CN116287824B - Titanium alloy with continuously adjustable phase structure and preparation method thereof - Google Patents

Titanium alloy with continuously adjustable phase structure and preparation method thereof Download PDF

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CN116287824B
CN116287824B CN202310090239.1A CN202310090239A CN116287824B CN 116287824 B CN116287824 B CN 116287824B CN 202310090239 A CN202310090239 A CN 202310090239A CN 116287824 B CN116287824 B CN 116287824B
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titanium alloy
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CN116287824A (en
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魏晓
金凯航
刘成
方迎春
王海文
张泽
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Zhejiang University ZJU
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/09—Mixtures of metallic powders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F12/00—Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
    • B22F12/50—Means for feeding of material, e.g. heads
    • B22F12/58—Means for feeding of material, e.g. heads for changing the material composition, e.g. by mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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Abstract

The application discloses a preparation method of a titanium alloy with continuously adjustable phase structure, which comprises the steps of mixing TA15 powder and 316L powder to obtain mixed powder, wherein the content of the 316L powder in the mixed powder is 1-9 wt%; ball milling, drying and sieving the mixed powder to obtain mixed alloy powder; and depositing the mixed alloy powder on the substrate by a laser metal deposition method to obtain the titanium alloy. According to the application, the prepared titanium alloy can be continuously regulated and controlled from alpha phase to beta phase by gradually increasing the quantity of 316L powder, so that the accurate regulation and control of mechanical properties are realized, and the requirement of customizing the mechanical properties is met. The application also discloses the titanium alloy with the continuously adjustable phase structure, which is prepared by adopting the preparation method of the titanium alloy with the continuously adjustable phase structure.

Description

Titanium alloy with continuously adjustable phase structure and preparation method thereof
Technical Field
The invention belongs to the field of metal alloys, and particularly relates to a titanium alloy with continuously adjustable phase structure and a preparation method thereof.
Background
Titanium alloys are receiving extensive attention and research in the field of aerospace structural materials with their high specific strength, fracture toughness and excellent oxidation resistance. The titanium alloy also has higher damage tolerance and forging and casting performances. These outstanding advantages have led to the great use of titanium alloys in the aerospace industry, the chemical industry, transportation and marine shipping industries. TA15 (Ti-6.5 Al-2Zr-1 Mo-1V) is one of the most popular medium strength near alpha titanium alloys, which has good heat resistance and weldability as well as excellent machinability, and thus is widely used in the manufacture of welded structures, load bearing structures and large-scale integral parts. Compared with widely used alpha+beta dual-phase titanium alloy TC4 (Ti-6 Al-4V), TA15 has higher working temperature (450-500 ℃), and has better mechanical property at medium and high temperature.
The metal additive manufacturing technology is a rapid manufacturing and forming technology integrating CAD technology and path algorithm theory, can realize rapid free forming without a mould, can realize random composite manufacturing of multiple materials, and has the characteristics of full digitalization and high flexibility. Additive manufacturing is based on a 3D model, slice calculation and processing are carried out on the model through software, a layer-by-layer printing path is constructed, and a final alloy part is obtained through layer-by-layer stacking. The laser metal deposition technology is realized by taking laser as an energy source and feeding powder synchronously by argon. The technology has the advantages of atmosphere protection, simple and convenient operation, high molding efficiency, small size limitation of molded parts, material repair and the like. Additive manufacturing techniques, particularly laser metal Deposition (LASER METAL Deposition) techniques, have been considered in recent years as promising techniques for producing complex geometry parts required for large scale integration TA15 in the aerospace industry.
The titanium alloy has low heat conductivity, the traditional machining mode can cause the cutting temperature to be too high so as to damage a machining tool, and meanwhile, the traditional titanium alloy machining process has the defects of large path difficulty, difficult technology and high cost in economy, so that the wide production and application of the titanium alloy are limited. The LMD technology can effectively produce high-quality parts due to the characteristic of coaxial powder feeding, has less size limitation of formed parts, can form large complex parts and gradient materials, can realize nondestructive local repair of damaged parts, greatly widens the production, manufacturing and application range of the titanium alloy, and lays a good production and processing foundation for subsequent practical application of the titanium alloy.
