CN116288090A - Process for improving metallurgical structure of titanium alloy bar friction stir additive manufacturing - Google Patents
Process for improving metallurgical structure of titanium alloy bar friction stir additive manufacturing Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
- B23K20/1215—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding for other purposes than joining, e.g. built-up welding
-
- 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
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0075—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for rods of limited length
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/08—Non-ferrous metals or alloys
- B23K2103/14—Titanium or alloys thereof
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- 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
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Abstract
The invention provides a process for improving metallurgical structure of titanium alloy bar friction stir additive manufacturing, which comprises the following steps: sequentially carrying out hydrogen placing treatment and high-temperature solution treatment on the first titanium alloy bar to obtain a second titanium alloy bar; taking a second titanium alloy bar as a raw material, adopting a friction stir additive manufacturing process, and depositing layer by layer in an upward growth mode from a first layer according to a preset program until a last layer is deposited to obtain a titanium alloy workpiece intermediate; and (3) annealing and dehydrogenation heat treatment are carried out on the intermediate of the titanium alloy workpiece, so that the required titanium alloy workpiece is obtained. According to the invention, the preprinted bar is subjected to high-temperature hydrogen placement, and then sealed for high-temperature solid solution, so that hydride is eliminated, the thermal deformation flow stress of the titanium alloy is reduced, and the thermoplasticity is increased, so that the hydrogen-placed titanium or titanium alloy is easy to deform at high temperature, the (alpha+beta)/beta transition temperature is effectively reduced, the stirring temperature is reduced, the processing performance is improved, the difficulty in subsequent stirring friction additive manufacturing is reduced, and the quality of a formed workpiece is improved.
Description
Technical Field
The invention relates to the technical field of additive manufacturing, in particular to a friction stir additive manufacturing technology of titanium alloy, and specifically relates to a process for improving metallurgical structure of friction stir additive manufacturing of titanium alloy bars.
Background
Metal additive manufacturing is a main branch of 3D printing technology, and generally adopts high energy beams (laser, electron beam, electric arc, plasma, etc.) as input heat sources, and performs layer-by-layer lamination of printed parts by melting discrete metal materials (powder materials and wires), so as to make up for the defects of traditional material reduction and equal material manufacturing. However, no matter how the forms of the light source and the product are changed, because the metal micro-area is rapidly heated under the action of a concentrated heat source in the additive manufacturing process, the metal micro-area is rapidly solidified by quenching, then the adjacent layer or layers are circularly remelted and cooled through multiple periods, variable cycles and intense heating and cooling in the layer-by-layer deposition process, and other deposited layer crystal grains are circularly micro-heat treated, so that the problems of poor metallurgical quality and coarse structure in the additive manufacturing exist.
Around the problem, scholars at home and abroad have conducted a great deal of exploratory research, and the problems of metallurgical structure of additive manufacturing are attempted to be solved by carrying out microstructure regulation and control in aspects of additive manufacturing technology, adding reinforced particles to refine grains, utilizing magnetic fields, electric fields, ultrasound, laser, micro forging and the like.
For example, chinese patent publication No. CN105483587a discloses a cyclic thermal hydrogen treatment process for improving the temperature plasticity of TC4 titanium alloy, which improves the ratio of α phase and β phase in TC4 titanium alloy by secondary hydrogen treatment, increases the content of β phase with better plasticity in the alloy, reduces the content of α' martensite, refines grains, and further improves the room temperature plasticity; after the secondary circulation thermal hydrogen treatment, the ultimate deformation rate of the TC4 titanium alloy is improved by 22.1 percent, the yield strength is reduced by 11.1 percent, and the yield ratio is reduced by 11.5 percent. However, the method is only a subsequent heat treatment process for the formed titanium alloy workpiece, the process is complicated, the problem of coarse structure caused by remelting cannot be solved from the source, and the refinement degree of grains is limited.
As another example, P.A. Kobryn et Al studied the law of columnar crystal generation by laser cladding of Ti-6Al-4V alloy, and the results show that high temperature gradient and large cooling rate are beneficial to the growth of columnar crystals, and high scanning speed can reduce the size of columnar crystals. But the control is carried out by the process, the tissue regulation is carried out from the angle of supercooling degree, high-energy heat sources such as additive manufacturing laser, electron beam and the like are heated, the solidification rate is 0.1m/s to 5m/s, the temperature gradient is already at a very high level, and fine grain strengthening is difficult to realize by adjusting process parameters.
