CN114346247A - Wire material for preparing 3D printing alloy powder and powder preparation method - Google Patents
Wire material for preparing 3D printing alloy powder and powder preparation method Download PDFInfo
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Abstract
The wire for preparing the 3D printing alloy powder comprises a wire body, wherein the wire body comprises a containing cavity and a metal single body which is positioned in the containing cavity and can be subjected to plasma atomization alloying to form the 3D printing alloy powder. The wire is provided with the accommodating cavity, and the metal single plastid in the accommodating cavity can be added as required, so that the composition adjustment is easy, the smelting, rolling and drawing processes are avoided, the production cost is reduced, and the wire is suitable for scientific research of small-batch alloy composition design. The preparation method of the 3D printing alloy powder comprises the steps of feeding wires into the center of a convergent plasma jet, melting and alloying the wires in the plasma jet, atomizing the wires by the plasma jet, and cooling and solidifying atomized small droplets after flying out of the plasma jet to form the 3D printing alloy powder. Compared with the PREP and EIGA processes, the method for preparing the alloy powder has the advantages that the grain size of the alloy powder is small, the yield of fine grain size powder is improved, and low-cost regulation and control of alloy components can be realized.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a method for preparing 3D printing titanium alloy powder by plasma atomization of cored wires.
Background
At present, the commercial 3D printing titanium alloy powder preparation methods mainly include plasma rotary electrode atomization (PREP), Electrode Induction Gas Atomization (EIGA), Mechanical Alloying (MA), and Plasma Atomization (PA).
The PREP technology processes titanium alloy into bar stock, utilizes plasma to heat and melt the end face of the bar stock, simultaneously the bar stock rotates at high speed, molten liquid drops are thrown out under the action of centrifugal force, and then the bar stock is cooled in an inert gas environment and is spheroidized under the action of surface tension, and finally spherical powder is formed. The particle size of the powder, namely the size of the liquid drop, is limited by the rotating speed of the bar stock, so that the particle size of the atomized powder is larger, and the requirement of the selective laser melting process is difficult to meet.
The EIGA atomization process adopts a design without a crucible and a flow guide pipe, avoids the pollution problem of a ceramic material in the melting and flow guide processes of a titanium alloy liquid, but has the defects of low yield of fine-grain-size powder (less than 53 mu m) and satellite ball and hollow powder contained in atomized powder.
The MA method is to repeatedly cold weld and break powder particles by long-term impact and collision between powder particles and an abrasive in a high-energy ball mill, and finally realize alloying by atomic diffusion, but the powder has irregular shape and poor fluidity, and inevitably contains grinding ball peeling impurities.
The recently developed wire plasma atomization technology (PA) adopts a confluence plasma torch to heat and melt a wire, meanwhile, molten titanium alloy liquid is atomized and crushed under the impact condition of supersonic plasma jet, and then small liquid drops are cooled and solidified after flying out of the plasma jet to form spherical powder, wherein the particle size of the powder is suitable for the requirement of a selective laser melting process. However, PA technology is owned by AP & C and Pyrogenesis, Canada (US5707419, CN108025364, CN 108025365), which imposes a strict technical lock on China.
The titanium alloy powder prepared by the PA technology has excellent performance, so the titanium alloy powder is widely concerned by scientific research institutions and enterprises. The Chengdu superior material science and technology Limited patent (CN106378460B) sends titanium alloy wire into convergent plasma jet, proposes that atomized liquid drops are subjected to laminar cooling through argon gas at 300-500 ℃, and then high-sphericity powder is obtained. The patent (CN205414417U) of Hunan Jiutai metallurgy science and technology Limited also sends the wire material into the center of the convergent plasma jet to realize atomization, and provides a device for preventing the ultrafine powder from being adhered to the wall of an atomization furnace. Beijing gold science and technology development Limited (CN108161019A) discloses a technology combining induction heating, radio frequency plasma melting and gas atomization, belonging to a gas atomization method, similar to EIGA. Hangzhou handicraft new material science and technology limited (CN210387591U) discloses a device for atomizing titanium alloy powder by induction heating gas, belonging to a gas atomization method and being similar to EIGA.