The alpha and beta phases in the titanium alloy are taken as main constituent phases, and the existence form and the phase content of the alpha and beta phases in the alloy have important influence on the microstructure and the mechanical property of the titanium alloy. The regulation and control of the microstructure and mechanical properties of the titanium alloy are staged and spanned by the traditional processing technology and heat treatment system, and the regulation and control have the characteristics of large tissue and property span and obvious difference, so that the fine adjustment of the microstructure and the demanded customization of the mechanical properties are difficult to realize, and still face great challenges at present. At present, in the traditional process, the improvement mode of the microstructure and mechanical property of the material by finely adjusting alloy components causes the problem of localized difference of component segregation and mechanical property due to the difference of element addition, and the treatment method is complex and complicated and has poor effect, but cannot be well solved.
Therefore, how to realize accurate and continuous regulation of the microstructure and mechanical properties of the material through phase regulation is a key problem facing the current situation.
Disclosure of Invention
The application aims to provide a titanium alloy with continuously adjustable phase structure and a preparation method thereof, and the prepared titanium alloy can be continuously regulated and controlled from alpha phase to beta phase by gradually increasing the quantity of 316L powder, so that the accurate regulation and control of mechanical properties are realized, and the requirement of customizing mechanical properties is met.
In order to achieve the above object, the present application provides a method for preparing a titanium alloy with continuously adjustable phase structure, comprising:
Mixing TA15 powder and 316L powder to obtain mixed powder, wherein the content of the 316L powder in the mixed powder is 1-9 wt%;
ball milling, drying and sieving the mixed powder to obtain mixed alloy powder;
And depositing the mixed alloy powder on the substrate by a laser metal deposition method to obtain a titanium alloy, wherein the titanium alloy comprises an alpha phase and a beta phase, the volume fraction of the alpha phase continuously decreases with the increase of the content of 316L powder in the mixed powder, and the volume fraction of the beta phase continuously increases with the increase of the content of 316L powder in the mixed powder.
Further, when 316L powder accounts for 0wt.% a to less than or equal to 3wt.% of the mixed powder, the volume fraction of the alpha phase is 79.6 to 97.3%, and the volume fraction of the beta phase is 1.2 to 18.5%; when the content of the 316L powder accounting for the mixed powder is b,3wt.% is less than or equal to 7wt.%, the volume fraction of the alpha phase is 39.2 to 79.6 percent, and the volume fraction of the beta phase is 18.5 to 54.2 percent; when the content of 316L powder in the mixed powder is c,7wt.% < c less than or equal to 9wt.%, the volume fraction of alpha phase is 0.9-39.2%, and the volume fraction of beta phase is 54.2-97.3%.
Further, when 316L powder accounts for 0wt.% a.ltoreq.3 wt.% of the mixed powder, the titanium alloy deposited on the substrate by the laser metal deposition method is a near-alpha titanium alloy; when the content of 316L powder accounting for the mixed powder is b,3wt.% is less than or equal to 7wt.%, and the titanium alloy deposited on the substrate by a laser metal deposition method is alpha+beta dual-phase titanium alloy; when the content of 316L powder in the mixed powder is c,7wt.% less than or equal to 9wt.%, the titanium alloy deposited on the substrate by the laser metal deposition method is a near-beta titanium alloy.
Further, when 316L powder accounts for 0 < a.ltoreq.3 wt.% of the mixed powder, the tensile strength of the titanium alloy deposited on the substrate by the laser metal deposition method is 968-1388 MPa; when the content of the 316L powder accounting for the mixed powder is b which is more than or equal to 3 and less than or equal to 7 wt%, the tensile strength of the titanium alloy deposited on the substrate by a laser metal deposition method is 1430-1556 MPa; when the content of the 316L powder accounting for the mixed powder is c, c is more than 7 and less than or equal to 9 wt%, the tensile strength of the titanium alloy deposited on the substrate by the laser metal deposition method is 1022-1148 MPa.