Friction Stir Additive Manufacturing (FSAM) is a solid phase metal additive manufacturing that breaks through the inherent drawbacks of metal additive manufacturing melt joining. The material supply of the friction stir deposition material adding technology can be wires, powder, bars and the like, the wires cannot be fully rubbed with the substrate, the generated friction heat is less, the material cannot be fully plasticized, and the defects such as discontinuous deposition layer and the like often occur; when the main shaft rotates, the powder is not easy to control the deposition direction, the thickness of the deposition layer is uneven, and the discharge hole is easy to be blocked; when the metal bar is used as a feeding material, friction between the bar rotating at high speed and the substrate can generate a large amount of heat, so that the metal material is plasticized, the plasticized material is easier to control, and the molding effect is better. However, the titanium alloy has the characteristics of large yield ratio, large high-temperature deformation resistance, low plasticity and poor processability, and severely restricts the material-increasing efficiency and the material-increasing quality of friction stir deposition material-increasing.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a process for improving the metallurgical structure of titanium alloy bar friction stir additive manufacturing, which comprises the steps of placing hydrogen on a preprinted bar at high temperature, then sealing for high-temperature solid solution, eliminating hydride, reducing the thermal deformation flow stress of the titanium alloy, increasing the thermoplasticity, so that the hydrogen-placed titanium or the titanium alloy is easy to deform at high temperature, effectively reducing the (alpha+beta)/beta transition temperature, reducing the stirring temperature, improving the processing performance, reducing the difficulty of subsequent friction stir additive manufacturing, and improving the quality of formed workpieces.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a process for improving the metallurgical structure of a titanium alloy bar friction stir additive manufacturing comprising the steps of:
sequentially carrying out hydrogen placing treatment and high-temperature solution treatment on the first titanium alloy bar to obtain a second titanium alloy bar; the hydrogen placing treatment is to place the first titanium alloy bar in a heat treatment furnace, introduce hydrogen with a certain percentage of the weight of the first titanium alloy bar, then heat-preserving the bar, and cool the bar to room temperature;
taking a second titanium alloy bar as a raw material, adopting a friction stir additive manufacturing process, and depositing layer by layer in an upward growth mode from a first layer according to a preset program until a last layer is deposited to obtain a titanium alloy workpiece intermediate;
annealing and dehydrogenation heat treatment are carried out on the intermediate of the titanium alloy workpiece, so that the required titanium alloy workpiece is obtained;
wherein, the processing stress of the titanium alloy is reduced by hydrogen placing treatment and high-temperature solution treatment.
In an alternative embodiment, the specific process of the hydrogen placing treatment comprises:
placing the first titanium alloy bar into a tubular hydrogen-placing heat treatment furnace, and vacuumizing to 1.5 x 10 -3 Heating to 700-800 ℃ at the speed of 10-20 ℃/min after Pa, introducing hydrogen after 10-30 min of heat preservation, and cooling to room temperature at the speed of 5-15 ℃/min after 1-4h of heat preservation.
In an alternative embodiment, 0.1 to 0.8% hydrogen is charged based on the weight percent of the titanium alloy rod.
In an alternative embodiment, the specific process of high temperature solution treatment includes:
placing the first titanium alloy bar after hydrogen placement into a heat treatment furnace, and heating to the transformation temperature T at a speed of 10-20 ℃/min p- Preserving heat for 20-40 min at the temperature of +10 ℃, and then quenching.
In an alternative embodiment, the friction stir additive manufacturing process is configured to determine the titanium alloy bar feed rate based on the titanium alloy workpiece parameters, and the operating parameters of the stirring head, and to set a printing program based thereon to perform print forming of the workpiece.
In an alternative embodiment, the process parameters of friction stir additive manufacturing include:
the rotation speed of the stirring head ranges from 200r/min to 3000r/min, the advancing speed of the stirring head ranges from 1 mm/min to 200mm/min, the pressing amount is 0.1 mm/min to 8mm/min, the pressing force ranges from 10 KN to 500KN, and the feeding speed is 1 mm/min to 100mm/min.
