CN112743092A - Method for refining 3D printing aluminum alloy crystal grains and improving thermal conductivity of aluminum alloy crystal grains - Google Patents
Method for refining 3D printing aluminum alloy crystal grains and improving thermal conductivity of aluminum alloy crystal grains Download PDFInfo
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Abstract
The invention discloses a method for refining 3D printing aluminum alloy grains and improving the thermal conductivity of the aluminum alloy grains. The method comprises the following steps: (1) carrying out high-temperature heat treatment on the MXene two-dimensional nano-layer sheet material; (2) ball milling MXene subjected to heat treatment and a ball milling medium; (3) mixing MXene subjected to ball milling treatment with aluminum alloy spherical powder in a colloid manner; (4) grinding and screening after drying treatment to obtain composite powder for selective laser melting forming; (5) and (4) carrying out selective laser melting on the composite powder obtained in the step (4) to form an aluminum alloy, and naturally cooling after forming is finished to obtain an aluminum alloy formed part. The MXene two-dimensional nano-layer sheet material is used as a nano additive to promote grain refinement; meanwhile, the characteristics of high thermal conductivity and large adhesion area of the lamellar structure are utilized to improve the thermal conductivity of the alloy.
Description
Technical Field
The invention belongs to the technical field of 3D printing of metal materials, and particularly relates to a method for refining 3D printing aluminum alloy grains and improving the thermal conductivity of the aluminum alloy grains.
Background
Along with the strong increase of the requirements of light weight and structural function integration, the application of the aluminum alloy is more and more extensive. In particular to the fields of electronic communication, aerospace and aviation and the like, the requirements on the heat-conducting property and the comprehensive mechanical property of the aluminum alloy material are higher and higher. But for some special-shaped parts and complex thin-wall structural parts, the traditional processing method is difficult to prepare. Selective Laser Melting (SLM) technology employs focused Laser beams to selectively melt metal or alloy powders layer by layer and build up them into a metallurgically bonded, dense-structure solid. Because the process is simple and the size precision of the formed part is high, the selective laser melting forming technology is the most promising new method for preparing the aluminum alloy part.
However, the aluminum alloy has high reflectivity to laser, contains more elements which are easy to burn, has a wide solidification temperature range, has high difficulty in laser printing and forming, and is easy to form coarse columnar crystals and hot cracks. In literature research (J.H. Martin, B.D. Yahata, J.M. Hundley, et Al Nature, 549(2017)365-2To refine the SLM-formed 7075 aluminum alloy grains. Although the problem of heat cracking is solved to a certain extent, the mechanical property is low due to the fact that a plurality of pores exist inside a formed part, wherein the highest tensile strength is only 417MPa, and the tensile strength is far lower than that of a 7075 aluminum alloy material prepared by a traditional ingot metallurgy method (more than 550 MPa). Meanwhile, the method has no obvious effect on improving the thermal conductivity.
On the other hand, the thermal conductivity of the common aluminum alloy is low, and the thermal conductivity can not meet the requirement of industrial development from 96W/(m.K) of the common ADC12 to 175W/(m.K) of AlSi 6. In order to improve the heat-conducting property of the aluminum alloy, most of the high-heat-conductivity aluminum alloy materials on the market improve the heat conductivity by controlling the element content and the forming process. Patent CN109022856A discloses a production process of an aluminum alloy ingot with high thermal conductivity, which prepares an aluminum alloy product with high thermal conductivity by controlling the melting temperature, adding a refining agent, performing light treatment and the like. However, this method is complicated and not suitable for 3D printing technology.