Further, when 316L powder accounts for 0wt.% a.ltoreq.3 wt.% of the mixed powder, the initial beta grain size of the titanium alloy deposited on the substrate by the laser metal deposition method is 86-125 μm; when the content of the 316L powder accounting for the mixed powder is b,3wt.% is less than or equal to 7wt.%, the initial beta grain size of the titanium alloy deposited on the substrate by a laser metal deposition method is 46-89 mu m; when the content of 316L powder in the mixed powder is c,7wt.% less than or equal to 9wt.%, the initial beta grain size of the titanium alloy deposited on the substrate by the laser metal deposition method is 38-49 mu m.
According to the laser metal deposition method provided by the embodiment of the application, mixed alloy powder is converted into titanium alloy from high temperature to low temperature, the phase conversion mode is that beta phase is converted into alpha phase at high temperature, when a small amount of 316L is added, most of beta phase is converted into alpha phase, the titanium alloy formed at normal temperature is near alpha type titanium alloy, as the content of 316L in the mixed alloy powder is increased, beta phase stabilizing element is continuously increased, beta phase is relatively stable, so that the beta phase is gradually reduced and converted into alpha phase, namely the volume fraction of alpha phase of the titanium alloy formed at normal temperature is continuously reduced along with the increase of the content of 316L powder in the mixed powder, and the volume fraction of beta phase is continuously increased along with the increase of the content of 316L powder in the mixed powder.
Since the initial beta-phase grain boundaries formed by the mixed alloy powder provided by the embodiment of the application at the high temperature of laser irradiation are also reserved at normal temperature, the embodiment of the application describes the grain size based on the initial beta-phase grains formed by the initial beta-phase grain boundaries, and the phenomenon that the initial beta-phase grains are continuously reduced with the increase of the content of 316L powder in the mixed powder is shown.
According to the invention, by gradually increasing the content of 316L powder, the phase structure of the titanium alloy can be obviously and continuously changed, namely, the phase structure is converted from near alpha phase to alpha+beta phase, and then the phase structure is converted from alpha+beta phase to near beta phase, so that the corresponding mechanical property can be obtained, namely, the tensile strength is increased and then reduced, thereby realizing the precise regulation and control of the mechanical property, and the grain size can be regulated and controlled from 44-273 mu m.
316L not only realizes the component regulation and control of the titanium alloy, but also can effectively reduce the phase transition temperature T β of the beta-alpha phase of the titanium alloy, and cause component fluctuation in the solidification process, thereby having important influence on the nucleation growth of crystal grains. Along with the increase of the 316L addition amount, the beta phase region expands to the low temperature region, the phase transition point of the titanium alloy is continuously reduced, and the beta phase content which is reserved to the room temperature in the solidification process is continuously increased, so that the phase structure morphology of the titanium alloy is effectively regulated and controlled. Meanwhile, the rising of the addition amount causes component fluctuation, leads the crystallization nucleation of the high-melting-point phase to be separated out in advance, prevents nucleation and growth of the subsequent phase, plays a role in refining grains, and influences the mechanical property of the titanium alloy.
Further, the mixed powder is subjected to ball milling, wherein the ball milling process comprises the following steps: the steel ball is made of 316L, the diameter of the steel ball is 3-6mm, the ball milling rotating speed is 150-250 r/min, and the ball milling time is 2-4 h.
Further, the mass ratio of the mixed powder to the steel ball is 1:2-4.
Further, the specific steps of drying the mixed powder after ball milling are as follows:
Placing the ball-milled mixed powder into a vacuum drying container, vacuumizing until the pressure in the container is less than 1Pa, and drying at 120 ℃ for 6-10 h.
Further, the screen mesh number of the screen powder is 80-200 meshes.
Further, the substrate is sequentially polished and cleaned before the mixed alloy powder is deposited on the substrate. The flat and bright substrate surface is obtained by polishing and cleaning.
Further, the substrate is a TC4 substrate, and the thickness is 10-20 mm.