However, limited by the monopoly of PA technology by canadian corporation, domestic 3D printed titanium alloy powders are still prepared using PREP and EIGA processes. So far, no commercial domestic PA equipment and PA titanium alloy powder are available.
Disclosure of Invention
The invention aims to solve the problem that the preparation of alloy powder in the prior art cannot well meet the requirements of small-batch production and component design, adopts a supersonic plasma torch and a convergent plasma jet structure developed by a patent (CN110039061A), and feeds cored wires into a convergence center of plasma jet to be melted and alloyed under the heating condition of high-enthalpy plasma jet, and the melted alloy liquid is atomized and crushed by the supersonic plasma jet, so that the smelting, rolling and multiple drawing processes in the conventional preparation process of titanium alloy wires are avoided, the process flow of atomized titanium alloy powder is shortened, the cored wires are easy to adjust the material components, the material development cost is reduced, and the wires for preparing 3D printing titanium alloy powder are provided.
The invention also aims to solve the problem that the low-melting-point metal simple substance is easy to burn out in the alloying process in the prior art, and provide the anti-burning powder core wire.
Still another object of the present invention is to provide a method for preparing a cored wire for 3D printing of titanium alloy powder by plasma atomization.
In order to achieve the purpose, the invention adopts the following specific technical scheme:
the wire for preparing 3D printing alloy powder comprises a wire body, wherein the wire body comprises a containing cavity and a metal single body which is positioned in the containing cavity and can be subjected to plasma atomization alloying to form the alloy powder for 3D printing.
The invention relates to an anti-burning powder core wire, which comprises a plurality of component units distributed along the radial direction from the center on any cross section of a containing cavity.
Preferably, the metal simple substance body comprises metal simple substance powder.
Preferably, the elemental metal powder comprises zirconium powder, niobium powder, tantalum powder, tin powder and titanium hydride powder.
Preferably, the device further comprises a wrapping skin wrapping the accommodating cavity, wherein the wrapping skin is formed by at least one simple metal capable of being subjected to plasma atomization alloying to form alloy powder for 3D printing.
Preferably, the wrapper comprises a pure titanium wrapper.
The preparation method of the alloy powder comprises the steps of feeding the wire into the center of the convergent plasma jet, melting and alloying the wire in the plasma jet, atomizing the wire by the plasma jet, and cooling and solidifying atomized small droplets after flying out of the plasma jet to form the 3D printing alloy powder.
Specifically, the method comprises the following specific steps:
the method comprises the following steps: adjusting the included angle between the plasma jet device and the wire to be 15-45 degrees;
step two: keeping the vacuum degree of the atomizing chamber lower than 2 Pa; backfilling the protective atmosphere to maintain the pressure of the atomizing chamber at 1000-100000 Pa;
step three: detecting the oxygen content of the atomizing chamber to ensure that the oxygen content of the atmosphere is less than 10 ppm;
step four: igniting a plasma gun under a protective atmosphere, and gradually increasing the current to a set value of 500A;
step five: and feeding the wire material into an atomization chamber for atomization.
Preferably, the method further comprises a wire straightening step before wire feeding, wherein the wire straightening step comprises adjusting a wire straightening mechanism to stably and uniformly feed the wire into the three plasma jet convergence positions through the wire guide pipe.
Compared with the prior art, the invention has the following beneficial effects:
the wire is provided with the containing cavity, and the structure of the wire is different from that of the existing solid alloy wire. Because the metal single plastid in the accommodating cavity can be added according to the requirement, the component design is easy to carry out; because the smelting, rolling and multiple drawing processes in the conventional alloy wire preparation process are not needed, the production cost is reduced, and the small-batch scientific research of alloy component design is facilitated.