In an alternative embodiment, the annealing and dehydrogenation heat treatment process comprises:
placing the titanium alloy workpiece intermediate into a vacuum heat treatment furnace, and vacuumizing to 1.5 x 10 -3 Pa, heating to 700-800 ℃ at a speed of 10-20 ℃/min, regulating the vacuum degree in the furnace, and keeping the vacuum degree in the furnace higher than 3 x 10 -3 Pa, preserving heat for 2-4 h, and cooling to room temperature at 5-15 ℃/min.
According to the technical scheme provided by the invention, the process for improving the metallurgical structure of the titanium alloy bar friction stir additive manufacturing is provided, firstly, hydrogen is placed on the preprinted bar at high temperature, the titanium alloy is in a state of low softening temperature and low flow stress through hydrogen placing treatment, after temporary alloying of the hydrogen, the diffusion of elements in the titanium alloy can be promoted, the phase transition temperature is obviously reduced, the capability of hydrogen induced high temperature plasticity is provided, the processing stress of the titanium alloy can be effectively reduced, and the difficulty of subsequent friction stir additive manufacturing is reduced.
And in the subsequent process, the stirring head is used for causing severe plastic deformation, mixing and crushing of materials in a processing area, so that the refining, homogenizing and densification of the microstructure of the materials are realized, coarse grain structures caused by rapid heating and rapid solidification of the traditional cladding-based metal additive manufacturing technology are avoided, and the mechanical properties of the workpiece are improved.
Drawings
FIG. 1 is a process flow diagram of a process for improving the metallurgical structure of a titanium alloy bar friction stir additive manufacturing of the present invention.
Fig. 2 is a schematic view of an example of a hydrogen placing treatment of a titanium alloy bar of the present invention.
FIG. 3 is a schematic illustration of an example friction stir additive manufacturing process of the present invention.
FIG. 4 is a microscopic view showing the microstructure of the titanium alloy workpiece obtained in example 1 of the present invention.
FIG. 5 is a microscopic view showing the microstructure of the titanium alloy workpiece obtained in example 2 of the present invention.
FIG. 6 is a microscopic view showing the microstructure of the titanium alloy workpiece obtained in example 3 of the present invention.
FIG. 7 is a microscopic view showing the microstructure of the titanium alloy workpiece obtained in example 4 of the present invention.
FIG. 8 is a microscopic view showing the microstructure of the titanium alloy workpiece obtained in example 5 of the present invention.
FIG. 9 is a microscopic view showing the microstructure of the titanium alloy workpiece obtained in example 6 of the present invention.
FIG. 10 is a microscopic view showing the microstructure of the titanium alloy workpiece obtained in comparative example 1 of the present invention.
FIG. 11 is a microscopic view showing the microstructure of the titanium alloy workpiece obtained in comparative example 2 of the present invention.
FIG. 12 is a microscopic view showing the microstructure of the titanium alloy workpiece obtained in comparative example 3 of the present invention.
Detailed Description
For a better understanding of the technical content of the present invention, specific examples are set forth below, along with the accompanying drawings.
Aspects of the invention are described in this disclosure with reference to the drawings, in which are shown a number of illustrative embodiments. The embodiments of the present disclosure are not necessarily intended to include all aspects of the invention. It should be appreciated that the various concepts and embodiments described above, as well as those described in more detail below, may be implemented in any of a wide variety of ways.
The working principle of the friction stir material additive manufacturing technology is that a metal material is conveyed to the surface of a substrate through the inside of a hollow main shaft which rotates, the metal material and the substrate generate intense friction to generate friction heat, the friction heat plastically softens the metal material, the plasticized material is combined with the substrate under the forging and pressing force of a shaft shoulder to form a first layer of deposition layer, and subsequent layers are continuously added on the initial layer along with the movement of the hollow shaft, so that the three-dimensional solid part is finally formed. The technology realizes the refinement, homogenization and densification of the microstructure of the material by causing severe plastic deformation, mixing and crushing of the material in the processing area through the stirring head. Because the solid phase deposition is adopted, the friction heat does not reach the melting point of the material, the material has no melting and solidification defects such as pore, shrinkage, dilution, element segregation, thermal cracking and the like, the material adding efficiency is high, the residual stress is small, and the compactness and uniformity of the part are good.