Further, the technological parameters of the laser technology deposition method are as follows: the laser power is 500-1000W, the scanning speed is 400-1000 mm/min, the path interval of laser scanning is set to 40-60% of the cross section size of the single-channel molten pool, the slice layer thickness is set to 60-80% of the cross section size of the single-channel molten pool, and the powder feeding speed is fixed to 5-8 g/min.
On the other hand, the application also provides the titanium alloy with the continuously adjustable phase structure, which is prepared by adopting the preparation method of the titanium alloy with the continuously adjustable phase structure.
Compared with the prior art, the invention has the beneficial effects that:
According to the invention, by mixing 1-9 wt.% of 316L (022 Cr17Ni12Mo 2) powder in TA15 (Ti-6.5 Al-2 Zr-Mo-V) powder, the beta phase transition temperature of the alloy is effectively reduced by adding beta phase stabilizing elements, the microstructure of the titanium alloy is obviously regulated, and meanwhile, the obvious changes of the alpha/beta phase content, the tensile strength and the elongation are realized through continuous regulation and control of the microstructure of the titanium alloy. The laser alloying of the reasonable addition of beta-phase elements such as Fe, cr, ni and the like in TA15 successfully realizes the precise regulation and control of the microstructure and mechanical properties of the titanium alloy. The preparation method has universality, can be popularized to the regulation and control of microstructure and mechanical properties of similar near alpha titanium alloy, and has the advantages of simple and convenient preparation process, short production period and high repeatability.
Drawings
FIG. 1 is a back-scattered electron (BSE) microstructure of the titanium alloy blocks prepared in examples 1-5 and comparative example 1 of the present application at the same magnification;
FIG. 2 is an XRD pattern of the titanium alloy blocks prepared in examples 1-5 and comparative example 1 of the present application;
FIG. 3 is a DSC of a titanium alloy block prepared in examples 1-5 of the present application and comparative example 1;
FIG. 4 is a graph showing the mechanical properties of the titanium alloy blocks prepared in examples 1 to 5 and comparative example 1 according to the present application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments.
Example 1
TA15 powder and 316L powder are obtained as powder raw materials for laser metal deposition, and the particle size of the powder is 45-150 mu m.
The mass of TA15 powder is 198g, mixing TA15 powder and 316L powder, wherein the content of the 316L powder is 1 wt%, putting a 316L steel ball with the diameter phi of 5mm into a stainless steel ball grinding tank, the mass ratio of the steel ball to the alloy powder is 5:2, and then putting the mixed powder into the stainless steel ball grinding tank for ball grinding at the speed of 200r/min for 3h.
Placing the mixed powder obtained after ball milling into a vacuum drying oven, vacuumizing until the pressure in the oven is less than 1Pa, the drying temperature is 120 ℃, the drying time is 8 hours, sieving the powder twice by using a screen with the aperture of 100 meshes after the drying is finished, and then loading the mixed powder into a powder feeder.
Taking 10 x 10cm of TC4 substrate with the thickness of 10mm, polishing the surface by sand paper to expose a flat and bright upper surface, cleaning and drying the polished upper surface by ethanol, and then placing the polished upper surface into laser additive manufacturing equipment.
Setting the laser power of laser metal deposition to be 800W and the scanning speed to be 600mm/min; scanning a single channel in advance, measuring the cross section size of a molten pool, setting the path distance to be 1.262mm according to the size of the single channel molten pool, setting the slice thickness to be 0.682mm, and fixing the powder feeding speed to be 6g/min to prepare a multi-channel multilayer titanium alloy block without macroscopic cracks.
Example 2
TA15 powder and 316L powder are obtained as powder raw materials for laser metal deposition, and the particle size of the powder is 45-150 mu m.
Mixing TA15 powder with 316L powder with the mass of 194g, wherein the content of the 316L powder is 3 wt%, putting a 316L steel ball with the diameter phi of 5mm into a stainless steel ball grinding tank, putting the mixed powder into the stainless steel ball grinding tank for ball grinding at the speed of 200r/min for 3h, wherein the mass ratio of the steel ball to the alloy powder is 3:1.
