CN110484783B - Aluminum-rare earth alloy powder and preparation method and application thereof - Google Patents
Aluminum-rare earth alloy powder and preparation method and application thereof Download PDFInfo
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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
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- 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
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Abstract
The invention provides aluminum-rare earth (Al-Re) alloy powder and a preparation method and application thereof. The Al-Re alloy powder comprises the following components in percentage by mass: re: 8.0-15.0%, Mn: 0.1-2.0%, Fe: 0.2-4.0%; more preferably, the coating also comprises 1.0-10.0% of TiB2Reinforcing the particles. The preparation method comprises mixing pure aluminum and TiB2Heating and smelting the/Al composite material master batch, sequentially adding Al-Re intermediate alloy, Al-Mn intermediate alloy and Al-Fe intermediate alloy into the melt, degassing, refining and then carrying out gas atomization to obtain the Al-Re alloy powder. The prepared Al-Re alloy powder has higher laser absorption rate and is suitable for laser additive manufacturing technology.
Description
Technical Field
The invention belongs to the technical field of material preparation, relates to Al-Re alloy powder, and more particularly relates to aluminum-rare earth (Al-Re) alloy powder, a preparation method and application thereof, which can be used for laser additive manufacturing.
Background
With the development of science and technology, the requirements of the fields of aerospace, weapon manufacturing and the like on materials are increasingly strict. In particular, structural materials for equipment in the field of automobile and aircraft engines not only require the materials to have precise and complex overall structures, but also require the materials to have relatively high mechanical properties under normal temperature and high temperature service. In various material forming technologies, compared with the traditional casting and extruding process, the laser additive manufacturing technology can form structural parts with complex shapes and can greatly improve the mechanical property of metal components. Therefore, laser additive manufacturing technology is becoming a key molding technology in the field of new material preparation and manufacturing.
However, aluminum alloy samples obtained by laser additive manufacturing and forming often have many defects due to the defects of poor flowability, high laser reflectivity, easy oxidation and the like of aluminum, and aluminum alloy powder which is currently available for laser additive manufacturing is mainly concentrated in Al-Si alloys. Such as hypoeutectic and eutectic Al-Si alloys containing 7 wt% Si to 10 wt% Si, have good fluidity and improved laser absorption due to the addition of Si element. Patent CN108486431A reports an Al-Si series aluminum alloy powder for selective laser melting technology, which comprises the following components: si: 7-15%, Mg: 0.8-3%, Mn: 1.2-2%, Zr: 0.5-1.5% and the balance of aluminum. However, the Al-Si alloy has poor thermal stability after being formed, the grain structure is rapidly coarsened at high temperature, the eutectic structure is collapsed, and the mechanical property is seriously degraded. The available alloy powder types are limited at present, and the development of novel alloy powder has important significance.
Disclosure of Invention
The invention aims to provide aluminum alloy powder and a preparation method and application thereof, so as to overcome the defects in the prior art and meet the application requirements of the related fields.
For an aluminum-rare earth (Al — Re) alloy, when the Re (La or Ce element) component is about 12 wt%, Al and Re are subjected to eutectic reaction to form a eutectic system, and the melt has good fluidity. Meanwhile, the Al-Re alloy has excellent thermal stability due to the extremely low diffusion coefficient and solid solubility of the Re element in Al. Re is added to generate rich transition energy level effect, laser energy with various wavelengths can be absorbed, the laser reflectivity is greatly reduced, and therefore the laser absorptivity is improved. Meanwhile, Mn and Fe with certain content are added into the alloy to promote the formation of Al6The high melting point phase of (Mn, Fe) can promote the improvement of the laser absorptivity of the powder. Al (Al)6The beneficial effects of the (Mn, Fe) refractory phase and Re are not interfered, and can jointly promote the improvement of the performance of the alloy powder. The Al-Re alloy powder has better thermal stability. While the element Re is Al6(Mn, Fe) high melting point phase and TiB2The particles can improve the laser absorption rate of the powder and are expected to make up the disadvantages of the Al-Si alloy powder. La is compared with CeThe unique price advantage of other rare earth elements is also an important factor for the implementation of the technical scheme of the invention.
