CN111057982A - Mn-Cu-based submicron/nano porous high-damping alloy and preparation method thereof - Google Patents
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Abstract
The invention discloses a Mn-Cu-based submicron/nano porous high damping alloy and a preparation method thereof, wherein the preparation method comprises the steps of carrying out heat treatment on a Mn-Cu-based alloy to ensure that α -Mn phase is desolventized and separated from the alloy to obtain a composite material with submicron or nano α -Mn precipitated phase dispersed and distributed on a Mn-Cu-based alloy matrix, and carrying out dealloying treatment on the composite material to ensure that α -Mn precipitated phase is removed to obtain the Mn-Cu-based submicron/nano porous high damping alloy.
Description
Technical Field
The invention relates to the technical field of Mn-Cu-based alloys, in particular to a Mn-Cu-based submicron/nano porous high-damping alloy and a preparation method thereof.
Background
The Mn-Cu alloy is a typical twin boundary relaxation type high damping alloy, and the high damping mechanism is the sliding of a high-density twin crystal interface under the action of stress. The vibration damping alloy has the advantages of high vibration damping capacity, good comprehensive performance, simple and convenient preparation process, good hot working, cold working and welding performance and the like, and has been well accepted in the relevant vibration damping and noise reduction industrial fields. In particular M2052 damping alloy (Mn-20Cu-5Ni-2Fe, at%) when the strain amplitude is 10-6And when the damping value is high, the damping value can reach 0.06, and the good low-strain high-damping response characteristic is shown. Meanwhile, the yield strength, the tensile strength and the elongation of the series of alloys respectively reach 200MPa, 500MPa and 30 percent. Therefore, the material has received much attention as a material with vibration and noise reduction function and structural integration. However, in some applications with specific requirements on the specific gravity of the material, such as aerospace, automobiles and other fields, "lightweight material" has become a necessary trend of development. In contrast, the high specific gravity of Mn-Cu alloys (7 g/cm)3) Greatly limiting its development.
The most direct method for achieving weight reduction of the material is to use a metal material having a low density, but another method is to form a functional metal material having a high specific gravity into a porous structure. The conventional foam material has higher damping characteristics than a parent compact material, for example, the damping performance of foamed aluminum is increased along with the increase of porosity, and is generally several times to more than one order of magnitude higher than that of the compact aluminum. Therefore, the nano or submicron porous Mn-Cu alloy not only keeps the high damping characteristic and excellent mechanical property of the Mn-Cu alloy material, but also reduces the specific gravity of the Mn-Cu alloy to a certain extent. As a structural material, the material has the characteristics of light weight and high specific strength; as a functional material, the material has various physical properties such as sound insulation (or sound absorption), heat insulation (or heat dissipation), flame retardance, damping, impact energy absorption, electromagnetic shielding and the like, and is a novel structure and function integrated material with extremely wide application prospect.
However, at present, the common preparation methods of porous metals mainly include casting method (solution foaming method), powder metallurgy foaming method (adding pore-forming agent), and the like. The melt foaming method has the problems of high foaming temperature, non-uniform pore size, non-uniform distribution, high difficulty in process operation and the like; although the powder metallurgy foaming method has the advantages of simple equipment and process, uniform prepared pore structure, easy adjustment of alloy components and the like, the conventional foaming agents such as carbonate, metal hydride and the like belong to a chemical foaming method, the foaming agents are mainly decomposed at high temperature to release gas for foaming and pore-forming, once heat treatment process parameters are not proper, the prepared sample has low porosity or generates collapse, and the microstructure and the macroscopic properties of the material are seriously influenced. And the biggest problem is that the conventional methods cannot or are difficult to prepare porous materials with nano-scale or submicron-scale pores.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a Mn-Cu-based submicron/nano porous high damping alloy and a preparation method thereof, wherein the high damping alloy has the advantages of uniform pore forming and pore size distribution in a nanometer or submicron size.
The invention provides a preparation method of Mn-Cu-based submicron/nano porous high damping alloy, which comprises the following steps:
s1, carrying out heat treatment on the Mn-Cu-based alloy to ensure that a α -Mn phase is precipitated from the alloy in a desolvation way, thus obtaining the composite material with submicron or nanometer α -Mn precipitated phases dispersed and distributed on the Mn-Cu-based alloy matrix;
s2, carrying out dealloying treatment on the composite material obtained in the step S1 to remove a α -Mn precipitated phase, and obtaining the Mn-Cu-based submicron/nano porous high damping alloy.
