CN114734042A - Si for laser additive manufacturing3N4Preparation method of/Al-8 Mg-based composite material powder - Google Patents
Si for laser additive manufacturing3N4Preparation method of/Al-8 Mg-based composite material powder Download PDFInfo
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
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- C22C32/0068—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only nitrides
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
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- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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Abstract
The invention relates to Si for laser additive manufacturing3N4The preparation method of/Al-8 Mg-based composite material powder uses pure Al, pure Mg and Si3N4The nano-ceramic particles are used as raw materials,preparing a micro-nano particle reinforced Al-8Mg alloy composite material by adopting a mechanical stirring and ultrasonic casting process, and preparing Si by a vacuum atomization method3N4A particulate reinforced aluminum matrix composite powder. The median particle diameter of the powder particles is controllable between 1 and 300 mu m, the sphericity rate is more than 94 percent, and the yield is more than or equal to 90 percent. Nanoscale Si3N4The particles are uniformly dispersed in the Al-Mg matrix, the grain structure of the composite material is uniform and fine isometric crystals, and the grain size of the composite material is about 1.6 mu m. The aluminum matrix composite powder prepared by the method has the advantages of high laser absorptivity, small size and good sphericity, and is suitable for laser additive manufacturing technology.
Description
Technical Field
The invention relates to the technical field of materials, in particular to Si for laser additive manufacturing3N4A preparation method of/Al-8 Mg-based composite material powder.
Background
The rapid development in the fields of modern aviation, aerospace and automobile industries puts higher requirements on the comprehensive mechanical properties of metal structural materials, such as higher specific strength, specific modulus, better fatigue resistance, corrosion resistance and the like. And any single material is difficult to meet the improvement of comprehensive performance. Under such circumstances, the generation and application of Metal Matrix Composites (MMCs) are becoming important subjects for scientific research. At present, the requirements of the equipment manufacturing industry such as large airplanes and the like on large, precise and complex-structure light, high-strength and high-toughness metal-based composite material components are more and more urgent, so as to meet the requirements of the equipment manufacturing industry on high performance, high reliability, high economy and high environmental protection. The laser additive manufacturing technology is gaining more and more favor in the industry due to the advantages of shorter production period, better personalized customization, more resource saving and the like.
In the field of aluminum alloy laser additive manufacturing, in view of the lower laser absorption rate of aluminum alloy, the aluminum alloy powder suitable for laser additive manufacturing is limited to an Al-Si system at present, and the application of aluminum-based materials in the field of laser additive manufacturing is severely limited. And the microstructure of the aluminum alloy section bar manufactured by the additive presents a typical coarse columnar grain structure, the hot cracking tendency is serious, the plasticity of the material is poor, and the anisotropy is obvious. At present, the methods for preparing prealloyed powder are mainly atomization method and rotary electrode method. Parts prepared by using the commercial powder have high dimensional accuracy and are applied to the fields of aerospace, medical treatment and the like. But the prepared part is easy to generate defects of higher residual stress, micron-level cracks, holes and the like, so that the fatigue strength, plasticity and toughness of the material are reduced, and the part has low production yield, insufficient reliability and high cost.
Disclosure of Invention
The invention aims to provide Si for laser additive manufacturing3N4A preparation method of Al-8 Mg-based composite material powder.
The invention realizes the purpose through the following technical scheme: si for laser additive manufacturing3N4The preparation method of the/Al-8 Mg-based composite material powder comprises the following steps:
(1) heating and melting industrial pure aluminum, then adding industrial pure magnesium according to the component design in proportion, covering with a high-temperature covering agent, and then heating;
(2) mixing nano-sized Si3N4Drying the ceramic particles and then adding the dried ceramic particles into the melt obtained in the step (1);
(3) adding a harmless aluminum alloy refining agent into the melt for degassing and refining, and removing the surface scum;
(4) mechanically stirring the mixed melt, wherein the electric power of a stirrer is 500w, the rotating speed is 1000r/min, and the stirring time is 30 min;
(5) carrying out ultrasonic treatment on the mixed melt in the step (4), and adopting an ultrasonic wave generator with the power of 500w and the frequency of 20kHz, wherein the ultrasonic time is 30 min;
(6) casting the composite material melt after ultrasonic treatment into a cast ingot;
(7) and carrying out vacuum gas atomization on the composite material cast ingot to prepare composite material powder, and collecting and vacuum-packaging the prepared composite powder.