The purpose of the invention is realized by the following technical scheme:
the invention provides Al-Re alloy powder which comprises the following components in percentage by mass:
Re:8.0~15.0%
Mn:0.1~2.0%
Fe:0.2~4.0%
the balance being Al and unavoidable impurities.
Preferably, the Al-Re alloy powder comprises the following components in percentage by mass:
Re:8.0~12.0%
Mn:0.5~1.0%
Fe:1.5~3.0%
the balance being Al and unavoidable impurities.
Preferably, the alloy powder further comprises TiB with the mass fraction of 1.0-10.0%2。
More preferably, the TiB2The mass fraction of (A) is 1.5-5.5%.
Preferably, the Re element is one or two of La and Ce.
Preferably, the TiB2The ceramic particles exist in the form of ceramic particles, and the size of the ceramic particles is 50-1200 nm.
The invention provides a preparation method of Al-Re alloy powder, which comprises the following steps:
p1, aluminum and TiB2Heating the/Al master batch, and heating to 660-780 ℃ to obtain a melt;
p2, adding Al-Re intermediate alloy, Al-Mn intermediate alloy and Al-Fe intermediate alloy into the melt obtained in the step P1 in sequence, refining and degassing, wherein the adopted refining temperature is 760-850 ℃, and the refining time is 10-20 min;
and P3, carrying out gas atomization on the melt obtained in the step P2 to obtain the Al-Re alloy powder.
Preferably, the aerosolization in step P3 is a conventional technique, as reported in patent CN107262730A, and specifically comprises the following steps:
and heating the melt to 740-900 ℃, and atomizing under the protection of Ar gas or He gas, wherein the atomizing pressure is 0.2-0.8 MPa, and the diameter of a nozzle used for atomizing is 0.5-3 mm.
The invention also provides application of the Al-Re alloy powder in laser additive manufacturing.
Compared with the prior art, the invention has the following beneficial effects:
the invention combines the advantages of Al-Re alloy and laser additive manufacturing to carry out structure refinement on the Al-Re alloy, further amplifies the advantage of thermal stability, and simultaneously Re and TiB2The addition of the reinforcing particles improves the laser absorption rate of the aluminum alloy powder.
The Al-Re alloy powder prepared by the invention can obtain the required particle size by industrial powder screening, and the powder yield is more than 70 percent; observing by using a scanning microscope, photographing, and then performing statistical calculation by using quantitative calculation software (IPP), wherein the sphericity is more than 90%; according to standard EN ISO 11551-.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The following examples provide an Al-Re alloy powder, a method of making the same, and applications thereof. By varying the composition of the alloying elements and TiB2The content of particles thus changes the properties of the powder. Changing the technological parameters of gas atomization is also one of the means of performance control.
Example 1
The embodiment provides Al-Ce-Fe-Mn alloy powder and a preparation method thereof, and the preparation method comprises the following steps:
al-14.8Ce-3.9Fe-0.1Mn alloy powder is prepared by taking pure Al, Al-Ce, Al-Fe and Al-Mn intermediate alloy as raw materials. Putting pure Al into a crucible, controlling the temperature of a resistance furnace to be 750 ℃, heating and melting, adding Al-Ce, Al-Fe and Al-Mn intermediate alloy after molten aluminum appears, continuously heating after covering by a high-temperature covering agent, removing floating slag on the surface after complete melting, and stirring by probing the bottom by using a graphite rod to ensure that a raw material block is completely melted. Adding an aluminum alloy refining agent into the melt for refining for 5min, then transferring the melt into a vacuum furnace for vacuumizing, keeping the temperature of the melt at about 820 ℃, and degassing for 10 min. The melt may be gas atomized after degassing. The gas atomization process comprises the following steps: the melt temperature is 800 ℃, He gas is used for protection and gas atomization, the atomization gas pressure is 0.8MPa, and the nozzle diameter is 2.5mm, thus obtaining Al-14.8Ce-3.9Fe-0.1Mn alloy powder.
