CN113600834B - Preparation method of high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition - Google Patents
Preparation method of high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition, which belongs to the technical field of high-temperature alloys and is characterized in that boron powder is used as reinforcing particles, and the addition amount of the boron powder is 0.05-0.13 wt%. The boron grain refiner is added to optimize the components of the high-niobium titanium-aluminum alloy, refine alloy grains and improve the room-temperature plasticity of the alloy; meanwhile, the temperature gradient between the substrate and the deposition layer is reduced through preheating, and cracks generated in the preparation of the high-niobium titanium-aluminum alloy based on laser melting deposition are eliminated and inhibited.
Description
Technical Field
The invention relates to the technical field of high-temperature alloys, in particular to a preparation method of a high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition.
Background
Lightweight titanium-aluminum alloys having excellent high-temperature properties are considered as important high-temperature structural materials in the future aviation field. However, the intrinsic brittleness of the intermetallic compound causes the low room temperature plasticity of the titanium-aluminum alloy, and the titanium-aluminum alloy is easy to crack in the processing process, thereby seriously hindering the application development of the titanium-aluminum alloy. In the high-niobium titanium-aluminum alloy, the addition of a large amount of niobium element increases the room-temperature brittleness of the alloy while improving the high-temperature strength of the alloy, and in addition, the existence of the ordered B2 phase not only further reduces the plasticity of the alloy, but also further increases the cracking problem of the alloy. The problems of poor plasticity and easy cracking of the high-niobium titanium-aluminum alloy seriously affect the application of the high-niobium titanium-aluminum alloy in larger-scale industrialization.
In recent years, researchers at home and abroad have conducted a great deal of research work in order to improve the room-temperature plasticity of titanium-aluminum-based alloys. At present, the grain refinement is considered to be the only effective means capable of simultaneously improving the strength and the plasticity of the titanium-aluminum alloy. There are studies showing that: when the grain size of the alloy is 50nm, the room temperature plasticity of the alloy reaches 50 percent, which is far more than the plasticity of the conventional grain size, and the alloy has superplasticity at normal temperature; the coarse as-cast structure is refined in the casting of the titanium-aluminum alloy, so that the mechanical property of the as-cast high-niobium titanium-aluminum alloy can be obviously improved. Therefore, the method has very important significance for obtaining fine and uniform lamellar structure by refining the crystal grains and improving the room temperature plasticity of the high-niobium titanium-aluminum alloy.
In addition, in the additive manufacturing process, the printing powder material is a key factor influencing the quality of a printed finished product, and determines the forming capability boundary of the additive manufacturing technology. The special surface structure of the nano particles enables nano-interaction energy to exist among the nano particles, so that the nano particles are agglomerated with each other. The high-energy ball milling method greatly reduces the sphericity of alloy powder particles after mixing the powder for a long time, causes great reduction of powder fluidity, and seriously influences the forming quality of additive manufacturing. Therefore, how to maintain the sphericity of the alloy powder particles is also an important problem to be solved urgently in the field.
Disclosure of Invention
The invention aims to provide a preparation method of a high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition, so as to solve the technical problems in the prior art.
In order to achieve the purpose, the invention provides the following scheme:
a preparation method of a high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition takes boron powder as reinforcing particles, and the addition amount of the boron powder is 0.05-0.13 wt%.
Further, the preparation method of the high-niobium TiAl alloy based on laser melting deposition and having excellent room temperature plasticity comprises the following steps:
(1) adding boron powder into an organic solvent to form a dispersion liquid, and performing ultrasonic crushing and dispersion treatment to form a particle suspension;
(2) adding spherical high-niobium titanium-aluminum alloy powder into the particle suspension obtained in the step (1) and uniformly mixing to obtain uniformly mixed suspension;
(3) mechanically stirring the uniformly mixed suspension obtained in the step (2) for 1-2 hours, and then drying and sieving to obtain particle-reinforced high-niobium TiAl alloy powder;
(4) preheating a substrate of a device for realizing laser melting deposition, and then processing and molding the particle-reinforced high-niobium titanium-aluminum alloy powder obtained in the step (3) by using a laser melting deposition technology to obtain the high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition.