Further, the covering agent adopted in the step (1) is JZF-03 type high-temperature covering agent, and the temperature is raised to 650-950 ℃.
Further, Si added in the step (2)3N4The ceramic particle size is nanometer, and the average particle size is less than 100 nm.
Further, the stirring head in the step (4) is a high-strength graphite stirring head.
Further, the diameter of the nozzle of the vacuum gas atomization process adopted in the step (7) is 3mm, the nozzle is in the shape of a Lava tube, and the atomization air pressure is 3 MPa.
Furthermore, the median particle diameter of the powder is controllable between 1 and 300 mu m, the sphericity rate is more than 94 percent, the yield is more than or equal to 80 percent, and the nano-Si is3N4The particles are uniformly dispersed in the aluminum matrix, the mass fraction of the particles is 0.5-30%, and the grain structure of the composite material is uniform and fine isometric crystals.
Further, the aluminum matrix composite powder has a laser absorptivity of > 30%.
Compared with the prior art, the Si for laser additive manufacturing of the invention3N4The preparation method of the/Al-8 Mg-based composite material powder has the beneficial effects that: effectively combines the advantages of mechanical stirring and ultrasonic oscillation, and the method adds the added nano ceramic particles to prepare the nano particle reinforced aluminum-based composite material powder, and the nano Si is uniformly dispersed and distributed in the composite material powder3N4The particles can greatly improve the strength of the material, effectively improve the laser absorption rate of the powder and greatly expand the material application range of laser additive manufacturing of the aluminum-based material.
The composite material powder is used for laser additive manufacturing, compared with the traditional aluminum alloy system powder, the strength and the plasticity of the prepared material are higher, and the nano Si powder is used for preparing the composite material3N4The heterogeneous nucleation of the particles can obtain uniform and fine isometric crystals. Because the nano Si is uniformly dispersed and distributed in the composite material tissue3N4The existence of particles and fine isometric crystals, the laser additive manufactured by the method of the invention can simultaneously have high strength and high plasticity.
Drawings
FIG. 1 is a schematic view of a mechanical stirring apparatus.
Fig. 2 is a schematic structural diagram of an ultrasonic oscillation device.
Fig. 3 is a schematic diagram of the powder structure.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
Experiment with high purity Al, industrial pure Mg, Si3N4The granules were prepared with 2 wt.% Si as the starting material3N4Reinforced Al-8 Mg-based composite material. Firstly, putting high-purity Al into a crucible to be melted, heating to 790 ℃, then adding industrial pure Mg according to component design, and covering with JZF-03 type high-temperature covering agent; mixing Si3N4Drying, adding the dried powder into the melt obtained in the step (1), and adding a JZJ type harmless aluminum alloy refining agent into the melt for degassing and refining; then, mechanically stirring at the stirring speed of 1000r/min for 30 min; then carrying out ultrasonic oscillation on the composite melt, wherein the ultrasonic frequency is 20kHz, and the ultrasonic time is 30 min; standing at 750 deg.C for 15min, and gas atomizing to obtain powder. The gas atomization process comprises the following steps: the solution temperature is 900 ℃, N is used2The gas is protected and atomized, the air pressure is 3MPa, and the diameter of a nozzle is 3 mm. The average diameter of the prepared powder is 30 microns, the sphericity rate is more than 94 percent, the yield is more than or equal to 80 percent, and Si is3N4Particle content 2 wt.%, composite powder grain average size 2.0 microns. The laser absorption rate was 50%.
Example 2
Experiment with high purity Al, industrial pure Mg, Si3N4The granules were prepared with 4 wt.% Si as the starting material3N4Reinforced Al-8 Mg-based composite material. Firstly, putting high-purity Al into a crucible to be melted, heating to 790 ℃, then adding industrial pure Mg according to component design, and covering with JZF-03 type high-temperature covering agent; mixing Si3N4Drying, adding the dried powder into the melt obtained in the step (1), and adding a JZJ type harmless aluminum alloy refining agent into the melt for degassing and refining; then, mechanically stirring at the stirring speed of 1000r/min for 30 min; then carrying out ultrasonic oscillation on the composite melt, wherein the ultrasonic frequency is 20kHz, and the ultrasonic time is 30 min; standing at 750 deg.C for 15min, and gas atomizing to obtain powder. The gas atomization process comprises the following steps: the solution temperature is 900 ℃, N is used2The gas is protected and atomized, the air pressure is 3MPa, and the diameter of a nozzle is 3 mm. The average diameter of the prepared powder is 30 microns, the sphericity rate is more than 94 percent, the yield is more than or equal to 80 percent, and Si is3N4Particle content 4 wt.%, composite powder grain average size 2.0 microns. The laser absorption rate was 50%.