Compared with the PREP and EIGA processes, the method for preparing the alloy powder has the advantages that the prepared 3D printing titanium alloy powder is small in particle size, and the yield of fine particle size powder is improved. Therefore, the invention can realize low-cost design of components by performing plasma atomization on the powder core wire material to 3D print the titanium alloy powder, and reduce the cost of 3D printing the alloy powder.
The invention will be further described with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic view of the structure of a powder core wire material in a preferred embodiment of the present invention.
FIG. 2a is a schematic cross-sectional view of a powder core wire material in accordance with a preferred embodiment of the present invention. The drawing is a schematic drawing drawn to facilitate understanding of the design concept of the present invention.
FIG. 2b is a schematic cross-sectional structure of an actual cored wire in a preferred embodiment of the present invention.
FIG. 3 shows the morphology (-100 mesh) of plasma atomized Ti2448 powder in accordance with a preferred embodiment of the present invention.
FIG. 4 is a cross-sectional structure of a plasma atomized Ti2448 powder in accordance with a preferred embodiment of the present invention.
FIG. 5 is a sectional structure and elemental distribution plot of a single particle of plasma atomized Ti2448 powder in accordance with a preferred embodiment of the present invention.
Fig. 6 is a XRD result of Ti2448 powder in a preferred embodiment of the present invention.
FIG. 7 shows the morphology (-270 mesh) of a plasma atomized TNTZ powder according to a preferred embodiment of the present invention.
Description of reference numerals:
100 wire bodies, 101 cross sections, 102 containing cavities,
10 metal simple substance, 111 metal simple substance powder, 121 wrapping skin,
20 component units.
Detailed Description
The present invention is further explained and illustrated by the following embodiments, which should be understood to make the technical solution of the present invention clearer and easier to understand, and not to limit the scope of the claims.
The wire for preparing 3D printing alloy powder comprises a wire body 100, wherein the wire body 100 comprises a containing cavity 102 and a metal single body 10 which is located in the containing cavity 102 and can be subjected to plasma alloying atomization to form the 3D printing alloy powder.
The invention relates to an anti-burning powder core wire, which comprises a plurality of component units 20 distributed radially from the center in any cross section 101 of a containing cavity 102, wherein any component unit 20 comprises at least two metal single bodies 10 with different melting points
In a preferred embodiment, the metal simple substance 10 includes a metal simple substance powder 111. Specifically, the elemental metal powder 111 includes zirconium powder, niobium powder, tantalum powder, tin powder, and titanium hydride powder.
In a preferred embodiment, the device further comprises a wrapping skin 121 wrapping the accommodating cavity 102, wherein the wrapping skin is formed by at least one metal simple substance capable of being atomized into 3D printing alloy powder through plasma alloying. Specifically, the wrapping skin 121 includes a pure titanium skin.
The preparation method of the alloy powder comprises the steps of feeding the wire into the center of the convergent plasma jet, melting and alloying the wire in the plasma jet, atomizing the wire by the plasma jet, and cooling and solidifying atomized small droplets after flying out of the plasma jet to form the 3D printing alloy powder.
Specifically, the method comprises the following specific steps:
the method comprises the following steps: adjusting the included angle between the plasma jet device and the wire to be 15-45 degrees;
step two: keeping the vacuum degree of the atomizing chamber lower than 2 Pa; backfilling the protective atmosphere to maintain the pressure of the atomizing chamber at 1000-100000 Pa;
step three: detecting the oxygen content of the atomizing chamber to ensure that the oxygen content of the atmosphere is less than 10 ppm;
step four: igniting a plasma gun under a protective atmosphere, and gradually increasing the current to a set value of 500A;
step five: and feeding the wire material into an atomization chamber for atomization.