Based on the method, the invention provides a process for improving the metallurgical structure of titanium alloy bar friction stir additive manufacturing, which comprises the steps of obtaining a hydrogen-containing titanium alloy bar after the preposed titanium alloy bar is subjected to hydrogen-containing treatment, and then carrying out high-temperature solution treatment on the hydrogen-containing titanium alloy bar so as to improve the shaping of the hydrogen-containing printing bar special for additive manufacturing; and then carrying out friction stir additive manufacturing by utilizing the solid-solution titanium alloy bar to obtain a titanium alloy workpiece, and finally carrying out dehydrogenation heat treatment and annealing on the manufactured titanium alloy workpiece to refine and improve the microstructure of the titanium alloy workpiece manufactured by the friction stir additive.
In an exemplary embodiment of the invention, as shown in connection with fig. 1, a process for improving the metallurgical structure of a titanium alloy bar friction stir additive manufacturing is provided, comprising the steps of:
sequentially carrying out hydrogen placing treatment and high-temperature solution treatment on the first titanium alloy bar to obtain a second titanium alloy bar; the hydrogen placing treatment is to place the first titanium alloy bar in a heat treatment furnace, introduce hydrogen with a certain percentage of the weight of the first titanium alloy bar, heat preservation, and cool to room temperature.
And taking the second titanium alloy bar as a raw material, adopting a friction stir additive manufacturing process, and depositing layer by layer in an upward growth mode from the first layer according to a preset program until the last layer is deposited to obtain the titanium alloy workpiece intermediate.
And (3) annealing and dehydrogenation heat treatment are carried out on the intermediate of the titanium alloy workpiece, so that the required titanium alloy workpiece is obtained.
Wherein, the processing stress of the titanium alloy is reduced by hydrogen placing treatment and high-temperature solution treatment.
It will be appreciated that the first titanium alloy rod may be purchased or prepared directly by methods known in the art, for example, by proportioning the alloy components in mass percent, smelting in a high vacuum arc furnace, stirring thoroughly, casting into a titanium alloy ingot, and cutting or extruding into titanium alloy rods for use.
In an alternative embodiment, as shown in connection with fig. 2, the specific process of the hydrogen placement treatment includes:
placing the first titanium alloy bar 1 into a tubular hydrogen-placing heat treatment furnace 2, and vacuumizing to 1.5 x 10 -3 Heating to 700-800 ℃ at the speed of 10-20 ℃/min after Pa, introducing hydrogen after 10-30 min of heat preservation, and cooling to room temperature at the speed of 5-15 ℃/min after 1-4h of heat preservation.
In an alternative embodiment, 0.1 to 0.8% hydrogen is charged based on the weight percent of the titanium alloy rod.
In an alternative embodiment, the specific process of high temperature solution treatment includes:
placing the first titanium alloy bar after hydrogen placement into a heat treatment furnace, and heating to the transformation temperature T at a speed of 10-20 ℃/min p- Preserving heat for 20-40 min at the temperature of +10 ℃, and then quenching.
In a preferred embodiment, as shown in fig. 3, the stirring head 3 for stirring and rubbing treatment may be constructed by a conventional stirring and rubbing head, in which a cylindrical second titanium alloy bar 4 is provided at the center, the second titanium alloy bar is sent to a position below the stirring head 3, and stirring and rubbing treatment is performed by a stirring pin provided at the lower end of the stirring head 3.
As in the embodiment shown in fig. 3, an example is exemplarily shown in which a cylindrical channel of metal bar is provided in the stirring head 3, and a deposition layer 6 is deposited layer by layer in an upward growth manner on the substrate 5.
In an alternative embodiment, the friction stir additive manufacturing process is configured to determine the titanium alloy bar feed rate based on the titanium alloy workpiece parameters, and the operating parameters of the stirring head, and to set a printing program based thereon to perform print forming of the workpiece.
In an alternative embodiment, the process parameters of friction stir additive manufacturing include:
the rotation speed of the stirring head ranges from 200r/min to 3000r/min, the advancing speed of the stirring head ranges from 1 mm/min to 200mm/min, the pressing amount is 0.1 mm/min to 8mm/min, the pressing force ranges from 10 KN to 500KN, and the feeding speed is 1 mm/min to 100mm/min.
In an alternative embodiment, the annealing and dehydrogenation heat treatment process comprises:
placing the titanium alloy workpiece intermediate into a vacuum heat treatment furnace, and vacuumizing to 1.5 x 10 -3 Pa, heating to 700-800 ℃ at a speed of 10-20 ℃/min, regulating the vacuum degree in the furnace, and keeping the vacuum degree in the furnace higher than 3 x 10 -3 Pa, preserving heat for 2-4 h, and cooling to room temperature at 5-15 ℃/min; the hydrogen is removed by vacuum annealing to avoid the change of chemical components of the final bar, thereby achieving the aim of improving the structure without changing the alloy components.