Preferably, the Mn — Cu based alloy is a binary alloy composed of manganese and copper, or a multi-element alloy composed of other alloying elements in addition to manganese and copper, and the other alloying elements are preferably at least one of iron, nickel, aluminum, and rare earth elements.
Preferably, in step S1, the heat treatment is an aging treatment, and the Mn-Cu base alloy is subjected to the aging treatment to cause α -Mn phase to be precipitated from the alloy, wherein the temperature of the aging treatment is 300-700 ℃, and the time is 1-100 h.
During aging treatment of Mn-Cu base alloy, amplitude modulation decomposition occurs in the alloy to gradually form Mn-rich and Cu-rich micro areas, and the aging treatment is continued until α -Mn phase in the alloy is dissolved out, namely, the 'overaging treatment' occurs "
Preferably, the dealloying is electrochemical dealloying in step S2, and the composite material obtained in step S1 is immersed in an etching solution as a working electrode to perform electrochemical etching, so that the α -Mn precipitate phase is dissolved in the etching solution, thereby removing the α -Mn precipitate phase.
After the composite material is subjected to electrochemical corrosion, redundant α -Mn precipitated phase in the alloy is removed, and nano or submicron holes are replaced, so that the Mn-Cu-based porous high-damping alloy with light weight, high strength and nano or submicron size is finally obtained.
Preferably, the corrosive solution is an acid or alkali solution with the concentration of 0.001-0.5mol/L, and is preferably an HCl solution, a citric acid solution, an NaOH solution or H2SO4And (NH)4)2SO4Mixed solution, H2SO4And MnSO4Mixing the solution or NaCl solution, and cooling the corrosive liquid to 20-90 deg.C.
Preferably, the working voltage of the electrochemical corrosion is-0.2-0.4V, and the working time is 0.5-100 h.
Preferably, the Mn-Cu base alloy is obtained by smelting by a vacuum smelting method. .
Preferably, the vacuum melting method specifically includes: adding the raw materials into a medium-frequency vacuum induction furnace, and obtaining an alloy ingot through air exhaust, preheating, argon filling, melting, refining, alloying, standing, temperature adjustment, pouring and demoulding.
The invention also provides a Mn-Cu-based submicron/nano porous high-damping alloy which is prepared by the preparation method.
Preferably, the submicron/nanometer porous high damping alloy has a porosity of 50-90% and a pore size of 10nm-1000 nm.
Compared with the prior art, the Mn-Cu-based submicron/nano porous high-damping alloy disclosed by the invention overcomes the problem of high density of the traditional high-damping Mn-Cu alloy, can effectively improve the damping performance of the Mn-Cu alloy through the porosity and the high density defect around a cavity, has the advantages of light weight and high specific strength, and is very likely to play an excellent shock absorption and noise reduction role in the fields of wider application fields, particularly aerospace and the like in the future.