Therefore, the existing 3D printing aluminum alloy is difficult to meet the requirements of grain refinement and heat-conducting property improvement at the same time.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for refining 3D printing aluminum alloy crystal grains and improving the thermal conductivity of the aluminum alloy crystal grains.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for refining 3D printing aluminum alloy grains and improving the thermal conductivity of the aluminum alloy grains comprises the following steps:
(1) carrying out high-temperature heat treatment on the MXene two-dimensional nano-layer sheet material;
(2) performing ball milling treatment on the MXene two-dimensional nano-layer sheet material subjected to heat treatment and a ball milling medium;
(3) mixing the MXene two-dimensional nano-layer sheet material subjected to ball milling treatment with a dispersant solution according to a certain proportion, and performing ultrasonic dispersion treatment to obtain a suspension;
(4) adding aluminum alloy powder into the suspension, carrying out ultrasonic oscillation, stirring and standing;
(5) filtering and washing the mixed solution obtained in the step (4), drying, grinding and screening to obtain composite powder for selective laser melting forming;
(6) and carrying out selective laser melting on the composite powder to form the aluminum alloy, and naturally cooling after forming to obtain an aluminum alloy formed part.
Further, in the step (1), the layer number of the MXene two-dimensional nano-layer sheet material is within 5.
Further, in the step (1), the heat treatment specifically includes: heating to 1200 ℃ at the speed of 10-20 ℃/min, preserving the heat for 2-4h, and naturally cooling to room temperature.
Further, in the step (2), the mass ratio of the ball milling medium to the MXene two-dimensional nano-layer sheet material is 5:1, the rotation speed of the ball milling treatment is 100-.
Further, in the step (3), the dispersant solution is prepared by adopting a liquid dispersant or mixing a solid dispersant and an organic solvent, wherein the organic solvent is absolute ethyl alcohol.
Further, in the step (3), the ratio of the MXene two-dimensional nano-layer sheet material to the dispersant solution is 1-2 g: 200 ml.
Further, in the step (4), the aluminum alloy powder particles are spherical or nearly spherical, and the particle size of the powder is 15-63 μm.
Further, in the step (4), the mass ratio of the aluminum alloy powder to the MXene two-dimensional nano-layer sheet material is 90-99: 1 was added to the suspension.
Further, in the step (4), the ultrasonic oscillation time is 30-60min, an electric stirrer is adopted for stirring, the stirring speed is 2000-3000rpm, the stirring time is 15-30min, and the standing time is 24-48 h.
Further, in the step (5), the grinding time is 30min, and the mixture is sieved by a 250M sieve.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) compared with other existing 3D printing aluminum alloys, MXene two-dimensional nano materials are introduced into the alloy used in the method and serve as nucleating agents, so that original coarse dendritic crystals are converted into isometric crystals with higher heat crack resistance, the effect of grain refinement is achieved on the alloy, and cracks in the forming process are reduced. And because of fine-grain reinforcement, the performance of the formed piece is enhanced to a certain extent.
(2) Compared with the common MXene two-dimensional material, the MXene two-dimensional material used by the method has higher actual heat conductivity value because the functional groups such as-OH, -F and the like on the surface of the MXene two-dimensional material are removed through the high-temperature heat treatment process and the high-temperature heating.
(3) Compared with the common grain refining alloy containing heterogeneous nucleating agent, the MXene two-dimensional nano material introduced into the alloy used in the method has smaller reaction with a matrix in SLM forming, can retain the form, increases the contact area with powder, forms a heat-conducting network under a certain amount and plays a role in enhancing the heat-conducting property of the alloy, such as a carbon tube. The conventional grain refiner does not have the effect of enhancing thermal conductivity.
(4) The aluminum alloy composite powder used by the method is prepared by mixing colloid, compared with the existing mechanical mixing method, the agglomeration can be well removed, the wetting between MXene and powder particles is facilitated, and meanwhile, the particle size of the composite powder is not obviously increased compared with that of the original powder.
Drawings
Fig. 1 is a flowchart of a method provided in embodiment 1 of the present invention.
FIG. 2 shows ball-milled Ti prepared in example 1 of the present invention2C-MXene morphology.
Fig. 3 shows the macro morphology of 7075 aluminum alloy powder provided in example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples. The exemplary embodiments and descriptions of the present invention are provided only for explaining the present invention and not for limiting the present invention.