For a better understanding, the present invention will be further described with reference to several specific examples, but the processing technique is not limited thereto, and the present invention is not limited thereto.
The workpieces printed in the following examples and comparative examples were rectangular parallelepiped titanium alloy workpieces of 80mm×60mm×4 mm.
Example 1
The titanium alloy bars used were TC4 and the compositions are shown in Table 1:
TABLE 1
| Ti | C | N | H | O | Al | V | |
| Composition of the components | Remainder material | 0.10 | 0.05 | 0.015 | 0.20 | 5.5 | 3.5 |
1) Carrying out hydrogen placing treatment on TC4 titanium alloy bar (with the diameter of 12mm and the length of 60 mm), placing the titanium alloy bar into a tubular hydrogen placing heat treatment furnace, and vacuumizing to 1.5 x 10 -3 Pa, heating to 750 ℃ at a speed of 10 ℃/min, preserving heat for 20min, filling 0.2% of hydrogen according to the weight percentage of the titanium alloy bar, preserving heat for 3h, and then cooling to room temperature at a speed of 10 ℃/min to obtain the hydrogen-placing materialTitanium alloy bar.
2) Carrying out solution heat treatment on the hydrogen-bearing titanium alloy bar, wherein the specific heat treatment process comprises the following steps: and (3) putting the bar into a heat treatment furnace, heating to 1008 ℃ at the speed of 10 ℃/min, preserving heat for 30min, and then quenching.
3) And (5) using the titanium alloy bar after solid solution to manufacture an additive to obtain a titanium alloy workpiece.
By adopting the friction stir material increasing manufacturing process, the rotation speed of the stirring head is 1200r/min, the advancing speed of the stirring head is 120mm/min, the pressing amount is 0.8mm/min, the pressing down force is 50KN, and the feeding speed is 100mm/min.
4) Annealing and dehydrogenation heat treatment are carried out on the manufactured titanium alloy workpiece; placing the titanium alloy workpiece into a vacuum heat treatment furnace, and vacuumizing to 1.5×10 -3 Pa, heating to 750 ℃ at a rate of 10 ℃/min. The vacuum degree in the furnace is higher than 3 x 10 -3 Pa, incubating for 3h, and then cooling to room temperature at 10deg.C/min.
Example 2
1) Carrying out hydrogen placing treatment on TC4 titanium alloy bar (with the diameter of 12mm and the length of 60 mm), placing the titanium alloy bar into a tubular hydrogen placing heat treatment furnace, and vacuumizing to 1.5 x 10 -3 Pa, heating to 750 ℃ at the speed of 10 ℃/min, preserving heat for 20min, filling 0.4% of hydrogen according to the weight percentage of the titanium alloy bar, preserving heat for 3h, and then cooling to room temperature at the speed of 10 ℃/min to obtain the hydrogen-containing titanium alloy bar.
2) Carrying out solution heat treatment on the TC4 titanium alloy bar, wherein the specific heat treatment process comprises the following steps: and (3) putting the bar into a heat treatment furnace, heating to 1008 ℃ at the speed of 10 ℃/min, preserving heat for 30min, and then quenching.
3) And (3) using the solid-dissolved titanium alloy bar for friction stir additive manufacturing to obtain the titanium alloy workpiece.
The stirring friction process is adopted, the rotation speed of the stirring head is 1000r/min, the advancing speed of the stirring head is 100mm/min, the pressing amount is 1.2mm/min, the downward pressure is 40KN, and the feeding speed is 80mm/min.
4) Annealing the manufactured titanium alloy workpiece; placing the titanium alloy workpiece into a vacuum heat treatment furnace, and vacuumizing to 1.5 x 10 -3 Pa, heating to 750 ℃ at a rate of 10 ℃/min. The vacuum degree in the furnace is higher than 3 x 10 -3 Pa, incubating for 3h, and then cooling to room temperature at 10deg.C/min.