Placing the mixed powder obtained after ball milling into a vacuum drying oven, vacuumizing until the pressure in the oven is less than 1Pa, the drying temperature is 120 ℃, the drying time is 8 hours, sieving the powder twice by using a screen with the aperture of 100 meshes after the drying is finished, and then loading the mixed powder into a powder feeder.
Taking 10 x 10cm of TC4 substrate with the thickness of 10mm, polishing the surface by sand paper to expose a flat and bright upper surface, cleaning and drying the polished upper surface by ethanol, and then placing the polished upper surface into laser additive manufacturing equipment.
Setting the laser power of laser metal deposition to be 800W and the scanning speed to be 900mm/min; scanning a single channel in advance, measuring the cross section size of a molten pool, setting the path distance to be 1.262mm according to the size of the single channel molten pool, setting the slice thickness to be 0.682mm, and fixing the powder feeding speed to be 5g/min to prepare a multi-channel multilayer titanium alloy block without macroscopic cracks.
Example 3
TA15 powder and 316L powder are obtained as powder raw materials for laser metal deposition, and the particle size of the powder is 45-150 mu m.
Mixing TA15 powder with 316L powder with the mass of 190g, wherein the content of the 316L powder is 5wt%, putting a 316L steel ball with the diameter phi of 5mm into a stainless steel ball grinding tank, putting the mixed powder into the stainless steel ball grinding tank for ball grinding at the speed of 200r/min for 3h, wherein the mass ratio of the steel ball to the alloy powder is 5:2.
Placing the mixed powder obtained after ball milling into a vacuum drying oven, vacuumizing until the pressure in the oven is less than 1Pa, the drying temperature is 120 ℃, the drying time is 8 hours, sieving the powder twice by using a screen with the aperture of 100 meshes after the drying is finished, and then loading the mixed powder into a powder feeder.
Taking 10 x 10cm of TC4 substrate with the thickness of 10mm, polishing the surface by sand paper to expose a flat and bright upper surface, cleaning and drying the polished upper surface by ethanol, and then placing the polished upper surface into laser additive manufacturing equipment.
Setting the laser power of laser metal deposition to be 800W and the scanning speed to be 600mm/min; scanning a single channel in advance, measuring the cross section size of a molten pool, setting the path distance to be 1.262mm according to the size of the single channel molten pool, setting the slice thickness to be 0.682mm, and fixing the powder feeding speed to be 6g/min to prepare a multi-channel multilayer titanium alloy block without macroscopic cracks.
Example 4
TA15 powder and 316L powder are obtained as powder raw materials for laser metal deposition, and the particle size of the powder is 45-150 mu m.
The mass of TA15 powder is 186g, mixing TA15 powder and 316L powder, wherein the content of the 316L powder is 7 wt%, putting a 316L steel ball with the diameter phi of 5mm into a stainless steel ball grinding tank, the mass ratio of the steel ball to the alloy powder is 5:2, and then putting the mixed powder into the stainless steel ball grinding tank for ball grinding at the speed of 200r/min for 3h.
Placing the mixed powder obtained after ball milling into a vacuum drying oven, vacuumizing until the pressure in the oven is less than 1Pa, the drying temperature is 120 ℃, the drying time is 8 hours, sieving the powder twice by using a screen with the aperture of 100 meshes after the drying is finished, and then loading the mixed powder into a powder feeder.
Taking 10 x 10cm of TC4 substrate with the thickness of 10mm, polishing the surface by sand paper to expose a flat and bright upper surface, cleaning and drying the polished upper surface by ethanol, and then placing the polished upper surface into laser additive manufacturing equipment.
Setting the laser power of laser metal deposition to be 800W and the scanning speed to be 600mm/min; scanning a single channel in advance, measuring the cross section size of a molten pool, setting the path distance to be 1.262mm according to the size of the single channel molten pool, setting the slice thickness to be 0.682mm, and fixing the powder feeding speed to be 6g/min to prepare a multi-channel multilayer titanium alloy block without macroscopic cracks.
