uniform alloy melt;
(2) Pouring: regulating the temperature of the melt to 690 ℃, and regulating the temperature of the melt in Ar and SF 6 Under the protection of the mixed gas, adopting a metal mold, and preparing a cylindrical magnesium alloy cast blank with the diameter of 60mm by gravity casting;
(3) And (3) heat treatment: the cut as-cast alloy ingot is subjected to heat preservation for 1h at 300 ℃, and then water quenching treatment is carried out;
(4) Plastic working: and (3) turning to remove an oxide layer on the surface of the alloy ingot after heat treatment in the step (4), processing into a cylindrical blank with the height of 120mm and the diameter of 65mm, placing the cylindrical blank into a die to perform forging deformation processing, forging the blank at the temperature of 450 ℃ and the temperature of 450 ℃ at the pressing speed of a pressing head of 2mm/s, obtaining a cake-shaped sample with the height of 20mm after forging, and then air-cooling to room temperature to obtain the high-performance Si-containing magnesium alloy.
The second phase composition of the obtained extruded alloy is Mg 2 Si、Mg 2 Ca; the grain size of the prepared alloy is below 15 microns; a sample with the length of 50mm is cut from the prepared forged magnesium alloy blank, a round bar-shaped tensile sample with the gauge length of 20mm and the diameter of the gauge length of 4mm is processed, and a tensile test is carried out, so that the tensile strength of the alloy is 315.2MPa, the yield strength is 257.4MPa, the elongation is 14.5%, and the alloy has good mechanical properties. A square pattern of 6mm by 6mm was further prepared, and the alloy of this example was measured to have a thermal conductivity value of 126W/mK. Taking a cylindrical sample with the diameter of 6mm, embedding and assembling the sample into a magnesium-air battery, and measuring alloy at 2.5 mA/cm by adopting a full-battery performance tester 2 、50 mA/cm 2 、120 mA/cm 2 Under the current density condition, the discharge voltage of the discharge battery is respectively 1.75V, 1.3V and 0.8V, and the alloy has excellent mechanical property, heat conduction property and discharge property.
Example 2
The design and selection of Mg-0.5Si-1.5Al-0.35Ca-0.5Mn (wt%) and proportioning according to the composition, the preparation method comprises the following steps:
(1) Smelting: cleaning a smelting furnace, heating to 450 ℃, putting a magnesium ingot preheated to 150 ℃ into a crucible of the smelting furnace, heating, and adding a No. 5 solvent to prevent combustion; heating the furnace temperature to 760 ℃ at a heating rate of 10 ℃/min, adding Mg-7Si intermediate alloy preheated to 150 ℃ after the magnesium ingot is completely melted, sequentially adding Mg-20Ca intermediate alloy and pure Al blocks preheated to about 150 ℃ after the magnesium ingot is melted, adding Mg-5Mn intermediate alloy after the magnesium ingot is melted, and preserving heat until the raw materials are fully melted; mechanically stirring for 3 minutes to make the melt uniform, then adjusting the furnace temperature to 720 ℃, blowing argon for refining and degassing treatment, skimming surface scum, and standing for 20 minutes to obtain uniform alloy melt;
(2) Pouring: regulating the temperature of the melt to 680 ℃, and controlling the flow ratio to be CO 2 ：SF 6 Preparing a cylindrical magnesium alloy cast blank with the diameter of 36mm by adopting a metal mold under the protection of mixed gas of 100:1;
(3) And (3) heat treatment: the cut as-cast alloy ingot is firstly preserved for 5 hours at 410 ℃ and then is subjected to water quenching treatment;
(4) Plastic working: cutting the heat-treated blank into a height of 100mm, removing surface oxide skin, and setting extrusion process parameters: the method comprises the steps of heating a deformed blank for 30 minutes to reach the set extrusion temperature of 300 ℃, putting the deformed blank into an extrusion barrel, carrying out extrusion processing according to the parameters to obtain a bar with the diameter of 6mm, and cooling the extruded bar by adopting air cooling, wherein the extrusion speed is respectively set to be 2m/min, 40m/min and the extrusion ratio is 36.