The yield of the prepared Al-14.8Ce-3.9Fe-0.1Mn alloy powder is 76%, the sphericity rate is 91% and the laser absorption rate of the powder is 70%.
Example 2
The embodiment provides Al-La-Fe-Mn alloy powder and a preparation method thereof, and the specific preparation method comprises the following steps:
al-8.1La-0.2Fe-2.0Mn alloy powder is prepared by taking pure Al, Al-La, Al-Fe and Al-Mn intermediate alloy as raw materials. Putting pure Al into a crucible, controlling the temperature of a resistance furnace to be 750 ℃, heating and melting, adding Al-La, Al-Fe and Al-Mn intermediate alloy after molten aluminum appears, continuously heating after covering by a high-temperature covering agent, removing floating slag on the surface after complete melting, and stirring by probing the bottom by using a graphite rod to ensure that a raw material block is completely melted. Adding an aluminum alloy refining agent into the melt for refining for 5min, then transferring the melt into a vacuum furnace for vacuumizing, keeping the temperature of the melt at about 810 ℃, and degassing for 10 min. The melt may be gas atomized after degassing. The gas atomization process comprises the following steps: the temperature of the melt is 790 ℃, Ar gas is used for protection and gas atomization, the atomization pressure is 0.8MPa, and the diameter of a nozzle is 1.5mm, thus obtaining Al-8.1La-0.2Fe-2.0Mn alloy powder.
The yield of the prepared Al-8.1La-0.2Fe-2.0Mn alloy powder is 73 percent, the sphericity rate is 92 percent, and the laser absorption rate of the powder is 68 percent.
Example 3
The embodiment provides Al-Ce-Fe-Mn alloy powder and a preparation method thereof, and the preparation method comprises the following steps:
al-11.9Ce-2.9Fe-0.5Mn alloy powder is prepared by taking pure Al, Al-Ce, Al-Fe and Al-Mn intermediate alloy as raw materials. Putting pure Al into a crucible, controlling the temperature of a resistance furnace to be 750 ℃, heating and melting, adding Al-Ce, Al-Fe and Al-Mn intermediate alloy after molten aluminum appears, continuously heating after covering by a high-temperature covering agent, removing floating slag on the surface after complete melting, and stirring by probing the bottom by using a graphite rod to ensure that a raw material block is completely melted. Adding an aluminum alloy refining agent into the melt for refining for 5min, then transferring the melt into a vacuum furnace for vacuumizing, keeping the temperature of the melt at about 820 ℃, and degassing for 10 min. The melt may be gas atomized after degassing. The gas atomization process comprises the following steps: the temperature of the melt is 810 ℃, He gas is used for protection and gas atomization, the atomization gas pressure is 0.6MPa, and the diameter of a nozzle is 1.5mm, so that Al-11.9Ce-2.9Fe-0.5Mn alloy powder can be obtained.
The yield of the prepared Al-11.9Ce-2.9Fe-0.5Mn alloy powder is 76%, the sphericity rate is 92% and the laser absorption rate of the powder is 72%.
Example 4
The embodiment provides Al-La-Fe-Mn alloy powder and a preparation method thereof, and the specific preparation method comprises the following steps:
al-8.0La-1.6Fe-1.0Mn alloy powder is prepared by taking pure Al, Al-La, Al-Fe and Al-Mn intermediate alloy as raw materials. Putting pure Al into a crucible, controlling the temperature of a resistance furnace to be 750 ℃, heating and melting, adding Al-La, Al-Fe and Al-Mn intermediate alloy after molten aluminum appears, continuously heating after covering by a high-temperature covering agent, removing floating slag on the surface after complete melting, and stirring by probing the bottom by using a graphite rod to ensure that a raw material block is completely melted. Adding an aluminum alloy refining agent into the melt for refining for 5min, then transferring the melt into a vacuum furnace for vacuumizing, keeping the temperature of the melt at about 810 ℃, and degassing for 10 min. The melt may be gas atomized after degassing. The gas atomization process comprises the following steps: the temperature of the melt is 790 ℃, Ar gas is used for protection and gas atomization, the atomization pressure is 0.6MPa, and the diameter of a nozzle is 1.0mm, thus obtaining Al-8.0La-1.6Fe-1.0Mn alloy powder.