The invention provides a method for refining 3D printing aluminum alloy grains and improving the thermal conductivity of the aluminum alloy grains, which utilizes 3D printing aluminum alloy powder and MXene two-dimensional nano-layer sheet materials. MXene is a novel two-dimensional layer sheet material, has the advantage of high ion migration speed due to the surface characteristics, has extremely high heat conductivity coefficient, serves as heterogeneous nucleation particles in a 3D printing laser beam melt, and can effectively achieve the effects of refining grains and improving mechanical properties. But the actual thermal conductivity is significantly reduced due to the surface functional groups such as-OH, -F, etc. introduced by the preparation process. Therefore, the MXene two-dimensional material used in the invention is subjected to high-temperature heat treatment to remove free water, adsorbed gas molecules and hydroxyl groups on the surface at high temperature, so that the actual heat conductivity coefficient is improved; and (3) crushing the mixture into nano sheets by high-energy ball milling, and further removing surface functional groups. Meanwhile, the mixed powder is prepared by adopting a colloid mixing method, so that agglomeration can be well removed, wetting between MXene and powder particles is facilitated, and the particle size of the composite powder is not obviously increased compared with that of the original powder.
The method comprises the following specific steps:
(1) placing MXene two-dimensional nano-layer sheet materials (the number of layers is less than or equal to five) into a vacuum tube furnace for high-temperature heat treatment, raising the temperature to 1200 ℃ at the speed of 10 ℃/min, then preserving the heat for 2h, and then naturally cooling to room temperature.
(2) Adding the MXene two-dimensional nano lamellar material after heat treatment and a ball-milling medium into a vacuum ball-milling tank under the protection of inert gas, sealing and carrying out ball-milling treatment, and grinding the MXene two-dimensional nano lamellar material into discrete nano lamellar with smaller volume in the repeated impact process with a milling ball and the inner wall of the ball-milling tank;
(3) mixing the MXene two-dimensional nano-layer sheet material subjected to ball milling treatment with a dispersant solution according to a certain proportion, and performing ultrasonic dispersion treatment for 30 min;
(4) adding aluminum alloy powder (spherical or nearly spherical, the particle size of the powder is 15-63 μm) into the suspension according to a certain proportion, ultrasonically oscillating, stirring by using an electric stirrer, and then standing;
(5) filtering and washing the mixed solution obtained in the step (4), drying the mixed solution in a vacuum drying oven, and then grinding and screening to obtain composite powder for selective laser melting forming;
(6) and (3) under the protection of argon with the purity of 99.99%, performing selective laser melting forming on the composite powder obtained in the step (5) to ensure that the oxygen content in the working cavity is lower than 300ppm, and naturally cooling to obtain the MXene refined aluminum alloy member.
Example 1
As shown in fig. 1, the specific steps of this embodiment are as follows:
(1) spherical aluminum alloy powder with the grain diameter of 15-63 mu m is selected.
(2) Mixing Ti2Uniformly spreading the C-MXene two-dimensional nano-layer sheet material in a crucible, placing the crucible in a vacuum tube furnace, vacuumizing, heating to 1200 ℃ at the speed of 10 ℃/min, and keeping the temperatureThe temperature is kept for 2h, and then the mixture is naturally cooled to the room temperature.
(3) Ti obtained by heat treatment2Adding the C-MXene two-dimensional nano lamellar material and a ball-milling medium into a vacuum ball-milling tank under the protection of inert gas, sealing and carrying out ball-milling treatment, wherein the ball-milling rotation speed is 120r/min, the ball-milling treatment time is 4h, and the mass ratio of ball materials is 5: 1. Ti is repeatedly impacted with the inner wall of the ball milling pot and the grinding ball2The C-MXene two-dimensional material is ground into discrete nanoplatelets of smaller volume as shown in fig. 2.
(4) Subjecting the Ti subjected to ball milling treatment2Mixing the C-MXene two-dimensional nano-layer sheet material and a liquid dispersant methyl pyrrolidone (NMP) according to the weight ratio of 1 g: mixing at a ratio of 100ml, and performing ultrasonic dispersion treatment to obtain suspension with ultrasonic treatment time of 30 min.
(5) And (2) mixing the aluminum alloy powder obtained in the step (1) with MXene two-dimensional nano-layer sheet material in a mass ratio of 99: 1 is added into the prepared suspension liquid and is subjected to ultrasonic oscillation for 30min, and an electric stirrer is adopted for stirring at the speed of 2000rpm for 20min to enable Ti to be stirred2The C-MXene two-dimensional nano-layer sheet material is uniformly dispersed and attached to the aluminum alloy matrix powder and then stands for 24 hours.