The second phase composition of the obtained extruded alloy is Mg 2 Si、Al 2 Ca. alpha-Mn. FIG. 1 is a microstructure of the alloy of example 2 in an extruded state at an extrusion speed of 2m/min, from which it can be seen that after extrusion, the alloy is partially recrystallized, the alloy structure consisting of deformed grains and recrystallized grains, the recrystallized grains having a size of about 5 microns or less; at an extrusion speed of 2m/min, the tensile strength of the alloy is 466.9MPa, the yield strength is 406.3MPa, and the elongation is 17.8%. The billet prepared at the extrusion speed of 2m/min of this example was selected, a square sample of 6 mm. Times.6 mm was processed, and the billet was prepared at the extrusion speed of 2m/min of the alloy of this example by measurement, with a thermal conductivity value of 105W/mK. Processing into cylindrical sample with diameter of 6mm, embedding, and assembling into magnesium-airBattery, using full battery performance tester, alloy measured at 2.5 mA/cm 2 、50 mA/cm 2 、120 mA/cm 2 Under the current density condition, the discharge voltage of the discharge battery is 1.73V, 1.32V and 0.73V respectively, and the alloy shows excellent mechanical property and excellent discharge performance and better heat conduction performance than commercial AZ31 alloy (heat conductivity 77W/(m.K)).
The alloy tensile strength 389.1MPa, yield strength 351.4MPa and elongation 26.5% at extrusion speed 40m/min, and its typical tensile stress strain curve is shown in FIG. 2. The thermal conductivity value is 107W/m.K by the same method; alloy measured at 2.5 mA/cm 2 、50 mA/cm 2 、120 mA/cm 2 Under the current density condition, the discharge voltage of the discharge battery is 1.70V, 1.31V and 0.71V respectively, and the alloy shows excellent mechanical property and excellent discharge performance and better heat conduction performance than commercial AZ31 alloy (thermal conductivity 78W/mK).
Example 3
The design and selection of Mg-0.5Si-0.8Zn-0.45Ca-0.3Mn (wt%) and proportioning according to the composition, the preparation method comprises the following steps:
(1) Smelting: cleaning a smelting furnace, heating to 450 ℃, putting a magnesium ingot preheated to 150 ℃ into a crucible of the smelting furnace, heating, and adding a No. 5 solvent to prevent combustion; heating the furnace temperature to 760 ℃ at a heating rate of 10 ℃/min, adding the Mg-7Si intermediate alloy and the Mg-5Mn intermediate alloy which are preheated to 150 ℃ after the magnesium ingot is completely melted, and sequentially adding the Mg-20Ca intermediate alloy and the pure Zn block which are preheated to about 150 ℃ after the magnesium ingot is melted, and preserving heat until the raw materials are fully melted; mechanically stirring for 3 minutes to make the melt uniform, then adjusting the furnace temperature to 730 ℃, blowing argon for refining and degassing treatment, skimming surface scum, and standing for 20 minutes to obtain uniform alloy melt;
(2) Pouring: regulating the temperature of the melt to 680 ℃, and controlling the flow ratio to be CO 2 ：SF 6 Preparing a cylindrical magnesium alloy cast blank with the diameter of 36mm by adopting a metal mold under the protection of mixed gas of 100:1;
(3) And (3) heat treatment: the cut as-cast alloy ingot is firstly preserved for 5 hours at 410 ℃ and then is subjected to water quenching treatment;
(4) Plastic working: cutting the heat-treated blank into a height of 100mm, removing surface oxide skin, and setting extrusion process parameters: the method comprises the steps of heating a deformed blank for 30 minutes at the preset extrusion temperature of 300 ℃, putting the deformed blank into an extrusion barrel, carrying out extrusion processing according to the parameters to obtain a bar with the diameter of 6mm, and cooling the extruded bar by adopting air cooling, wherein the extrusion speed is set to 40m/min, and the extrusion ratio is 36.