The yield of the prepared Al-8.0La-1.6Fe-1.0Mn alloy powder is 73 percent, the sphericity rate is 93 percent, and the laser absorption rate of the powder is 71 percent.
Example 5
This example provides a TiB2The preparation method of the/Al-La-Fe-Mn alloy powder comprises the following steps:
with pure Al, TiB29.4 wt% TiB is prepared by taking the master batch of the/Al composite material, Al-La, Al-Fe and Al-Mn intermediate alloy as raw materials2Al-11.7La-1.5Fe-0.6Mn alloy powder. Pure Al and TiB are firstly mixed2Putting the/Al composite material master batch into a crucible, controlling the temperature of a resistance furnace to 770 ℃, heating and melting, adding Al-La, Al-Fe and Al-Mn intermediate alloy after molten aluminum is generated, continuously heating after being covered by a high-temperature covering agent, removing floating slag on the surface after complete melting, and stirring by using a graphite rod to probe the bottom so as to ensure that the raw material blocks are completely melted. Adding an aluminum alloy refining agent into the melt for refining for 5min, then transferring the melt into a vacuum furnace for vacuumizing, keeping the temperature of the melt at about 830 ℃, and degassing for 10 min. The melt may be gas atomized after degassing. The gas atomization process comprises the following steps: the temperature of the fused mass is 810 ℃, Ar gas is used for protection and gas atomization, the atomization pressure is 0.6MPa, the diameter of a nozzle is 1.0mm, and 9.4wt percent TiB can be obtained2Al-11.7La-1.5Fe-0.6Mn alloy powder.
9.4 wt% TiB obtained2The yield of the alloy powder of Al-11.7La-1.5Fe-0.6Mn is 75%, the sphericity rate is 94% and the laser absorption rate of the powder is 73%.
Example 6
This example provides a TiB2The specific preparation method of the/Al-La-Fe-Mn alloy powder is basically the same as that of the example 5, except that: TiB of this example2The particle content was 1.0 wt%. .
1.0 wt% TiB obtained2The yield of the alloy powder of Al-11.7La-1.5Fe-0.6Mn is 75%, the sphericity rate is 93% and the laser absorption rate of the powder is 70%.
Example 7
This example provides a TiB2The preparation method of the/Al-La-Fe-Mn alloy powder comprises the following steps:
with pure Al, TiB2The master batch of the/Al composite material, Al-La, Al-Fe and Al-Mn intermediate alloy are taken as raw materials to prepare 5.0wt percent of TiB2Al-10.5La-2.4Fe-0.8Mn alloy powder. Pure Al and TiB are firstly mixed2Putting the/Al composite material master batch into a crucible, controlling the temperature of a resistance furnace to be 760 ℃, heating and melting, adding Al-La, Al-Fe and Al-Mn intermediate alloy after molten aluminum is generated, covering by a high-temperature covering agent, continuing heating, removing floating slag on the surface after complete melting, and stirring by using a graphite rod to probe the bottom so as to ensure that the raw material blocks are completely melted. Adding an aluminum alloy refining agent into the melt for refining for 5min, then transferring the melt into a vacuum furnace for vacuumizing, keeping the temperature of the melt at about 810 ℃, and degassing for 10 min. The melt may be gas atomized after degassing. The gas atomization process comprises the following steps: the melt temperature is 800 ℃, Ar gas is used for protection and gas atomization, the atomization pressure is 0.6MPa, the nozzle diameter is 1.0mm, and 5.0wt percent TiB can be obtained2Al-10.5La-2.4Fe-0.8Mn alloy powder.