In a preferred embodiment, the method further comprises a wire straightening step before wire feeding, wherein the wire straightening step comprises adjusting a wire straightening mechanism to stably and uniformly feed the wire into a three-plasma jet converging position through a wire guide pipe.
The following detailed description is presented to facilitate a better understanding of the invention.
Example 1
The Ti2448 alloy according to example 1 is prepared by using pure titanium ribbon (99.9 wt.%), Zr powder (99.99 wt.%), D50 ═ 16 μm), TiH2 powder (99.99 wt.%), D50 ═ 20 μm), Nb powder (99.99 wt.%), D50 ═ 6 μm) and subsphaeroidal Sn powder (99.9 wt.%, D50 ═ 12 μm) as raw materials, and the adopted raw material metal elemental powders all require low oxygen content, and the 3D printing Ti2448 alloy powder is prepared by a powder core wire plasma atomization technique.
The Ti2448 alloy wire is prepared by rolling a pure metal titanium belt wrapped with a powder material. The niobium-zirconium-tin powder is prepared according to the weight ratio of Nb, Zr and Sn of 24:4:8, firstly, the niobium powder and the tin powder are premixed, then the premixed powder is mechanically stirred and mixed with the zirconium powder and the titanium hydride powder in a V-shaped mixer, and the mixing process is carried out under the protection of high-purity argon; secondly, cutting a metal foil strip with the thickness of 0.4-1.0mm into strips with the width of 10-14mm, and rolling the strips into U-shaped grooves after passing through a plurality of rollers; and then uniformly feeding the premixed powder into a U-shaped groove (the filling rate is determined according to the target component of the titanium alloy), rolling by a plurality of rollers, gradually closing the U-shaped groove, and finally completely wrapping the premixed powder inside a titanium metal foil strip to form the Ti2448 cored wire, wherein the diameter of the rolled Ti2448 cored wire is 2.0-3.0 mm.
The invention adopts a method of low-pressure plasma atomization of powder core wires to prepare 3D printing Ti2448 alloy powder (the device is the device in patent CN 110039061A). Firstly, straightening Ti2448 powder core wires by a straightening mechanism, then sending the straightened powder core wires into a convergence center of a plurality of plasma jet flows, rapidly melting the wires, carrying out in-situ alloying on all elements, simultaneously carrying out atomization and crushing on molten liquid drops under the impact of supersonic plasma jet flows, cooling and solidifying the crushed liquid drops after flying out of the plasma jet flows, and forming 3D printing Ti2448 alloy powder. The plasma atomized Ti2448 alloy powder has excellent sphericity (FIG. 3) and no hollow powder defects (FIG. 4) due to sufficient time for spheroidization of atomized droplets under surface tension during flight of the plasma jet. The wire is alloyed in situ in the plasma jet, and elements are distributed uniformly (figure 5), which is beneficial to obtaining 3D printing tissue with uniform components. The plasma atomization powder XRD result of the powder core wire shows that the powder is in a beta phase, no other elemental metal element peak is found (figure 6), and the powder core wire is shown to be alloyed in plasma jet.
In the embodiment 1, the converged plasma jet is used for heating and melting the powder core wire and realizing in-situ alloying, and then liquid drops are atomized and crushed to obtain 3D printing alloy powder. The atomization preparation process of the 3D printed Ti2448 alloy powder comprises the following steps:
the method comprises the following steps: adjusting the included angle between the plasma gun and the wire to be 15-45 degrees;
step two: adjusting the wire straightening mechanism to stably and uniformly send the wires into three plasma jet convergence positions through the wire guide pipe;
step three: opening a mechanical pump, and pumping an atomizing chamber of the Roots pump to a vacuum degree lower than 2 Pa; backfilling argon to maintain the pressure of the atomization chamber at 1000-100000 Pa; and simultaneously opening a cooling water circulating system of the atomizing chamber;
step four: the oxygen sensor detects the oxygen content of the atomizing chamber and ensures that the oxygen content of the atmosphere is less than 10 ppm;
step five: turning on an argon switch, igniting a plasma gun, and gradually increasing the current to a set value of 500A;
step six: opening the wire feeder, adjusting the wire feeding speed and starting atomization;
step seven: after the atomization is finished, the wire feeder and the plasma power supply are sequentially closed;
step eight: and passivating the powder, screening and batching under atmosphere protection, and then carrying out vacuum packaging and storage.