The second phase composition of the obtained extruded alloy is Mg 2 Si、Mg 2 Ca. alpha-Mn. FIG. 3 is a microstructure of the alloy of example 3 in an extruded state at an extrusion speed of 40m/min, from which it can be seen that the alloy undergoes almost complete recrystallization after extrusion processing, with a recrystallization ratio of about 95%, the alloy structure consisting of deformed grains and recrystallized grains, the recrystallized grains having a size of about 20 microns or less; the tensile strength of the alloy is 335.4MPa, the yield strength is 304.7MPa, the elongation is 13.8%, and the alloy has excellent strength and plasticity; a square pattern of 6mm by 6mm was further prepared, and the alloy of this example was measured to have a thermal conductivity of 126W/mK. Preparing a cylindrical sample with the diameter of 6mm, embedding and assembling the sample into a magnesium-air battery, and measuring alloy at 2.5 mA/cm by adopting a full-battery performance tester 2 、50 mA/cm 2 、120 mA/cm 2 Under the current density condition, the discharge voltage of the discharge battery is 1.76V, 1.31V and 0.74V respectively, and the alloy shows excellent mechanical property, heat conduction property and discharge property.
Example 4
Mg-1.5 Si-0.2 Al-0.5Ca-0.7Mn (wt%) is designed and selected, and the preparation method comprises the following steps:
(1) Smelting: cleaning a smelting furnace, heating to 450 ℃, putting a magnesium ingot preheated to 150 ℃ into a crucible of the smelting furnace, heating, and adding a No. 5 solvent to prevent combustion; heating the furnace temperature to 750 ℃ at the heating rate of 10 ℃/min, adding the Mg-7Si intermediate alloy and the Mg-5Mn intermediate alloy which are preheated to 150 ℃ after the magnesium ingot is completely melted, and sequentially adding the Mg-20Ca intermediate alloy and the pure Al block which are preheated to about 150 ℃ after the magnesium ingot is melted, and preserving heat until the raw materials are fully melted; mechanically stirring for 3 minutes to make the melt uniform, then adjusting the furnace temperature to 720 ℃, blowing argon for refining and degassing treatment, skimming surface scum, and standing for 20 minutes to obtain uniform alloy melt;
(2) Regulating the temperature of the melt to 680 ℃, and controlling the flow ratio to be CO 2 ：SF 6 Preparing a cylindrical magnesium alloy cast blank with the diameter of 36mm by adopting a metal mold under the protection of mixed gas of 100:1;
(3) And (3) heat treatment: the cut as-cast alloy ingot is firstly preserved for 5 hours at 410 ℃ and then is subjected to water quenching treatment;
(4) Plastic working: cutting the heat-treated blank into a height of 100mm, removing surface oxide skin, and setting extrusion process parameters: the method comprises the steps of heating a deformed blank for 30 minutes at the preset extrusion temperature of 310 ℃, putting the deformed blank into an extrusion barrel, carrying out extrusion processing according to the parameters to obtain a bar with the diameter of 6mm, and cooling the extruded bar by adopting air cooling, wherein the extrusion speed is set to 25m/min, and the extrusion ratio is 36.