(6) Filtering the mixed solution after uniform mixing, washing the solid obtained by filtering with absolute ethyl alcohol, drying in a vacuum drying oven at 60 ℃ for 20h, taking out, grinding for 30min, and sieving powder with the particle size of below 250M for selective laser melting forming.
Example 2
The specific steps of this example are as follows:
(1) spherical 7075 aluminum alloy powder with the grain diameter of 15-63 μm is selected, and the macro morphology of the powder is shown in figure 3.
(2) Mixing Ti3C2Uniformly spreading the MXene two-dimensional nano-layer sheet material in a crucible, placing the crucible in a vacuum tube furnace, vacuumizing, heating to 1200 ℃ at the speed of 10 ℃/min, preserving the temperature for 2h, and naturally cooling to room temperature.
(3) Ti obtained by heat treatment3C2Adding the-MXene two-dimensional nano lamellar material and a ball-milling medium into a vacuum ball-milling tank under the protection of inert gas, sealing and carrying out ball-milling treatment, wherein ballsThe grinding speed is 120r/min, the ball milling treatment time is 4h, and the mass ratio of the ball materials is 5: 1. Ti is repeatedly impacted with the inner wall of the ball milling pot and the grinding ball3C2-MXene two-dimensional nanolaminate material ground into discrete nanoplatelets of smaller volume.
(4) Subjecting the Ti subjected to ball milling treatment3C2Mixed solution of MXene two-dimensional nano lamellar material and solid dispersant polyvinyl pyrrolidone (PVP) is mixed according to the proportion of 1 g: 100ml of the mixture is subjected to ultrasonic dispersion treatment to obtain suspension, the ultrasonic time is 30min, and the mixed solution of the solid dispersing agent is 25ml of absolute ethyl alcohol and 0.1g of PVP.
(5) And (2) mixing the aluminum alloy powder obtained in the step (1) with MXene two-dimensional nano-layer sheet material in a mass ratio of 99: 1 adding into the prepared suspension, and performing ultrasonic oscillation for 30min while stirring with electric stirrer at 2000rpm for 20min to obtain Ti3C2The MXene two-dimensional nano-layer sheet material is uniformly dispersed and attached to the aluminum alloy matrix powder and then stands for 24 hours.
(6) Filtering the mixed solution after uniform mixing, washing the solid obtained by filtering with absolute ethyl alcohol, drying in a vacuum drying oven at 60 ℃ for 20h, taking out, grinding for 30min, and sieving powder with the particle size of below 250M for selective laser melting forming.
To demonstrate the effectiveness of the method of the present invention, the procedure of example 1 was repeated as a comparative example, but with AlSi10Mg aluminum alloy powder as the starting material and no MXene two-dimensional nano-ply material added.
The aluminum alloy composite powder prepared in examples 1 and 2 and the composite powder prepared in the comparative example were processed and formed by a suitable 3D printing process on a selective laser melting and forming device under the protection of argon gas with a purity of 99.99%, and the oxygen content in the working chamber was guaranteed to be less than 300ppm during forming. The printed samples were processed into test specimens and tested for thermal conductivity, tensile strength and elongation, with the results shown in table 2:
TABLE 2 results of thermal conductivity, tensile strength and elongation
| Coefficient of thermal conductivity (W/m k) | Tensile strength (MPa) | Elongation (%) | |
| Example 1 | 216 | 493 | 9.8 |
| Example 2 | 235 | 510 | 11.2 |
| Comparative example | 119 | 412 | 6.3 |
As can be seen from the results in table 2, compared with the 3D printed aluminum alloy formed part of the comparative example without the MXene two-dimensional nano-layer sheet material, the aluminum alloy of the present invention has more excellent thermal conductivity, and has higher tensile strength and elongation due to grain refinement.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A method for refining 3D printing aluminum alloy grains and improving the thermal conductivity of the aluminum alloy grains is characterized by comprising the following steps:
(1) carrying out high-temperature heat treatment on the MXene two-dimensional nano-layer sheet material;
(2) performing ball milling treatment on the MXene two-dimensional nano-layer sheet material subjected to heat treatment and a ball milling medium;
(3) mixing the MXene two-dimensional nano-layer sheet material subjected to ball milling treatment with a dispersant solution according to a certain proportion, and performing ultrasonic dispersion treatment to obtain a suspension;
(4) adding aluminum alloy powder into the suspension, carrying out ultrasonic oscillation, stirring and standing;
(5) filtering and washing the mixed solution obtained in the step (4), drying, grinding and screening to obtain composite powder for selective laser melting forming;
(6) and carrying out selective laser melting on the composite powder to form the aluminum alloy, and naturally cooling after forming to obtain an aluminum alloy formed part.