Example 5
TA15 powder and 316L powder are obtained as powder raw materials for laser metal deposition, and the particle size of the powder is 45-150 mu m.
Mixing TA15 powder with 316L powder with the mass of 182g, wherein the content of the 316L powder is 9 wt%, putting a 316L steel ball with the diameter phi of 5mm into a stainless steel ball grinding tank, putting the mixed powder into the stainless steel ball grinding tank for ball grinding at the speed of 200r/min for 3h, wherein the mass ratio of the steel ball to the alloy powder is 5:2.
Placing the mixed powder obtained after ball milling into a vacuum drying oven, vacuumizing until the pressure in the oven is less than 1Pa, the drying temperature is 120 ℃, the drying time is 8 hours, sieving the powder twice by using a screen with the aperture of 100 meshes after the drying is finished, and then loading the mixed powder into a powder feeder.
Taking 10 x 10cm of TC4 substrate with the thickness of 10mm, polishing the surface by sand paper to expose a flat and bright upper surface, cleaning and drying the polished upper surface by ethanol, and then placing the polished upper surface into laser additive manufacturing equipment.
Setting the laser power of laser metal deposition to be 800W and the scanning speed to be 600mm/min; scanning a single channel in advance, measuring the cross section size of a molten pool, setting the path distance to be 1.262mm according to the size of the single channel molten pool, setting the slice thickness to be 0.682mm, and fixing the powder feeding speed to be 6g/min to prepare a multi-channel multilayer titanium alloy block without macroscopic cracks.
Comparative example 1
In contrast to the implementation, 316L of powder was not added.
Performance comparison:
Referring to fig. 1, fig. 1 shows the structure patterns of comparative example 1, examples 1 to 5, wherein (a) of fig. 1 is the structure pattern of the titanium alloy block prepared in comparative example 1, fig. 1 (b) is the structure pattern of the titanium alloy block prepared in example 1, fig. 1 (c) is the structure pattern of the titanium alloy block prepared in example 2, fig. 1 (d) is the structure pattern of the titanium alloy block prepared in example 3, fig. 1 (e) is the structure pattern of the titanium alloy block prepared in example 4, and fig. 1 (f) is the structure pattern of the titanium alloy block prepared in example 5, and grain boundaries of initial β grains remain in a series of alloys, the main components of which are α phases, and as the addition amount of 316L increases, the initial β grains are significantly increased in number of grains and the density of grain boundaries are refined with the same magnification. Grain size statistics find that the initial beta grain size refines from 273 μm to 44 μm, indicating that the addition of 316L can effectively refine the grain size of the titanium alloy.
Referring to fig. 2, fig. 2 shows XRD curves of comparative example 1 and example 5, wherein the curve corresponding to TA15 is an XRD curve when 316L is not added, the curve corresponding to TA15-1 is an XRD curve when 316L is added to 1wt.% of the mixed powder, the curve corresponding to TA15-3 is an XRD curve when 316L is added to 3wt.% of the mixed powder, the curve corresponding to TA15-5 is an XRD curve when 316L is added to 5wt.% of the mixed powder, the curve corresponding to TA15-7 is an XRD curve when 316L is added to 7wt.% of the mixed powder, and the curve corresponding to TA15-9 is an XRD curve when 316L is added to 9wt.% of the mixed powder, as shown in fig. 2, with an increase in the 316L addition amount, a continuous transition from the near alpha phase to the alpha+beta phase is realized in the XRD curve, and an increase in the beta phase peak intensity represented by 39.5 ° and a decrease in the peak intensity of 40 ° can be observed. This phenomenon is mainly caused by the fact that the beta-phase region is enlarged due to the addition of the beta-phase stabilizing element in 316L, so that the beta-phase region is not converted into alpha phase after the solidification process, and the original beta-phase is reserved. The volume fractions of the α phase and the β phase corresponding to the above samples are shown in the following table, and it can be seen that as the addition amount of 316L increases, the volume fraction of the α phase continuously decreases and the volume fraction of the β phase continuously increases.