In this embodiment 1, the preparation of 3D printing powder is realized by a powder core wire plasma atomization method, which not only improves the yield (higher than 30%) of fine particle size powder (smaller than 53 μm), but also improves the sphericity of the powder, reduces the defects of hollow powder, and provides a certain reference for some alloy materials difficult to wire drawing, such as cast high temperature alloy and high entropy alloy.
Example 2
The TNTZ (Ti-29 Nb-13 Ta-4.6 Zr) alloy powder core wire is prepared by rolling a titanium foil tape wrapped with a powder material. The filler powders were Zr powder (99.99 wt.%, D50 ═ 16 μm), Nb powder (99.99 wt.%, D50 ═ 6 μm), Ta powder (99.99 wt.%, D50 ═ 0.6 μm), and TiH2 powder (99.99%, D50 ═ 20 μm); the width of the titanium strip is 10-14mm, and the thickness is 0.4-1.0 mm. Firstly, placing powder into a V-shaped mixer according to a set component proportion for mechanical stirring and mixing, introducing argon for protection, and simultaneously adding a powder surfactant in the stirring process to improve the flowability of the powder; and rolling the titanium strip into a U-shaped groove by a roller, uniformly feeding the premixed powder into the U-shaped groove by ultrasonic vibration, gradually closing the U-shaped groove into a circle after rolling by a plurality of subsequent rollers, and completely wrapping the premixed powder on the inner part of the titanium foil strip to form the TNTZ powder core wire material.
In this example 2, TNTZ alloy powder for 3D printing is prepared by a powder core wire plasma atomization method. In the same way as the device in the embodiment 1, the heat source adopts three converged plasma jet flows, and the included angle between the axis of the plasma torch and the wire is 15-45 degrees. Firstly, straightening the prepared TNTZ powder core wire material by a straightening mechanism, then sending the straightened wire material into a convergence center of three plasma jet flows through a wire guide pipe, heating and melting the wire material by the plasma jet flows, carrying out in-situ alloying on titanium alloy, simultaneously atomizing and crushing large molten droplets under the impact of supersonic plasma jet flows, further alloying the formed small droplets in the plasma jet flows, spheroidizing under the action of surface tension, cooling and solidifying after flying out of the plasma jet flows to form TNTZ alloy powder, wherein the shape of the powder after grading is shown in figure 7, and finally sieving the powder which is suitable for 3D printing and has the particle size requirement under the atmosphere protection condition.
Aiming at the difficulty in efficiently preparing 3D printing titanium alloy powder by the current PREP and EIGA processes, the invention adopts high-purity raw materials (titanium foil strips and micron and submicron powder) to prepare 3D printing Ti2448 and TNTZ powder core wires, and then realizes the atomization preparation of the powder by a plasma in-situ alloying method. The high enthalpy plasma is beneficial to heating and melting the titanium alloy powder core wire material and realizing in-situ alloying, overcomes the defects of the prior art, provides a new choice for developing 3D printing fine-grain-size titanium alloy powder at low cost, and lays a foundation for preparing high-quality titanium alloy parts by 3D printing, wherein the powder is spherical and has no satellite ball or ceramic inclusion.
While the present invention has been described by way of examples, and not by way of limitation, other variations of the disclosed embodiments, as would be readily apparent to one of skill in the art, are intended to be within the scope of the present invention, as defined by the claims.