2. The method for refining the grains and improving the thermal conductivity of the 3D printed aluminum alloy according to claim 1, wherein the number of MXene two-dimensional nano-layer sheets in step (1) is within 5.
3. The method for refining the crystal grains and improving the thermal conductivity of the 3D printed aluminum alloy as claimed in claim 1, wherein in the step (1), the heat treatment is specifically as follows: heating to 1200 ℃ at the speed of 10-20 ℃/min, preserving the heat for 2-4h, and naturally cooling to room temperature.
4. The method for refining the 3D printing aluminum alloy crystal grains and improving the thermal conductivity thereof as claimed in claim 1, wherein in the step (2), the mass ratio of the ball milling medium to the MXene two-dimensional nano-layer sheet material is 5:1, the rotation speed of the ball milling treatment is 100-.
5. The method for refining the crystal grains of the 3D printed aluminum alloy and improving the thermal conductivity of the crystal grains of the 3D printed aluminum alloy as claimed in claim 1, wherein in the step (3), the dispersant solution is prepared by adopting a liquid dispersant or mixing a solid dispersant with an organic solvent, and the organic solvent is absolute ethyl alcohol.
6. The method for refining the crystal grains and improving the thermal conductivity of the 3D printed aluminum alloy according to claim 1, wherein in the step (3), the ratio of the MXene two-dimensional nano-layer sheet material to the dispersant solution is 1-2 g: 200 ml.
7. The method for refining the crystal grains and improving the thermal conductivity of the 3D printed aluminum alloy as claimed in claim 1, wherein in the step (4), the aluminum alloy powder particles are spherical or nearly spherical, and the particle diameter of the powder is 15-63 μm.
8. The method for refining the crystal grains and improving the thermal conductivity of the 3D printed aluminum alloy according to claim 1, wherein in the step (4), the mass ratio of the aluminum alloy powder to the MXene two-dimensional nano-layer sheet material is 90-99: 1 was added to the suspension.
9. The method for refining the 3D printing aluminum alloy grains and improving the thermal conductivity thereof as claimed in claim 1, wherein in the step (4), the ultrasonic oscillation time is 30-60min, an electric stirrer is adopted for stirring, the stirring speed is 2000-3000rpm, the stirring time is 15-30min, and the standing time is 24-48 h.
10. The method for refining the grains and improving the thermal conductivity of the 3D printed aluminum alloy as claimed in claim 1, wherein in the step (5), the grinding time is 30min and the grains are sieved by a 250M screen.
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| CN114941093A (en) * | 2022-06-30 | 2022-08-26 | 南京工业职业技术大学 | MXene/CNT reinforced aluminum alloy and preparation method thereof |
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| US20060198754A1 (en) * | 2005-03-03 | 2006-09-07 | The Boeing Company | Method for preparing high-temperature nanophase aluminum-alloy sheets and aluminum-alloy sheets prepared thereby |
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| CN111472033A (en) * | 2020-04-22 | 2020-07-31 | 哈尔滨工业大学 | MXene reinforced aluminum alloy wire with composite coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114941093A (en) * | 2022-06-30 | 2022-08-26 | 南京工业职业技术大学 | MXene/CNT reinforced aluminum alloy and preparation method thereof |
| CN114941093B (en) * | 2022-06-30 | 2023-06-23 | 南京工业职业技术大学 | MXene/CNT reinforced aluminum alloy and preparation method thereof |
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