Meanwhile, the preparation method of the Mn-Cu-based micro-nano porous high-damping alloy disclosed by the invention can effectively overcome the problem that nano-scale or sub-micron-scale pores cannot be or are difficult to prepare in the conventional preparation methods of porous materials such as a melt foaming method, a powder metallurgy method and the like, and can efficiently prepare the Mn-Cu-based high-damping porous material with uniform pore structure and pore size distribution in nano or sub-micron scale; meanwhile, the preparation process is simple and easy to operate, time-saving and energy-saving, does not need expensive die cost, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is a microstructure diagram of a Mn-Cu based submicron/nanoporous high damping alloy prepared in example 1 of the present invention;
FIG. 2 is a microstructure diagram of a Mn-Cu based submicron/nanoporous high damping alloy prepared in example 2 of the present invention;
FIG. 3 is a diagram showing the damping performance test results of the Mn-Cu based submicron/nanoporous high damping alloy prepared in example 1 of the invention at different measurement frequencies;
FIG. 4 is a graph of the mechanical property test results of the Mn-Cu based submicron/nanoporous high damping alloy prepared in example 1 of the invention.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A Mn-Cu-based micro-nano porous high-damping alloy is prepared by the following steps:
(1) putting pure metals Mn and Cu as raw materials into a medium-frequency vacuum induction furnace, vacuumizing to below 10Pa, powering on for preheating, and continuing to pump air to keep the vacuum degree below 10Pa all the time; after the gas extraction is finished, filling argon into the vacuum chamber to enable the pressure to reach 0.005MPa, simultaneously enabling the metal raw material to be rapidly melted with the power supply power of 300kW, and standing for 15min with the power supply power of 80kW after melting down to finish refining; standing for 20min at the power of 60 kW; then, the temperature of the molten liquid is raised to rupture a conjunctiva, then pouring is started, and the pouring time is controlled within 5min to obtain an alloy ingot, namely a Mn-Cu base alloy with alloy components of 70 wt% of Mn and 30 wt% of Cu;
(2) putting the Mn-Cu-based alloy obtained in the step (1) into a vacuum heat treatment furnace, introducing argon for protection, carrying out aging treatment for 2h at 500 ℃, and cooling along with the furnace after the aging treatment is finished to obtain a composite material with submicron or nano α -Mn precipitated phase dispersed and distributed on a Mn-Cu-based alloy matrix;
(3) and (3) grinding and polishing the composite material obtained in the step (2) by using sand paper, cleaning, then soaking the composite material serving as a working electrode of an electrochemical workstation together with a counter electrode (platinum sheet) and a reference electrode (Ag/Agcl electrode) in an HCl solution with the concentration of 0.01mol/L and the temperature of 30 ℃, carrying out electrochemical corrosion treatment for 1h in a constant voltage mode at the voltage of-0.2V until the current in a current time curve approaches zero infinitely, taking out the composite material, then putting the composite material into a container containing oxygen-free deionized water for soaking and cleaning, and carrying out vacuum drying at room temperature to obtain the Mn-Cu-based submicron/nano porous high-damping alloy.
Referring to fig. 1, the porosity structure of the Mn-Cu-based submicron/nano porous high damping alloy prepared by the method is analyzed, and the porosity is as high as 70%; the structure is a submicron pore structure with the size of about 100 nm and 300 nm.
Referring to fig. 3, the internal temperature loss spectra of the prepared Mn-Cu-based submicron/nanoporous high-damping alloy at different measurement frequencies are analyzed, and the low-frequency torsional pendulum method is adopted to measure, so that the damping performance of the alloy is excellent as a whole at the frequencies of 0.5Hz, 1.0Hz, 2.0Hz and 4.0Hz, and the damping loss factor IF is changed regularly along with the temperature rise.
Referring to fig. 4, it is found that the stress-strain compression curve of the Mn — Cu-based submicron/nanoporous high-damping alloy prepared as described above is analyzed, and the overall mechanical properties of the alloy are excellent.
Example 2
A Mn-Cu-based micro-nano porous high-damping alloy is prepared by the following steps:
(1) putting pure metals Mn and Cu as raw materials into a medium-frequency vacuum induction furnace, vacuumizing to below 10Pa, powering on for preheating, and continuing to pump air to keep the vacuum degree below 10Pa all the time; after the gas pumping is finished, argon is filled into the vacuum chamber to enable the pressure to reach 0.001MPa, meanwhile, the metal raw materials are rapidly melted by power supply power of 260kW, and standing is carried out for 10min by power supply power of 100kW after melting down to finish refining; increasing the power of a power supply to 240kW, adding pure metals Fe and Al as alloy materials, smelting for 8min, and standing for 15min at the power of 80 kW; then, the temperature of the molten liquid is raised to rupture a conjunctiva, then pouring is started, and the pouring time is controlled within 7min to obtain an alloy ingot, namely Mn-Cu-based alloy with alloy components of 76 wt% of Mn, 16 wt% of Cu, 6 wt% of Fe and 2 wt% of Al;
(2) placing the Mn-Cu-based alloy obtained in the step (1) in a vacuum heat treatment furnace, introducing argon for protection, carrying out aging treatment for 1h at 700 ℃, and cooling along with the furnace after the aging treatment is finished to obtain a composite material with submicron or nano α -Mn precipitated phase dispersed and distributed on a Mn-Cu-based alloy matrix;
(3) and (3) polishing and polishing the composite material obtained in the step (2) by using sand paper, cleaning, then soaking the composite material serving as a working electrode of an electrochemical workstation together with a counter electrode (platinum sheet) and a reference electrode (Ag/Agcl electrode) in NaOH solution with the concentration of 0.5mol/L and the temperature of 70 ℃, performing electrochemical corrosion treatment for 0.5h in a constant voltage mode at the voltage of 0.4V until the current in a current time curve approaches zero infinitely, taking out the composite material, then putting the composite material into a container containing oxygen-free deionized water for soaking and cleaning, and performing vacuum drying at room temperature to obtain the Mn-Cu-based submicron/nano porous high-damping alloy.