Example 3
Experiment is highPure Al, industrial pure Mg, Si3N4The granules were made up of 6 wt.% Si3N4Reinforced Al-8 Mg-based composite material. Firstly, putting high-purity Al into a crucible to be melted, heating to 790 ℃, then adding industrial pure Mg according to component design, and covering with JZF-03 type high-temperature covering agent; mixing Si3N4Drying, adding the dried powder into the melt obtained in the step (1), and adding a JZJ type harmless aluminum alloy refining agent into the melt for degassing and refining; then, mechanically stirring at the stirring speed of 1000r/min for 30 min; then carrying out ultrasonic oscillation on the composite melt, wherein the ultrasonic frequency is 20kHz, and the ultrasonic time is 30 min; standing at 750 deg.C for 15min, and gas atomizing to obtain powder. The gas atomization process comprises the following steps: the temperature of the solution is 900 ℃, N is used2The gas is protected and atomized, the air pressure is 3MPa, and the diameter of a nozzle is 3 mm. The average diameter of the prepared powder is 30 micrometers, the sphericity rate is more than 94 percent, the yield is more than or equal to 80 percent, and the Si content is3N4Particle content 6 wt.%, composite powder grain average size 2.0 microns. The laser absorption rate was 50%.
Example 4
Experiment with high purity Al, industrial pure Mg, Si3N4The granules were prepared with 8 wt.% Si as the starting material3N4Reinforced Al-8 Mg-based composite material. Firstly, putting high-purity Al into a crucible to be melted, heating to 790 ℃, then adding industrial pure Mg according to component design, and covering with JZF-03 type high-temperature covering agent; mixing Si3N4Drying, adding the dried powder into the melt obtained in the step (1), and adding a JZJ type harmless aluminum alloy refining agent into the melt for degassing and refining; then, mechanically stirring at the stirring speed of 1000r/min for 30 min; then carrying out ultrasonic oscillation on the composite melt, wherein the ultrasonic frequency is 20kHz, and the ultrasonic time is 30 min; standing at 750 deg.C for 15min, and gas atomizing to obtain powder. The gas atomization process comprises the following steps: the temperature of the solution is 900 ℃, N is used2Gas protection and gas atomization are carried out, the air pressure is 3MPa, and the diameter of a nozzle is 3 mm. The average diameter of the prepared powder is 30 microns, the sphericity rate is more than 94 percent, the yield is more than or equal to 80 percent, and Si is3N4Particle content 8 wt.%, composite powder grain average size 1.5 microns. The laser absorption rate was 50%.
Example 5
Experiments are carried out on high-purity Al, industrial pure Mg, Al-Mn intermediate alloy and Si3N4The granules were made up of 4 wt.% Si3N4Reinforced Al-8Mg-0.1 Mn-based composite material. Firstly, putting high-purity Al into a crucible to be melted, heating to 790 ℃, then adding industrial pure Mg and Al-Mn intermediate alloy according to component design, and covering with JZF-03 type high-temperature covering agent; mixing Si3N4Drying, adding the dried powder into the melt obtained in the step (1), and adding a JZJ type harmless aluminum alloy refining agent into the melt for degassing and refining; then, mechanically stirring at the stirring speed of 1000r/min for 30 min; then carrying out ultrasonic oscillation on the composite melt, wherein the ultrasonic frequency is 20kHz, and the ultrasonic time is 30 min; standing at 750 deg.C for 15min, and gas atomizing to obtain powder. The gas atomization process comprises the following steps: the temperature of the solution is 900 ℃, N is used2Gas protection and gas atomization are carried out, the air pressure is 3MPa, and the diameter of a nozzle is 3 mm. The average diameter of the prepared powder is 30 microns, the sphericity rate is more than 94 percent, the yield is more than or equal to 80 percent, and Si is3N4Particle content 4 wt.%, composite powder grain average size 2.0 microns. The laser absorption rate was 50%.
The inside of furnace body 104 is equipped with graphite crucible 103 for holding fuse-element 102, contains powder granule 105 in the fuse-element 102, and fuse-element 102 top forms oxide skin 101 with air contact part, stirs the fuse-element through stirring head 106, and ultrasonic generator 107 carries out ultrasonic oscillation to the fuse-element.