Further, in the step (2), the oxygen content of the spherical high-niobium TiAl alloy powder is less than 700ppm, and the particle size is 53-150 μm. If the oxygen content in the spherical high-niobium titanium-aluminum alloy powder is too high, the forming is affected, finally, a large number of defects such as air holes exist in a formed part, and the plasticity of the alloy is seriously reduced due to the too high oxygen content.
Further, in the step (1), the particle size of the boron powder is 90-120 nm.
Further, in the step (1), the organic solvent is absolute ethyl alcohol, and the addition amount of the organic solvent is 10-20% of the weight of the spherical high-niobium TiAl alloy powder.
Further, in the step (1), the frequency of ultrasonic crushing and dispersing is 20-25 KHz, and the time is 15-60 min.
Further, in the step (2), the uniform mixing method is ultrasonic and mechanical stirring dispersion, wherein the ultrasonic frequency is 20-25 KHz, the stirring speed is 50-100 r/min, and the time is 15-45 min.
Further, the method is characterized in that in the step (3), the drying process is carried out in a vacuum drying oven, the drying temperature is 60-80 ℃, and the drying time is 12-24 hours.
Further, in the step (4), the preheating heating device adopts an electromagnetic induction coil, the electromagnetic induction coil is arranged on a supporting plate of the substrate, and the preheating temperature is 900-1000 ℃.
Further, in the step (4), the machining specifically includes: according to the processing path of the layering and slicing information of the CAD model of the preset forming part, powder synchronously fed by the nozzle is melted layer by layer, rapidly solidified and deposited layer by laser, and finally the preset forming part is obtained.
The invention selects simple substance boron as a grain refiner, can precipitate fine boride pinning grain boundary, inhibits the growth of grains and plays a role in fine grain strengthening; the precipitated boride blocks dislocation motion to play a role in precipitation strengthening; meanwhile, the addition of boron also has the effects of improving the segregation of beta phase and Al element, converting columnar crystal into isometric crystal and the like. In addition, the refined crystal grains can also inhibit the rapid expansion of cracks and improve the comprehensive mechanical property of the alloy.
The laser melting deposition technology adopts a coaxial powder feeding mode, has low scanning speed and low cooling speed, and is beneficial to inhibiting residual stress and brittleness alpha of titanium-aluminum alloy during solidification 2 And (4) generation of phases. In addition, the height of a laser focusing point can be freely adjusted in the laser melting deposition process, a laser beam is defocused above a deposition layer, and powder is fully preheated before entering a molten pool under the condition of high enough laser power, so that the aim of eliminating cracks is fulfilled.
The method for uniformly mixing the boron powder and the spherical high-niobium titanium-aluminum alloy powder is ultrasonic combined with mechanical stirring and dispersion. The ultrasonic wave depends on the ultrasonic cavitation of the liquid and has good dispersion effect in the liquid. When ultrasonic vibration is transmitted to liquid, strong cavitation effect can be excited in the liquid, so that a large number of cavitation bubbles are generated in the liquid, micro-jet flow is generated in the liquid along with the generation and explosion of the cavitation bubbles, large solid particles in the liquid are smashed, and meanwhile, the solid and the liquid are more fully mixed due to the vibration and dispersion effect of ultrasonic waves.
The invention discloses the following technical effects:
(1) according to the invention, elemental boron is introduced as a grain refiner, so that a fine grain strengthening effect is achieved, and when the addition amount of boron is 0.13wt% of the weight of the alloy, the refining effect is most obvious; the precipitated boride blocks dislocation motion to play a role in precipitation strengthening; meanwhile, the segregation of beta phase and Al element is effectively improved, and columnar crystal is converted into isometric crystal. In addition, the refined crystal grains can inhibit the rapid propagation of cracks and improve the comprehensive mechanical property of the alloy.
(2) The invention adopts an ultrasonic-stirring method to prepare the particle-reinforced high-niobium titanium-aluminum alloy powder, the method has wide raw material selection, simple and easy operation of the preparation method and low preparation cost, and the boron powder is well dispersed and uniformly dispersed and adsorbed on the high-niobium titanium-aluminum alloy spherical powder under the ultrasonic action on the basis of ensuring that the good spherical shape of the high-niobium titanium-aluminum alloy is not damaged. The particle-reinforced high-niobium TiAl alloy powder prepared by the method has high sphericity and good fluidity and meets the requirements of laser melting deposition technology.