Claims (10)
1. A wire for preparing 3D printing alloy powder, characterized in that: the wire body (100) comprises a containing cavity (102) and a metal single body (10) which is located in the containing cavity (102) and can be subjected to plasma melting alloying and atomization to form alloy powder for 3D printing.
2. The wire for preparing 3D printing alloy powder according to claim 1, wherein: any cross section (101) of the containing cavity (102) is composed of a plurality of component units (20) distributed from the center in the radial direction, and any component unit (20) comprises at least two metal single bodies (10) with different melting points.
3. The wire for preparing 3D printing alloy powder according to claim 1, wherein: the metal simple substance body (10) comprises metal simple substance powder (111).
4. The wire for preparing 3D printing alloy powder according to claim 4, wherein: the metal simple substance powder (111) comprises zirconium powder, niobium powder, tantalum powder, tin powder and titanium hydride powder.
5. A wire for preparing 3D printing alloy powder according to any one of claims 1 to 4, wherein: the coating device further comprises a coating skin (121) coating the containing cavity (102), wherein the coating skin is formed by at least one metal simple substance capable of forming alloy powder for 3D printing through plasma alloying atomization.
6. The wire for preparing 3D printing alloy powder according to claim 5, wherein: the wrapping skin (121) comprises pure titanium skin.
7. A method for preparing alloy powder is characterized in that: the method comprises the steps of feeding the wire material as claimed in any one of claims 1 to 6 into the center of a convergent plasma jet, melting and alloying the wire material in the plasma jet, and then atomizing the wire material by the plasma jet, wherein atomized small droplets are cooled and solidified after flying out of the plasma jet to form 3D printing alloy powder.
8. The method for producing an alloy powder according to claim 7, characterized in that: the method comprises the following specific steps:
the method comprises the following steps: adjusting the included angle between the plasma jet device and the wire;
step two: maintaining the vacuum degree of the atomizing chamber; backfilling protective atmosphere and maintaining the pressure of the atomizing chamber;
step three: detecting the oxygen content of the atomizing chamber to ensure the oxygen content of the atmosphere;
step four: igniting the plasma gun under the protective atmosphere, and gradually increasing the current to a set value;
step five: and feeding the wire material into an atomization chamber for atomization.
9. The method for producing an alloy powder according to claim 8, characterized in that: in the first step, the included angle between the plasma jet device and the wire is 15-45 degrees; in the second step, the vacuum degree of the atomizing chamber is kept lower than 2 Pa; backfilling the protective atmosphere to maintain the pressure of the atomizing chamber at 1000-100000 Pa; and in the third step, detecting the oxygen content of the atomizing chamber and ensuring that the oxygen content of the atmosphere is less than 10 ppm.
10. The method for producing an alloy powder according to claim 8, characterized in that: and before the wire feeding, the method also comprises a wire correcting step, which comprises adjusting a wire correcting mechanism to stably and uniformly feed the wires into a three-beam plasma jet converging position through a wire guide pipe.
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| CN110039061A (en) * | 2019-05-31 | 2019-07-23 | 广东省材料与加工研究所 | The preparation method of silk material low-voltage plasma atomising device and 3D printing high strength alumin ium alloy powder |
| CN210387591U (en) * | 2019-03-07 | 2020-04-24 | 杭州卓工新材料科技有限公司 | Preparation facilities of titanium and titanium alloy powder for 3D prints |
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- 2020-09-28 CN CN202011038449.9A patent/CN114346247A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101413096A (en) * | 2007-10-15 | 2009-04-22 | 北京赛亿表面工程技术有限公司 | Method for producing Ni-Al bimetal composite material solid core wire material |
| WO2018121688A1 (en) * | 2016-12-29 | 2018-07-05 | 江民德 | 3d printing spherical powder preparation method utilizing plasma |
| CN108746582A (en) * | 2018-05-21 | 2018-11-06 | 江苏大学 | Laser gain material manufacture NiTi micro-nano powder cored filament materials of rare earth enhancing and preparation method thereof |
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