The second phase composition of the obtained extruded alloy is Mg 2 Si、Al 2 Ca、Mg 2 Ca. alpha-Mn. FIG. 4 is a microstructure of the alloy of example 4 in an extruded state at an extrusion speed of 25m/min, from which it can be seen that almost complete recrystallization of the alloy occurs after extrusion, the microstructure of the alloy consisting of very few deformed grains and recrystallized grains having a size of about 20 microns or less; the tensile strength of the alloy is 346.3MPa, the yield strength is 306.2MPa and the elongation is 18.4%. A square pattern of 6mm by 6mm was further prepared, and the alloy of this example was measured to prepare a billet at an extrusion rate of 2m/min, with a thermal conductivity value of 105W/mK. Taking a cylindrical sample with the diameter of 6mm, embedding and assembling the sample into a magnesium-air battery, and measuring alloy at 2.5 mA/cm by adopting a full-battery performance tester 2 、50 mA/cm 2 、120 mA/cm 2 Under the current density condition, the discharge voltage of the discharge battery is 1.7V, 1.31V and 0.72V respectively, and the alloy shows excellent mechanical property and excellent discharge performance, compared with commercial AZ31 alloyGold (thermal conductivity 78W/mK) has better thermal conductivity.
Example 5
Mg-1.5Si-0.6Zn-0.35Ca-0.5Mn (wt%) is designed and selected, and the preparation method comprises the following steps:
(1) Smelting: cleaning a smelting furnace, heating to 450 ℃, putting a magnesium ingot preheated to 150 ℃ into a crucible of the smelting furnace, heating, and adding a No. 5 solvent to prevent combustion; heating the furnace temperature to 760 ℃ at a heating rate of 10 ℃/min, adding the Mg-10Si intermediate alloy and the Mg-5Mn intermediate alloy which are preheated to 150 ℃ after the magnesium ingot is completely melted, and sequentially adding the Mg-20Ca intermediate alloy and the pure Zn block which are preheated to about 150 ℃ after the magnesium ingot is melted, and preserving heat until the raw materials are fully melted; mechanically stirring for 3 minutes to make the melt uniform, then adjusting the furnace temperature to 720 ℃, blowing argon for refining and degassing treatment, skimming surface scum, and keeping the temperature and standing for 20 minutes to obtain uniform alloy melt;
(2) Regulating the temperature of the melt to 695 ℃ and controlling the flow ratio to be CO 2 ：SF 6 Preparing a cylindrical magnesium alloy cast blank with the diameter of 36mm by adopting a metal mold under the protection of mixed gas of 100:1;
(3) And (3) heat treatment: the cut as-cast alloy ingot is firstly preserved for 5 hours at 410 ℃ and then is subjected to water quenching treatment;
(4) Plastic working: cutting the heat-treated blank into a height of 100mm, removing surface oxide skin, and setting extrusion process parameters: the method comprises the steps of heating a deformed blank for 30 minutes at the preset extrusion temperature of 300 ℃, putting the deformed blank into an extrusion barrel, carrying out extrusion processing according to the parameters to obtain a bar with the diameter of 6mm, and cooling the extruded bar by adopting air cooling, wherein the extrusion speed is set to be 50m/min, the extrusion ratio is 36.
The second phase composition of the obtained extruded alloy is Mg 2 Si、Mg 2 Ca. alpha-Mn. FIG. 5 is a microstructure of the alloy of example 5 in an extruded state at an extrusion speed of 50m/min, from which it can be seen that the alloy is partially recrystallized after extrusion to a recrystallization rate of about 95%, the alloy structure being composed of deformed grainsAnd recrystallized grains having a size of 25 microns or less; the tensile strength of the alloy is 337.6MPa, the yield strength is 278.3MPa, and the elongation is 12.1%; a square pattern of 6mm by 6mm was further prepared, and its thermal conductivity was measured to be 126.8W/mK. Taking a cylindrical sample with the diameter of 6mm from the alloy of the embodiment, embedding and assembling the sample into a magnesium-air battery, and measuring the alloy at 2.5 mA/cm by adopting a full-battery performance tester 2 、50 mA/cm 2 、120 mA/cm 2 Under the current density condition, the discharge voltage of the discharge battery is 1.72V, 1.32V and 0.73V respectively, and the alloy shows excellent mechanical property, heat conduction property and discharge property.