TABLE 1 alpha/beta phase volume fraction summary table
Referring to fig. 3, fig. 3 shows DSC curves of comparative example 1, examples 1 to 5. Wherein the curve corresponding to TA15 is a DSC curve when 316L is not added, the curve corresponding to TA15-1 is a DSC curve when 316L is added and accounts for 1wt.% of the mixed powder, the curve corresponding to TA15-3 is a DSC curve when 316L is added and accounts for 3wt.% of the mixed powder, the curve corresponding to TA15-5 is a DSC curve when 316L is added and accounts for 5wt.% of the mixed powder, the curve corresponding to TA15-7 is a DSC curve when 316L is added and accounts for 7wt.% of the mixed powder, and the curve corresponding to TA15-9 is a DSC curve when 316L is added and accounts for 9wt.% of the mixed powder. As shown in fig. 3, as the 316L addition increases, the phase transition temperature of the material decreases continuously from 964.4 ℃ at the initial 0wt.% addition to 730.1 ℃ at the 9wt.% addition, mainly because the elements such as Fe, cr, ni and the like in the 316L powder are all β -phase stabilizing elements, and after addition, the β -phase region in the titanium alloy phase diagram expands toward the low temperature region, thereby decreasing the phase transition temperature of the β - > α phase, which is shown in the DSC curve as a continuously decreasing phase transition temperature.
Referring to fig. 4, fig. 4 shows the tensile strength curves of comparative example 1, examples 1 to 5. Wherein the curve corresponding to TA15 is the tensile strength curve when 316L is not added, the curve corresponding to TA15-1 is the tensile strength curve when 316L is added and is 1wt.% of the mixed powder, the curve corresponding to TA15-3 is the tensile strength curve when 316L is added and is 3wt.% of the mixed powder, the curve corresponding to TA15-5 is the tensile strength curve when 316L is added and is 5wt.% of the mixed powder, the curve corresponding to TA15-7 is the tensile strength curve when 316L is added and is 7wt.% of the mixed powder, and the curve corresponding to TA15-9 is the tensile strength curve when 316L is added and is 9wt.% of the mixed powder. As shown in fig. 4, with the increase of the 316L addition amount, the tensile strength of the titanium alloy shows a trend of increasing and then decreasing, mainly because elements such as Fe, cr, ni and the like in the 316L powder enter β -Ti in a solid solution manner, so that the strength of the material is effectively improved. While with small additions (0 to 3 wt.%) a better adaptation of the strength and plasticity of the titanium alloy is achieved, the elongation of the material is not significantly reduced while the strength is significantly improved. In the addition amount stage of 3 to 5wt.%, the elongation of the titanium alloy is remarkably reduced mainly due to the addition of beta stabilizing elements such as Fe, cr, ni and the like, the beta phase content in the titanium alloy matrix is improved, and meanwhile, the beta phase in the initial beta crystal grains is strengthened, so that the difference of mechanical properties between the inside of the crystal grains and the crystal boundary is caused: when the tensile loading process is carried out, dislocation inside the beta grains can smoothly pass through, but a large amount of dislocation gathers and entangles at the grain boundary, so that stress concentration at the grain boundary is caused, and the dislocation becomes a crack initiation point, which is a main reason for rapid material failure. As 316L continues to be added, the content of beta phase further increases, the suitability of mechanical properties at the grain interior and grain boundary continues to decrease, the mechanical properties of the material become worse, and a tensile property change curve as shown in fig. 4 is presented.