Prepared 5.0 wt% TiB2The yield of the alloy powder of Al-10.5La-2.4Fe-0.8Mn is 78%, the sphericity rate is 96% and the laser absorption rate of the powder is 75%.
Example 8
This example provides an Al-La-Fe-Mn alloy powder and a method for preparing the same, the method being substantially the same as in example 7 except that: this example does not contain TiB2。
The yield of the prepared Al-10.5La-2.4Fe-0.8Mn alloy powder is 76%, the sphericity rate is 94% and the laser absorption rate of the powder is 71%.
Comparative example 1
This example provides an Al-La-Fe-Mn alloy powder and a method for preparing the same, the method being substantially the same as in example 8 except that: the alloy powder of this example had a composition of Al-6.0La-2.4Fe-0.8 Mn.
The yield of the prepared Al-6.0La-2.4Fe-0.8Mn alloy powder is 74%, the sphericity rate is 93% and the laser absorption rate of the powder is 66%.
Comparative example 2
This example provides an Al-Yb-Fe-Mn alloy powder and a method for producing the same, which is substantially the same as in example 8 except that: the alloy powder of this example had a composition of Al-10.5Yb-2.4Fe-0.8 Mn.
The yield of the prepared Al-10.5Yb-2.4Fe-0.8Mn alloy powder is 73 percent, the sphericity rate is 91 percent, and the laser absorption rate of the powder is 64 percent.
Comparative example 3
This example provides an Al-La-Cu-Mn alloy powder and a method for preparing the same, and the specific method is substantially the same as in example 8, except that: the alloy powder composition of this example was Al-10.5La-2.4Cu-0.8 Mn.
The yield of the prepared Al-10.5La-2.4Cu-0.8Mn alloy powder is 72 percent, the sphericity rate is 91 percent, and the laser absorption rate of the powder is 65 percent.
Comparative example 4
This example provides an Al-La-Cu-Fe alloy powder and a method for preparing the same, and the specific method is substantially the same as example 8, except that: the alloy powder composition of this example was Al-10.5La-0.8Cu-2.4 Fe.
The yield of the prepared Al-10.5La-0.8Cu-2.4Fe alloy powder is 72 percent, the sphericity rate is 92 percent, and the laser absorption rate of the powder is 63 percent.
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (5)
1. The Al-RE alloy powder is characterized by comprising the following components in percentage by mass:
RE:8.0~15.0%
Mn:0.1~2.0%
Fe:0.2~4.0%
the balance of Al and inevitable impurities;
the alloy powder also comprises 1.0-10.0 mass percent of TiB2;
The RE element is one or two of La and Ce;
the preparation method of the Al-RE alloy powder comprises the following steps:
p1, aluminum and TiB2Heating the/Al master batch, and heating to 660-780 ℃ to obtain a melt;
p2, adding Al-RE intermediate alloy, Al-Mn intermediate alloy and Al-Fe intermediate alloy into the melt obtained in the step P1 in sequence, refining and degassing, wherein the adopted refining temperature is 760-850 ℃, and the refining time is 10-20 min;
p3, carrying out gas atomization on the melt obtained in the step P2 to obtain the Al-RE alloy powder.
2. The Al-RE alloy powder according to claim 1, comprising the following components in mass fraction:
RE:8.0~12.0%
Mn:0.5~1.0%
Fe:1.5~3.0%
the balance being Al and unavoidable impurities.
3. The Al-RE alloy powder of claim 1, wherein the TiB2The mass fraction of (A) is 1.5-5.5%.
4. The Al-RE alloy powder of claim 1 or 3, wherein the TiB2The ceramic particles exist in the form of ceramic particles, and the size of the ceramic particles is 50-1200 nm.
5. Use of the Al-RE alloy powder according to any of claims 1-4 in laser additive manufacturing.
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