(3) The invention adopts the laser melting deposition technology to prepare the formed high-niobium titanium-aluminum alloy, and selects the alloy with the same components as the deposited layer as the substrate, thereby reducing the thermal expansion coefficient between the substrate and the deposited layer; the substrate is preheated by an electromagnetic induction heating mode before deposition, the temperature of the substrate is not lower than 900 ℃ by a temperature control device in the deposition process, and the cooling rate is controlled by the temperature control device and a cooling device after the deposition is finished, so that the temperature gradient between the substrate and the deposition layer is reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is an SEM image of the alloy powder, wherein a is an SEM image of the high niobium tialoy powder raw material used in all examples, and b is an SEM image of the particle-reinforced high niobium tialoy powder prepared in step (3) of example 3.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. It is intended that the specification and examples be considered as exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
The raw materials used in this example:
spherical high-niobium TiAl alloy powder: 200g of the alloy powder, 53-150 mu m of particle size, less than 700ppm of oxygen, 17.41wt% of niobium, 53.13 wt% of titanium and 29.46 wt% of aluminum; the SEM image of the raw material spherical high-Nb TiAl alloy powder is shown in FIG. 1 (a).
Boron powder: the dosage is 0.1g, and the particle size is 90-110 nm;
anhydrous ethanol: the dosage is 20 g.
The method comprises the following specific steps:
(1) adding 0.1g of boron powder into 20g of absolute ethyl alcohol to form dispersion liquid, and carrying out ultrasonic crushing and dispersion treatment for 15min under the condition that the ultrasonic frequency is 20KHz to form reinforced particle suspension.
(2) Adding 200g of spherical high-niobium titanium-aluminum alloy powder into the reinforced particle suspension obtained in the step (1), stirring for 15min by adopting an ultrasonic and mechanical stirring and dispersing method, and uniformly mixing to obtain a uniformly mixed suspension. Wherein the ultrasonic frequency of ultrasonic and mechanical stirring dispersion is 20KHz, and the stirring speed of mechanical stirring is 50 r/min.
(3) Stirring the uniformly mixed suspension obtained in the step (2) for 2 hours under the conditions that the stirring power is 60W and the stirring speed is 100r/min until the organic solvent is basically volatilized, then drying for 24 hours in a vacuum drying oven at the temperature of 60 ℃, and screening to obtain particle-reinforced high-niobium titanium-aluminum alloy powder;
(4) preheating the substrate to 900 ℃ by using an electromagnetic induction heating device, then maintaining the temperature of the substrate to be not lower than 900 ℃, and performing layer-by-layer melting, rapid solidification and layer-by-layer deposition on powder synchronously fed by a nozzle by using laser according to a processing path of the layered slicing information of a CAD model of the preset forming part to finally obtain the preset forming part, namely the high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition.
Example 2
The raw materials used in this example:
spherical high-niobium TiAl alloy powder: 200g of the alloy powder, 53-150 mu m of particle size, less than 700ppm of oxygen, 17.41wt% of niobium, 53.13 wt% of titanium and 29.46 wt% of aluminum; the SEM image of the raw material spherical high-Nb TiAl alloy powder is shown in FIG. 1 (a).
Boron powder: the dosage is 0.15g, and the particle size is 90-110 nm;
absolute ethanol: the dosage is 30 g.
The method comprises the following specific steps:
(1) 0.15g of boron powder is added into 30g of absolute ethyl alcohol to form dispersion liquid, and the dispersion liquid is subjected to ultrasonic crushing and dispersion treatment for 30min under the condition that the ultrasonic frequency is 23KHz to form reinforced particle suspension.
(2) Adding spherical high-niobium titanium-aluminum alloy powder into the reinforced particle suspension obtained in the step (1), stirring for 30min by adopting an ultrasonic and mechanical stirring and dispersing method, and uniformly mixing to obtain a uniformly mixed suspension. Wherein the ultrasonic frequency of ultrasonic and mechanical stirring dispersion is 23KHz, and the stirring speed of mechanical stirring is 80 r/min.