Claims (7)

1. A method for preparing a titanium alloy with a continuously adjustable phase structure, which is characterized by comprising the following steps:
Mixing TA15 powder and 316L powder to obtain mixed powder, wherein the content of the 316L powder in the mixed powder is 1-9 wt%;
ball milling, drying and sieving the mixed powder to obtain mixed alloy powder;
Depositing mixed alloy powder on a substrate by a laser metal deposition method to obtain a titanium alloy, wherein the titanium alloy comprises an alpha phase and a beta phase, the volume fraction of the alpha phase is continuously reduced along with the increase of the content of 316L powder in the mixed powder, and the volume fraction of the beta phase is continuously increased along with the increase of the content of 316L powder in the mixed powder;
when the content of 316L powder accounting for the mixed powder is a, 0wt percent of the mixed powder is less than or equal to 3 percent by weight, the titanium alloy is near alpha titanium alloy;
When the content of the 316L powder accounting for the mixed powder is b, 3wt percent of b is less than or equal to 7 percent and wt percent, the titanium alloy is alpha+beta dual-phase titanium alloy;
When the content of the 316L powder accounting for the mixed powder is c,7 wt percent of c is less than or equal to 9 percent of wt percent, the titanium alloy is near beta titanium alloy;
when the content of 316L powder accounting for the mixed powder is a,0 wt percent of the mixed powder is less than or equal to 3 percent by weight, the initial beta grain size of the titanium alloy is 86-125 mu m;
when the content of the 316L powder accounting for the mixed powder is b, 3wt percent of b is less than or equal to 7 percent of wt percent, the initial beta grain size of the titanium alloy is 46-89 mu m;
When the content of the 316L powder accounting for the mixed powder is c,7 wt percent of c is less than or equal to 9 percent of wt percent, the initial beta grain size of the titanium alloy is 38-49 mu m;
The technological parameters of the laser metal deposition method are as follows: the laser power is 500-1000W, the scanning speed is 400-1000 mm/min, the path distance of laser scanning is set to 40-60% of the cross section size of the single-pass molten pool, the slice layer thickness is set to 60-80% of the cross section size of the single-pass molten pool, and the powder feeding speed is fixed to 5-8 g/min.
2. The method for producing a titanium alloy with a continuously adjustable phase structure according to claim 1, wherein when 316L of powder is a, 0wt wt.% < a > is not more than 3wt.% of the mixed powder, the volume fraction of the α phase is 79.6 to 97.3%, and the volume fraction of the β phase is 1.2 to 18.5%;
When the content of the 316L powder accounting for the mixed powder is b, 3wt percent of b is less than or equal to 7 percent and wt percent, the volume fraction of the alpha phase is 39.2 to 79.6 percent, and the volume fraction of the beta phase is 18.5 to 54.2 percent;
When the content of the 316L powder accounting for the mixed powder is c,7 wt percent of c is less than or equal to 9 percent and wt percent, the volume fraction of the alpha phase is 0.9-39.2 percent, and the volume fraction of the beta phase is 54.2-97.3 percent.
3. The method for producing a titanium alloy with a continuously adjustable phase structure according to claim 1, wherein when 316L powder is a,0 wt wt.% a is less than or equal to 3wt.% of the mixed powder, the tensile strength of the titanium alloy is 968 to 1388 MPa;
When the content of the 316L powder accounting for the mixed powder is b,3 wt percent of b is less than or equal to 7 percent and wt percent, the tensile strength of the titanium alloy is 1430-1556 MPa;
When the content of the 316L powder accounting for the mixed powder is c, 7-wt percent of c is less than or equal to 9-wt percent, the tensile strength of the titanium alloy is 1022-1148 MPa.
4. The method for preparing the titanium alloy with the continuously adjustable phase structure according to claim 1, wherein the mixed powder is subjected to ball milling, and the ball milling process is as follows: the steel ball is made of 316L, the diameter of the steel ball is 3-6 mm, the ball milling rotating speed is 150-250 r/min, and the ball milling time is 2-4 h.
5. The method for preparing the titanium alloy with the continuously adjustable phase structure according to claim 1, wherein the mass ratio of the mixed powder to the steel balls is 1:2-4.
6. The method for producing a titanium alloy with a continuously adjustable phase structure according to claim 1, wherein the mesh number of the sieve powder is 80 to 200 mesh.
7. A titanium alloy with continuously adjustable phase structure, which is prepared by the preparation method of the titanium alloy with continuously adjustable phase structure according to any one of claims 1-6.
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