Example 3
1) Carrying out hydrogen placing treatment on TC4 titanium alloy bar (with the diameter of 12mm and the length of 60 mm), placing the titanium alloy bar into a tubular hydrogen placing heat treatment furnace, and vacuumizing to 1.5 x 10 -3 Pa, heating to 750 ℃ at the speed of 10 ℃/min, preserving heat for 20min, filling 0.5% of hydrogen according to the weight percentage of the titanium alloy bar, preserving heat for 3h, and then cooling to room temperature at the speed of 10 ℃/min to obtain the hydrogen-containing titanium alloy bar.
2) Carrying out solution heat treatment on the TC4 titanium alloy bar, wherein the specific heat treatment process comprises the following steps: and (3) putting the bar into a heat treatment furnace, heating to 1008 ℃ at the speed of 10 ℃/min, preserving heat for 30min, and then quenching.
3) And (3) using the solid-dissolved titanium alloy bar for friction stir additive manufacturing to obtain the titanium alloy workpiece.
The stirring friction process is adopted, the rotation speed of the stirring head is 800r/min, the advancing speed of the stirring head is 80mm/min, the pressing amount is 1.5mm/min, the pressing down force is 30KN, and the feeding speed is 60mm/min.
4) Annealing the manufactured titanium alloy workpiece; placing the titanium alloy workpiece into a vacuum heat treatment furnace, and vacuumizing to 1.5×10 -3 Pa, heating to 750 ℃ at a rate of 10 ℃/min. The vacuum degree in the furnace is higher than 3 x 10 -3 Pa, incubating for 2-4 h, and then cooling to room temperature at 10deg.C/min.
Example 4
1) Carrying out hydrogen placing treatment on TC4 titanium alloy bar (with the diameter of 12mm and the length of 60 mm), placing the titanium alloy bar into a tubular hydrogen placing heat treatment furnace, and vacuumizing to 1.5 x 10 -3 Pa, heating to 750 ℃ at the speed of 10 ℃/min, preserving heat for 20min, filling 0.8% of hydrogen according to the weight percentage of the titanium alloy bar, preserving heat for 3h, and then cooling to room temperature at the speed of 10 ℃/min to obtain the hydrogen-containing titanium alloy bar.
2) Carrying out solution heat treatment on the TC4 titanium alloy bar, wherein the specific heat treatment process comprises the following steps: and (3) putting the bar into a heat treatment furnace, heating to 1008 ℃ at the speed of 10 ℃/min, preserving heat for 30min, and then quenching.
3) And (3) using the solid-dissolved titanium alloy bar for friction stir additive manufacturing to obtain the titanium alloy workpiece.
The stirring friction process is adopted, the rotation speed of the stirring head is 1100r/min, the advancing speed of the stirring head is 110mm/min, the pressing amount is 1.3mm/min, the pressing down force is 50KN, and the feeding speed is 90mm/min.
4) Annealing the manufactured titanium alloy workpiece; placing the titanium alloy workpiece into a vacuum heat treatment furnace, and vacuumizing to 1.5×10 -3 Pa, heating to 750 ℃ at a speed of 10-20 ℃/min. The vacuum degree in the furnace is higher than 3 x 10 -3 Pa, incubating for 3h, and then cooling to room temperature at 10deg.C/min.
Example 5
The titanium alloy bars used in this example were TA1 and the compositions shown in Table 2:
TABLE 2
| Ti | Fe | C | N | H | O | |
| Composition of the components | Remainder material | 0.066 | 0.016 | 0.0061 | 0.0007 | 0.10 |
1) Carrying out hydrogen placing treatment on a TA1 titanium alloy bar (with the diameter of 12mm and the length of 60 mm), placing the titanium alloy bar into a tubular hydrogen placing heat treatment furnace, and vacuumizing to 1.5x10 -3 Pa, heating to 700-800 ℃ at a speed of 15 ℃/min, preserving heat for 25min, filling 0.4% of hydrogen according to the weight percentage of the titanium alloy bar, preserving heat for 1-4h, and then cooling to room temperature at a speed of 15 ℃/min to obtain the hydrogen-containing titanium alloy bar.
2) Carrying out solution heat treatment on the TA1 titanium alloy bar, wherein the specific heat treatment process comprises the following steps: and (3) placing the bar into a heat treatment furnace, heating to 895 ℃ at a speed of 20 ℃/min, preserving heat for 30min, and then quenching.