Example 6
Mg-1Si-0.25Mn-0.5Al-0.6Ca-0.5Zn (wt%) is designed and selected, and the preparation method comprises the following steps:
(1) Smelting: cleaning the smelting furnace, heating to 450 ℃, putting pure Mg (99.95 wt%) ingot preheated to 150 ℃ into a crucible of the smelting furnace for heating, and introducing CO 2 ：SF 6 Mixed gas protection of =100:1 (flow ratio) prevents combustion; heating the furnace temperature to 740 ℃ at the heating rate of 10 ℃/min, adding the Mg-7Si intermediate alloy and the Mg-5Mn intermediate alloy which are preheated to about 150 ℃ after the magnesium ingot is completely melted, and sequentially adding the Mg-20Ca intermediate alloy (the actual detection content of Ca is 19.92 wt%), the pure Zn (99.9 wt%) ingot and the pure Al (99.9 wt%) ingot after the magnesium ingot is melted, and preserving heat until the intermediate alloy is fully melted; stirring the raw materials for 2 minutes after the raw materials are completely melted to ensure that the melt is uniform, then adjusting the furnace temperature to 720 ℃, blowing argon for refining and degassing treatment, skimming surface scum, keeping the temperature and standing for 20 minutes, and standing for treatment to obtain alloy melt;
(2) Pouring: regulating the temperature of the melt to 680 ℃, and controlling the flow ratio to be CO 2 ：SF 6 Under the protection of mixed gas of 100:1, a cylindrical magnesium alloy cast blank with the diameter of 60mm is prepared by adopting metal mold casting;
(3) And (3) heat treatment: the cut as-cast alloy ingot is firstly subjected to heat treatment at 410 ℃ for 6 hours, then is heated to 460 ℃ for 5 hours, and is then subjected to water quenching treatment;
(4) Extrusion processing: cutting the blank after heat treatment into corresponding specifications, removing surface oxide skin, and then setting extrusion process parameters: extrusion temperature 280 ℃, extrusion speed set to 4m/min, extrusion ratio 100: and 1, heating the deformed blank for 30 minutes to reach the required extrusion temperature of 280 ℃, putting the deformed blank into an extrusion cylinder, and carrying out extrusion processing according to the parameters to obtain a bar with the diameter of 6mm, and cooling the extruded bar by adopting air cooling to obtain the high-performance Si-containing magnesium alloy.
The second phase composition of the obtained extruded alloy is Mg 2 Si、Al 2 Ca 、Mg 2 Ca. alpha-Mn; FIG. 6 shows the microstructure of the alloy of example 6 in an extrusion state at an extrusion speed of 4m/min, wherein after extrusion, the alloy is almost completely recrystallized, the grain size is less than 8 microns, the tensile strength of the alloy is 442.5MPa, the yield strength is 399.7 MPa, the elongation is 20.8%, and the alloy has high strength and excellent mechanical properties; further preparing a square pattern of 6mm multiplied by 6mm, and measuring to obtain a billet with the heat conductivity reaching 102W/m x K at the extrusion speed of 2m/min of the alloy of the embodiment; taking a cylindrical sample with the diameter of 6mm from the alloy of the embodiment, embedding and assembling the sample into a magnesium-air battery, and measuring the alloy at 2.5 mA/cm by adopting a full-battery performance tester 2 、50 mA/cm 2 、120 mA/cm 2 The discharge voltage of the discharge cell was 1.72V, 1.34, V, and 0.72, V, respectively, at current density.