Referring to fig. 2, the pore structure of the Mn-Cu-based submicron/nano porous high damping alloy prepared by the method is analyzed, and the porosity is as high as 50%; the structure is a nano-pore structure, and the size is about 1-70 nm.
Example 3
A Mn-Cu-based micro-nano porous high-damping alloy is prepared by the following steps:
(1) putting pure metals Mn and Cu as raw materials into a medium-frequency vacuum induction furnace, vacuumizing to below 10Pa, powering on for preheating, and continuing to pump air to keep the vacuum degree below 10Pa all the time; after the gas pumping is finished, argon is filled into the vacuum chamber to enable the pressure to reach 0.002MPa, meanwhile, the metal raw materials are rapidly melted by power supply power of 280kW, and standing is carried out for 10min by power supply power of 90kW after melting down to finish refining; increasing the power of a power supply to 200kW, adding pure metal Ni as an alloy material, smelting for 10min, and standing for 20min at the power of a power supply of 60 kW; then, the temperature of the molten liquid is raised to rupture a conjunctiva, then pouring is started, and the pouring time is controlled within 6min to obtain an alloy ingot, namely a Mn-Cu base alloy with alloy components of 80 wt% of Mn, 10 wt% of Cu and 10 wt% of Ni;
(2) putting the Mn-Cu-based alloy obtained in the step (1) into a vacuum heat treatment furnace, introducing argon for protection, carrying out aging treatment for 3 hours at the temperature of 300 ℃, and cooling along with the furnace after the aging treatment is finished to obtain a composite material with submicron or nano α -Mn precipitated phase dispersed and distributed on a Mn-Cu-based alloy matrix;
(3) grinding and polishing the composite material obtained in the step (2) by using abrasive paper, cleaning, taking the composite material as a working electrode of an electrochemical workstation, and soaking the working electrode, a counter electrode (platinum sheet) and a reference electrode (Ag/Agcl electrode) together in H with the concentration of 0.1mol/L and the temperature of 90 DEG C2SO4And (NH)4)2SO4And (3) carrying out electrochemical corrosion treatment for 5h in a constant voltage mode at 0.2V in the mixed solution until the current in a current time curve approaches zero infinitely, taking out the composite material, then putting the composite material into a container containing oxygen-free deionized water for soaking and cleaning, and carrying out vacuum drying at room temperature to obtain the Mn-Cu-based submicron/nano porous high-damping alloy.
Example 4
A Mn-Cu-based micro-nano porous high-damping alloy is prepared by the following steps:
(1) putting pure metals Mn and Cu as raw materials into a medium-frequency vacuum induction furnace, vacuumizing to below 10Pa, powering on for preheating, and continuing to pump air to keep the vacuum degree below 10Pa all the time; after the gas pumping is finished, filling argon into the vacuum chamber to enable the pressure to reach 0.003MPa, simultaneously enabling the metal raw materials to be rapidly melted with the power supply power of 260kW, and standing for 15min with the power supply power of 80kW after melting down to finish refining; increasing the power of a power supply to 200kW, adding pure metal Y as an alloy material, smelting for 10min, and standing for 15min at the power of 80 kW; then, the temperature of the molten liquid is raised to rupture a conjunctiva, then pouring is started, and the pouring time is controlled within 5-7min, so that an alloy ingot is obtained, namely a Mn-Cu base alloy with alloy components of 72 wt% of Mn, 15 wt% of Cu and 13 wt% of Y;
(2) placing the Mn-Cu-based alloy obtained in the step (1) in a vacuum heat treatment furnace, introducing argon for protection, carrying out aging treatment for 5 hours at the temperature of 600 ℃, and cooling along with the furnace after the aging treatment is finished to obtain a composite material with submicron or nano α -Mn precipitated phases dispersed and distributed on a Mn-Cu-based alloy matrix;
(3) and (3) grinding and polishing the composite material obtained in the step (2) by using sand paper, cleaning, then soaking the composite material serving as a working electrode of an electrochemical workstation together with a counter electrode (platinum sheet) and a reference electrode (Ag/Agcl electrode) in a citric acid solution with the concentration of 0.002mol/L and the temperature of 50 ℃, performing electrochemical corrosion treatment for 10 hours in a constant voltage mode at the voltage of-0.2V until the current in a current time curve approaches zero infinitely, taking out the composite material, then putting the composite material into a container containing oxygen-free deionized water for soaking and cleaning, and performing vacuum drying at room temperature to obtain the Mn-Cu-based submicron/nano porous high-damping alloy.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical scope of the present invention, and equivalents and modifications thereof should be included in the technical scope of the present invention.