3) And (3) using the solid-dissolved titanium alloy bar for friction stir additive manufacturing to obtain the titanium alloy workpiece.
The stirring friction process is adopted, the rotation speed of the stirring head is 1400r/min, the advancing speed of the stirring head is 140mm/min, the pressing amount is 1.2mm/min, the downward pressure is 40KN, and the feeding speed is 100mm/min.
4) Annealing the manufactured titanium alloy workpiece; placing the titanium alloy workpiece into a vacuum heat treatment furnace, and vacuumizing to 1.5×10 -3 Pa, heating to 750 ℃ at a rate of 20 ℃/min. The vacuum degree in the furnace is higher than 3 x 10 -3 Pa, incubating for 3h, and then cooling to room temperature at 10deg.C/min.
Example 6
The titanium alloy bars used in this example were TB2 and the compositions shown in Table 3:
TABLE 3 Table 3
| Ti | C | N | H | O | Al | V | Cr | Mo | |
| Composition of the components | Remainder material | ≤0.05 | ≤0.04 | ≤0.015 | ≤0.15 | 2.5-3.5 | 4.7-5.7 | 7.5-8.5 | 4.7-5.7 |
1) Hydrogen placing the TB2 titanium alloy bar (with the diameter of 12mm and the length of 60 mm), placing the titanium alloy bar into a tubular hydrogen placing heat treatment furnace, and vacuumizing to 1.5x10 DEG. -3 Pa, heating to 800 ℃ at a speed of 20 ℃/min, preserving heat for 30min, filling 0.4% of hydrogen according to the weight percentage of the titanium alloy bar, preserving heat for 4h, and then cooling to room temperature at a speed of 15 ℃/min to obtain the hydrogen-containing titanium alloy bar.
2) Carrying out solution heat treatment on the TB2 titanium alloy bar, wherein the specific heat treatment process comprises the following steps: and (3) putting the bar into a heat treatment furnace, heating to 790 ℃ at a speed of 20 ℃/min, preserving heat for 30min, and then quenching.
3) And (3) using the solid-dissolved titanium alloy bar for friction stir additive manufacturing to obtain the titanium alloy workpiece.
The stirring friction process is adopted, the rotation speed of the stirring head is 1300r/min, the advancing speed of the stirring head is 130mm/min, the pressing amount is 1.2mm/min, the downward pressure is 40KN, and the feeding speed is 100mm/min.
4) Annealing the manufactured titanium alloy workpiece; placing the titanium alloy workpiece into a vacuum heat treatment furnace, and vacuumizing to 1.5×10 -3 Pa, heating to 750 ℃ at a rate of 20 ℃/min. The vacuum degree in the furnace is higher than 3 x 10 -3 Pa, incubating for 3h, and then cooling to room temperature at 10deg.C/min.
Comparative example 1
1) The TC4 titanium alloy bar (with the diameter of 12mm and the length of 60 mm) is subjected to heat treatment, and the specific heat treatment process is as follows: and (3) putting the bar into a heat treatment furnace, heating to 1008 ℃ at the speed of 10 ℃/min, preserving heat for 30min, and then quenching.
2) And (3) using the solid-dissolved titanium alloy bar for friction stir additive manufacturing to obtain the titanium alloy workpiece.
The stirring friction process is adopted, the rotation speed of the stirring head is 1500r/min, the advancing speed of the stirring head is 80mm/min, the pressing amount is 2mm/min, the pressing force is 80KN, and the feeding speed is 60mm/min.
3) Annealing the manufactured titanium alloy workpiece; placing the titanium alloy workpiece into a vacuum heat treatment furnace, and vacuumizing to 1.5×10 -3 Pa, heating to 750 ℃ at a rate of 10 ℃/min. The vacuum degree in the furnace is higher than 3 x 10 -3 Pa, incubating for 3h, and then cooling to room temperature at 10deg.C/min.
Comparative example 2
1) TA1 titanium alloy bar (diameter is 12mm, length is 60 mm) is subjected to heat treatment, and the specific heat treatment process is as follows: and (3) putting the bar into a heat treatment furnace, heating to 895 ℃ at a speed of 15 ℃/min, preserving heat for 30min, and then quenching.
2) And (3) using the titanium alloy bar after heat treatment for friction stir additive manufacturing to obtain the titanium alloy workpiece.