Comparative example 1
Mg-1.5Si-0.6Zn-0.35Ca-0.5Mn (wt%) is designed and selected, and the preparation method comprises the following steps:
(1) Smelting: cleaning a smelting furnace, heating to 450 ℃, putting a magnesium ingot preheated to 150 ℃ into a crucible of the smelting furnace, heating, and adding a No. 5 solvent to prevent combustion; heating the furnace temperature to 760 ℃ at a heating rate of 10 ℃/min, adding the Mg-10Si intermediate alloy and the Mg-5Mn intermediate alloy which are preheated to 150 ℃ after the magnesium ingot is completely melted, and sequentially adding the Mg-20Ca intermediate alloy and the pure Zn block which are preheated to about 150 ℃ after the magnesium ingot is melted, and preserving heat until the raw materials are fully melted; mechanically stirring for 3 minutes to make the melt uniform, then adjusting the furnace temperature to 720 ℃, blowing argon for refining and degassing treatment, skimming surface scum, and keeping the temperature and standing for 20 minutes to obtain uniform alloy melt;
(2) Pouring: regulating the temperature of the melt to 730 ℃ and controlling the flow ratio to be CO 2 ：SF 6 Preparing a cylindrical magnesium alloy cast blank with the diameter of 36mm by adopting a metal mold under the protection of mixed gas of 100:1;
(3) And (3) heat treatment: the cut as-cast alloy ingot is firstly preserved for 5 hours at 410 ℃ and then is subjected to water quenching treatment;
(4) Plastic working: cutting the heat-treated blank into a height of 100mm, removing surface oxide skin, and setting extrusion process parameters: the blank temperature is 300 ℃, the extrusion barrel temperature is 300 ℃, the die temperature is 300 ℃, the extrusion speed is set to be 100m/min, the extrusion ratio is 36, the deformed blank is heated for 30 minutes to reach the set extrusion temperature of 300 ℃, the deformed blank is put into the extrusion barrel, and extrusion processing is carried out according to the parameters, so that the alloy blank is cracked and cannot be extruded and formed.
Observing the microstructure of the as-cast alloy obtained in the step (2) to find that the microstructure of the alloy has a large amount of blocky and a small amount of dendritic Mg 2 The Si phase can be 30 μm or more in size, indicating that the Mg in the alloy is high if the casting temperature is high (730 ℃ C.) even under the condition of adding Ca, mn, zn and other elements 2 The Si phase cannot be modified and refined into a fine grain phase. Eventually leading to deterioration of plastic deformation properties of the alloy, and cracking occurs during extrusion. Controlling the processing and preparation process is one of the keys of the invention.
Comparative example 2
Selecting the current commercial magnesium alloy AZ31, homogenizing the alloy cast ingot at 400 ℃ for 24 hours, peeling, extruding at an extrusion speed of 25 m/mm, an extrusion ratio of 36 and an extrusion temperature of 360 ℃. Heating the deformed blank for 30 minutes to reach the required extrusion temperature of 360 ℃, putting the deformed blank into an extrusion cylinder, carrying out extrusion processing according to the parameters to obtain a bar with the diameter of 10 mm, and cooling the extruded bar by adopting air cooling to obtain the alloy of the comparative example AZ 31. The second phase group of the obtained extruded alloy has only a small amount of alpha-Mn phase, the average yield strength, tensile strength and elongation of the AZ31 alloy are about 123.4MPa, 199.4MPa and 12.6%, respectively, and the alloy of the invention shows a higher extrusion speedExcellent strength. Its thermal conductivity is 78W/(m.K), after inlaid, it is assembled into magnesium-air battery, and the alloy measured by adopting full-cell performance tester is 2.5 mA/cm 2 、50 mA/cm 2 、120 mA/cm 2 The discharge voltages of the discharge cells were 1.20V, 0.92V, and 0.32V, respectively, at current densities. Compared with the alloy of the comparative example, the alloy of the invention has more excellent plastic processing property, mechanical property, heat conducting property and discharge property.
The starting materials and equipment used in the above examples were all obtained by known means and the operating procedures used are within the skills of a person skilled in the art.
Claims (9)
1. The high-performance Si-containing magnesium alloy comprises the following components in percentage by mass: si:0.2-3.5%, ca:0.05-1.2% of magnesium, additive elements and unavoidable impurities, wherein the additive elements are at least one of Mn, zn and Al, and the addition amounts are as follows in percentage: mn:0-1.1%, zn:0-1.1%, al:0-2.5%.