Claims (10)
1. A preparation method of Mn-Cu-based submicron/nano porous high damping alloy is characterized by comprising the following steps:
s1, carrying out heat treatment on the Mn-Cu-based alloy to ensure that a α -Mn phase is precipitated from the alloy in a desolvation way, thus obtaining the composite material with submicron or nanometer α -Mn precipitated phases dispersed and distributed on the Mn-Cu-based alloy matrix;
s2, carrying out dealloying treatment on the composite material obtained in the step S1 to remove a α -Mn precipitated phase, and obtaining the Mn-Cu-based submicron/nano porous high damping alloy.
2. The method for preparing the Mn-Cu based submicron/nanometer porous high damping alloy according to claim 1, characterized in that the Mn-Cu based alloy is a binary alloy composed of manganese and copper or a multi-element alloy composed of other alloying elements besides manganese and copper, and the other alloying elements are preferably at least one of iron, nickel, aluminum and rare earth elements.
3. The method for preparing Mn-Cu based submicron/nanoporous high damping alloy according to claim 1 or 2, wherein the heat treatment is aging treatment in step S1, preferably, the Mn-Cu based alloy is subjected to aging treatment to desolventize α -Mn phase from the alloy, the temperature of the aging treatment is 300-700 ℃, and the time is 1-100 h.
4. A method for preparing a Mn-Cu based submicron/nanoporous high damping alloy according to any one of the claims 1 to 3, wherein the dealloying is electrochemical dealloying in step S2, preferably, the composite material obtained in step S1 is used as a working electrode and immersed in an etching solution for electrochemical etching, and the α -Mn precipitate phase is dissolved in the etching solution, so that the α -Mn precipitate phase is removed.
5. The method for preparing Mn-Cu based submicron/nanometer porous high damping alloy according to claim 4, characterized in that the corrosive solution is acid or alkali solution with concentration of 0.001-0.5mol/L, preferably HCl solution, citric acid solution, NaOH solution, H solution2SO4And (NH)4)2SO4Mixed solution, H2SO4And MnSO4Mixing the solution or NaCl solution, and cooling the corrosive liquid to 20-90 deg.C.
6. The method for preparing Mn-Cu based submicron/nano porous high damping alloy according to claim 4 or 5, characterized in that the working voltage of electrochemical corrosion is-0.2-0.4V, and the working time is 0.5-100 h.
7. The method for preparing the Mn-Cu based submicron/nanoporous high damping alloy according to any one of the claims 1 to 6, wherein the Mn-Cu based alloy is obtained by smelting by a vacuum smelting method.
8. The method for preparing the Mn-Cu based submicron/nanometer porous high damping alloy according to claim 7, characterized in that the vacuum melting method specifically comprises: adding the raw materials into a medium-frequency vacuum induction furnace, and obtaining an alloy ingot through air exhaust, preheating, argon filling, melting, refining, alloying, standing, temperature adjustment and pouring.
9. A Mn-Cu based submicron/nanoporous high damping alloy, which is characterized by being prepared by the preparation method of any one of claims 1 to 8.
10. The Mn-Cu based submicron/nanoporous high damping alloy according to claim 9, wherein the submicron/nanoporous high damping alloy has a porosity of 50-90% and a pore size of 10nm-1000 nm.
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| WO2023201684A1 (en) * | 2022-04-22 | 2023-10-26 | 宁德时代新能源科技股份有限公司 | Porous material and preparation method therefor, current collector, secondary battery and device |
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