(3) Stirring the uniformly mixed suspension obtained in the step (2) for 1.5 hours under the conditions that the stirring power is 100W and the stirring speed is 200r/min until the organic solvent is basically volatilized, then drying the suspension in a vacuum drying oven at 70 ℃ for 20 hours, and sieving the suspension to obtain particle-enhanced high-niobium titanium-aluminum alloy powder;
(4) preheating the substrate to 950 ℃ by using an electromagnetic induction coil arranged on a supporting plate of the substrate, then maintaining the temperature of the substrate to be not lower than 900 ℃, and according to the processing path of the layered slicing information of the CAD model of the preset forming part, carrying out layer-by-layer melting, rapid solidification and layer-by-layer deposition on the powder synchronously fed by a nozzle by using laser to finally obtain the preset forming part, namely the high-niobium titanium-aluminum alloy with excellent room temperature plasticity based on laser melting deposition.
Example 3
The raw materials used in this example:
spherical high-niobium TiAl alloy powder: 200g of the alloy powder, 53-150 mu m of particle size, less than 700ppm of oxygen, 17.41wt% of niobium, 53.13 wt% of titanium and 29.46 wt% of aluminum; (ii) a The SEM image of the raw material spherical high-Nb TiAl alloy powder is shown in FIG. 1 (a).
Boron powder: the dosage is 0.26g, and the particle size is 100-120 nm;
anhydrous ethanol: the dosage is 40 g.
The method comprises the following specific steps:
(1) adding 0.26g of boron powder into 40g of absolute ethyl alcohol to form dispersion liquid, and carrying out ultrasonic crushing and dispersion treatment for 60min under the condition that the ultrasonic frequency is 25KHz to form reinforced particle suspension.
(2) Adding the spherical high-niobium titanium-aluminum alloy powder into the reinforced particle suspension obtained in the step (1), stirring for 45min by adopting an ultrasonic and mechanical stirring and dispersing method, and uniformly mixing to obtain a uniformly mixed suspension. Wherein the ultrasonic frequency of ultrasonic and mechanical stirring dispersion is 25KHz, and the stirring speed of mechanical stirring is 100 r/min.
(3) Stirring the uniformly mixed suspension obtained in the step (2) for 1h under the conditions that the stirring power is 120W and the stirring speed is 300r/min until the organic solvent is basically volatilized, then drying in a vacuum drying oven at the temperature of 80 ℃ for 12h, and sieving to obtain particle-reinforced high-niobium titanium-aluminum alloy powder;
(4) preheating the substrate to 1000 ℃ by using an electromagnetic induction heating device, then maintaining the temperature of the substrate to be not lower than 900 ℃, and performing layer-by-layer melting, rapid solidification and layer-by-layer deposition on powder synchronously fed by a nozzle by using laser according to a processing path of the layered slicing information of a CAD model of the preset forming part to finally obtain the preset forming part, namely the high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition.
The SEM image of the high nb ti-al alloy prepared in this example is shown in fig. 1(b), from which it can be seen that: on the basis that the good spherical shape of the high-niobium titanium-aluminum alloy is not damaged basically, the boron powder can be uniformly dispersed and adsorbed on the high-niobium titanium-aluminum alloy spherical powder. The particle-reinforced high-niobium TiAl alloy powder prepared by the method of the embodiment has high sphericity and good fluidity.
Comparative example 1
The only difference from example 1 is that no boron element was added.
Comparative example 2
The only difference from comparative example 1 is that the preparation process is vacuum melting.
Comparative example 3
The only difference from example 3 is that the substrate was not preheated.
The formability, inter-lamellar spacing, tensile strength and elongation data of the high Nb TiAl alloys prepared in examples 1-3 and comparative examples 1-3 are compared in Table 1 below, wherein the grain size is measured as E112-96 and the tensile strength and elongation are measured as GBT 228-.