2. The method for preparing the high-performance Si-containing magnesium alloy according to claim 1, comprising the steps of:
(1) Smelting: cleaning a magnesium alloy smelting furnace and a crucible, heating to 400-500 ℃ and preheating for 0.3-2 hours, adding pure magnesium under the protection of protective gas or covering agent, adding pure magnesium, and heating and melting at 730-800 ℃; then adding an Mg-Si intermediate alloy and an Mg-Ca intermediate alloy, after the intermediate alloy and the Mg-Si intermediate alloy are completely melted, sequentially adding at least one of pure Zn, pure Al and an Mg-Mn intermediate alloy, after the intermediate alloy and the Mg-Si intermediate alloy are melted, uniformly stirring, then refining, degassing and deslagging, and standing for 5-100min to obtain an alloy melt;
(2) Pouring: regulating the temperature of the melt to 665-700 ℃ and Ar and SF 6 Or SF 6 With CO 2 Under the protection of mixed gas, casting the magnesium alloy melt which is evenly smelted by adopting a sand casting, metal mold casting or semi-continuous casting mode to obtain an as-cast alloy ingot;
(3) And (3) heat treatment: carrying out heat treatment on the alloy cast ingot prepared in the step (2) in a heat treatment furnace, wherein the heat treatment temperature is 160-550 ℃ and the time is 0.5-48 hours, and then cooling to room temperature in an air cooling or water cooling mode;
(4) Plastic working: cutting the blank after heat treatment into corresponding specifications, removing surface oxide skin, heating to deformation temperature, placing into a deformation mold for deformation processing, wherein the deformation temperature is 180-520 ℃ and the strain rate is 0.001s -1 -20s -1 And the strain amount is more than 0.8, and the blank after thermal deformation is directly cooled to room temperature to obtain the magnesium alloy material.
3. The method for preparing the high-performance Si-containing magnesium alloy according to claim 2, wherein: the protective gas in the step (1) is as follows: ar and SF 6 Or SF 6 With CO 2 Or Ar, SF 6 、CO 2 And (3) mixing the three gases.
4. The method for preparing the high-performance Si-containing magnesium alloy according to claim 2, wherein: the covering agent in the step (1) is RJ-5.
5. The method for preparing the high-performance Si-containing magnesium alloy according to claim 2, wherein: the Mg-Si intermediate alloy in the step (1) is a Mg-7Si intermediate alloy, the Mg-Mn intermediate alloy is a Mg-5Mn intermediate alloy, and the Mg-Ca intermediate alloy is a Mg-20Ca intermediate alloy.
6. The method for preparing the high-performance Si-containing magnesium alloy according to claim 2, wherein: the refining in the step (1) is refining agent refining or argon blowing refining or a combination thereof.
7. The method for preparing the high-performance Si-containing magnesium alloy according to claim 2, wherein: the heat treatment in the step (3) is single-stage heat treatment or double-stage heat treatment, wherein the single-stage heat treatment is carried out at a certain constant temperature between 160 and 410 ℃ for 0.5 to 20 hours, then cooling is carried out, the double-stage heat treatment is carried out at a certain constant temperature between 400 and 430 ℃ for 5 to 24 hours, and then the temperature is raised to a certain temperature between 450 and 550 ℃ for 1 to 24 hours.
8. The method for preparing the high-performance Si-containing magnesium alloy according to claim 2, wherein: the plastic working in the step (4) is forging, rolling or extrusion, wherein the deformation speed of the extrusion is 0.1-50m/min, and the extrusion ratio is 5-100: and 1, directly cooling the blank after thermal deformation to room temperature at the extrusion temperature of 230-500 ℃ to obtain the magnesium alloy material.
9. The method for preparing the high-performance Si-containing magnesium alloy according to claim 2, wherein: the die in the step (4) is a die for forming a plate, a rod, a tube, a wire or a section.
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