The method effectively combines the advantages of mechanical stirring and ultrasonic oscillation, and the nano-particle reinforced aluminum-based composite material powder is prepared by adding the added nano-ceramic particles through the method, wherein nano-Si is uniformly dispersed and distributed in the composite material powder3N4The particles can greatly improve the strength of the material, effectively improve the laser absorption rate of the powder and greatly expand the material application range of laser additive manufacturing of the aluminum-based material.
The composite material powder is used for laser additive manufacturing, compared with the traditional aluminum alloy system powder, the strength and the plasticity of the prepared material are higher, and the nano Si powder is used for preparing the composite material3N4Heterogeneous nucleation of particles to obtain uniform and fine equiaxed particlesAnd (4) crystallizing. Because the nano Si is uniformly dispersed and distributed in the composite material tissue3N4The existence of particles and fine isometric crystals, the laser additive manufactured aluminum matrix composite material part prepared by the method has high strength and high plasticity.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. Si for laser additive manufacturing3N4The preparation method of the/Al-8 Mg-based composite material powder is characterized by comprising the following steps of:
(1) heating and melting industrial pure aluminum, then adding industrial pure magnesium according to the component design in proportion, covering with a high-temperature covering agent, and then heating;
(2) mixing nano-sized Si3N4Drying the ceramic particles and then adding the dried ceramic particles into the melt obtained in the step (1);
(3) adding a harmless aluminum alloy refining agent into the melt for degassing and refining, and removing the surface scum;
(4) mechanically stirring the mixed melt, wherein the electric power of a stirrer is 500w, the rotating speed is 1000r/min, and the stirring time is 30 min;
(5) carrying out ultrasonic treatment on the mixed melt in the step (4), and adopting an ultrasonic wave generator with the power of 500w and the frequency of 20kHz, wherein the ultrasonic time is 30 min;
(6) casting the composite material melt after ultrasonic treatment into a cast ingot;
(7) and carrying out vacuum gas atomization on the composite material cast ingot to prepare composite material powder, and collecting and vacuum-packaging the prepared composite powder.
2. Si for laser additive manufacturing according to claim 13N4The preparation method of the/Al-8 Mg-based composite material powder is characterized by comprising the following steps: the covering agent adopted in the step (1) is JZF-03 type high-temperature covering agent, and the temperature is raised to 650-950 ℃.
3. Si for laser additive manufacturing according to claim 13N4The preparation method of the/Al-8 Mg-based composite material powder is characterized by comprising the following steps: si added in the step (2)3N4The ceramic particle size is nanometer, and the average particle size is less than 100 nm.
4. Si for laser additive manufacturing according to claim 13N4The preparation method of the/Al-8 Mg-based composite material powder is characterized by comprising the following steps: and (4) the stirring head in the step (4) is a high-strength graphite stirring head.
5. Si for laser additive manufacturing according to claim 13N4The preparation method of the/Al-8 Mg-based composite material powder is characterized by comprising the following steps: the diameter of the nozzle of the vacuum gas atomization process adopted in the step (7) is 3mm, the nozzle is in the shape of a Lava tube, and the atomization air pressure is 3 MPa.
6. Si for laser additive manufacturing according to claim 13N4The preparation method of the/Al-8 Mg-based composite material powder is characterized by comprising the following steps: the powder is prepared fromThe final median particle diameter is controllable between 1 and 300 mu m, the sphericity rate is more than 94 percent, the yield is more than or equal to 80 percent, and the nano-Si is3N4The particles are uniformly dispersed in the aluminum matrix, the mass fraction of the particles is 0.5-30%, and the grain structure of the composite material is uniform and fine isometric crystals.
7. Si for laser additive manufacturing according to claim 13N4The preparation method of the/Al-8 Mg-based composite material powder is characterized by comprising the following steps: the aluminum-based composite material powder has laser absorptivity>30％。
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| WO2025022242A1 (en) * | 2023-07-21 | 2025-01-30 | NIWC - Neue Innovative Werkstoffe Chemnitz GmbH | Method for producing a metal-matrix composite powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2025022242A1 (en) * | 2023-07-21 | 2025-01-30 | NIWC - Neue Innovative Werkstoffe Chemnitz GmbH | Method for producing a metal-matrix composite powder |
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