TABLE 1
| Examples | Formability | Lamellar spacing, μm | Tensile strength, MPa | Elongation percentage of% |
| Example 1 | Is not cracked | 0.37～0.49 | 556 | 0.34 |
| Example 2 | Is not cracked | 0.24～0.35 | 619 | 0.39 |
| Example 3 | Is not cracked | 0.11～0.22 | 749 | 0.50 |
| Comparative example 1 | Is not cracked | 0.52～1.11 | 445 | 0.25 |
| Comparative example 2 | Is not cracked | 30～40 | 273 | 0.14 |
| Comparative example 3 | Macroscopic cracking | - | - | - |
As can be seen from table 1:
(1) the substrate is preheated in an electromagnetic induction heating mode, so that the temperature gradient between the substrate and the deposition layer is reduced, the formation of cracks in the laser melting deposition process can be well inhibited, and a high-niobium titanium-aluminum alloy sample which is crack-free, high in density and uniform in tissue components is prepared;
(2) compared with a vacuum melting forming technology, the high-niobium titanium-aluminum alloy formed by the laser melting deposition technology has a finer structure, and the tensile strength and room temperature plasticity of the alloy are higher; after the elemental boron is introduced, the lamella spacing is reduced, the lamella crystal grains are refined, and the room temperature plasticity and the tensile strength of the alloy are improved; when the addition amount of the boron element reaches 0.13wt%, the alloy shows the best comprehensive mechanical property.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (9)
1. The preparation method of the high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition is characterized in that boron powder is used as reinforcing particles, and the addition amount of the boron powder is 0.05-0.13 wt%;
the preparation method comprises the following steps:
(1) adding boron powder into an organic solvent to form a dispersion liquid, and performing ultrasonic crushing and dispersion treatment to form a particle suspension;
(2) adding spherical high-niobium titanium-aluminum alloy powder into the particle suspension obtained in the step (1) and uniformly mixing to obtain uniformly mixed suspension; the ratio of niobium in the spherical high-niobium titanium-aluminum alloy powder is 17.41 wt%;
(3) mechanically stirring the uniformly mixed suspension obtained in the step (2) for 1-2 hours, and then drying and sieving to obtain particle-reinforced high-niobium TiAl alloy powder;
(4) preheating a substrate of the device for realizing laser melting deposition to 900-1000 ℃, and then processing and forming the particle-reinforced high-niobium titanium-aluminum alloy powder obtained in the step (3) by using a laser melting deposition technology to obtain the high-niobium titanium-aluminum alloy with excellent room-temperature plasticity based on laser melting deposition.
2. The method for preparing a high-niobium TiAl alloy based on laser melting deposition and having excellent room temperature plasticity according to claim 1, wherein in the step (2), the spherical high-niobium TiAl alloy powder has an oxygen content of 700ppm or less and a particle diameter of 53 to 150 μm.
3. The method for preparing a high-niobium TiAl alloy based on laser melting deposition and having excellent room temperature plasticity according to claim 1, wherein in the step (1), the powder particle size of the boron powder is 90-120 nm.
4. The method for preparing a high-niobium TiAl alloy based on laser melting deposition with excellent room temperature plasticity, according to claim 1, wherein in the step (1), the organic solvent is absolute ethyl alcohol, and the addition amount of the organic solvent is 10-20% of the weight of the spherical high-niobium TiAl alloy powder.
5. The preparation method of the high-niobium TiAl alloy based on laser melting deposition and having excellent room temperature plasticity, according to claim 1, wherein in the step (1), the ultrasonic crushing and dispersing frequency is 20 to 25KHz, and the time is 15 to 60 min.
6. The preparation method of the high-niobium TiAl alloy based on laser melting deposition and having excellent room temperature plasticity is characterized in that in the step (2), the uniform mixing method is ultrasonic combined with mechanical stirring and dispersing, wherein the ultrasonic frequency is 20-25 KHz, the stirring speed is 50-100 r/min, and the time is 15-45 min.
7. The preparation method of the high-niobium TiAl alloy based on laser melting deposition and having excellent room temperature plasticity, according to claim 1, wherein in the step (3), the drying process is carried out in a vacuum drying oven, the drying temperature is 60-80 ℃, and the drying time is 12-24 h.
8. The method for manufacturing a high-niobium titanium-aluminum alloy excellent in room-temperature plasticity based on laser melting deposition according to claim 1, wherein in the step (4), the preheating heating device employs an electromagnetic induction coil, and the electromagnetic induction coil is disposed on a pallet of a substrate.
9. The method for preparing a high-niobium TiAl alloy based on laser fusion deposition and having excellent room temperature plasticity according to claim 1, wherein in the step (4), the processing and forming specifically comprises: according to the processing path of the layered slice information of the CAD model of the preset forming part, the powder synchronously fed by the nozzle is melted layer by layer, rapidly solidified and deposited layer by laser, and finally the preset forming part is obtained.
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