The stirring friction process is adopted, the rotating speed range of the stirring head is 1800r/min, the advancing speed range of the stirring head is 80mm/min, the pressing amount is 2mm/min, the pressing down force is 100KN, and the feeding speed is 60mm/min.
4) Annealing the manufactured titanium alloy workpiece; placing the titanium alloy workpiece into a vacuum heat treatment furnace, and vacuumizing to 1.5×10 -3 Pa, heating to 750 ℃ at a rate of 20 ℃/min. The vacuum degree in the furnace is higher than 3 x 10 -3 Pa, incubating for 3h, and then cooling to room temperature at 10deg.C/min.
Comparative example 3
1) The TB2 titanium alloy bar (with the diameter of 12mm and the length of 60 mm) is subjected to heat treatment, and the specific heat treatment process comprises the following steps: and (3) putting the bar into a heat treatment furnace, heating to 790 ℃ at a speed of 20 ℃/min, preserving heat for 30min, and then quenching.
2) And (3) using the titanium alloy bar after heat treatment for friction stir additive manufacturing to obtain the titanium alloy workpiece.
By adopting a friction stir process, the rotation speed range of the stirring head is 1700r/min, the advancing speed range of the stirring head is 90mm/min, the pressing amount is 3mm/min, the pressing down force is 100KN, and the feeding speed is 60mm/min.
3) Annealing the manufactured titanium alloy workpiece; placing the titanium alloy workpiece into a vacuum heat treatment furnace, and vacuumizing to 1.5×10 -3 Pa, heating to 750 ℃ at a rate of 20 ℃/min. The vacuum degree in the furnace is higher than 3 x 10 -3 Pa, incubating for 3h, and then cooling to room temperature at 10deg.C/min.
Performance testing
The mechanical properties of the final titanium alloy metallurgical structures were tested and printed in the processes of examples 1-6 and comparative examples 1-3, and the results are shown in Table 4.
TABLE 4 mechanical Properties of titanium alloy workpieces
In the field of additive manufacturing, the formation of columnar crystals and coarse primary grains is rooted in thermodynamic power problems of metallurgical processes, supernormal metallurgical conditions and cyclic deposition in micro-melting pools of the additive manufacturing processes lead to insufficient temperature and component supercooling, and non-spontaneous nucleation point reduction is a core problem.
According to the method, the solubility of hydrogen in the titanium alloy is utilized to carry out hydrogen placing treatment on the titanium alloy bar, on one hand, hydrogen is an eutectoid reaction element of titanium, and coarse titanium alloy tissues can be thinned; on the other hand, the thermal deformation flow stress of the titanium alloy can be reduced by hydrogen placement, and the thermoplasticity is increased, so that the hydrogen placement titanium or the titanium alloy is easy to deform at high temperature, meanwhile, hydrogen is a beta phase stabilizing element, the (alpha+beta)/beta transition temperature can be effectively reduced, the stirring temperature can be reduced, the deformation degree of a die and the abrasion degree of the die are reduced, and the dimensional accuracy of the titanium alloy is further improved.
From the results in table 4, it can be seen that the hydrogen placement can very effectively refine grains during printing, improve the structure and improve the material performance; this is because the relationship between the strength of the alloy material and the grain size accords with the Hall-Petch relationship, the finer the grain is, the higher the strength of the alloy is, and only the grain is refined, the strength and the plasticity of the material can be improved at the same time. At the same time, the method does not change the components of the titanium alloy through the final dehydrogenation treatment. By combining the preparation processes of the embodiment and the comparative example, the method can be used for improving the processing performance of the titanium alloy and reducing the difficulty of titanium alloy friction stir additive manufacturing, wherein the titanium alloy has high strength and poor plasticity and obviously requires more intense stirring parameters to realize the additive manufacturing process when the hydrogen placing process is not adopted.
By combining the test results of examples 1-6, it can be seen that the hydrogen placing treatment is performed on different kinds of titanium alloy bars, hydrogen is used as a eutectoid reaction element of titanium, coarse titanium alloy structures can be still refined, so that grains of printing structures are refined, then the thermal deformation flow stress of the titanium alloy can be reduced by hydrogen placing, and the thermoplasticity is increased, so that the hydrogen placed titanium or titanium alloy is easy to deform at high temperature. However, the reinforcing effect was also different in the different types of titanium alloys, and it was apparent from the data that the (α+β) TC4 titanium alloy was more excellent in performance.
By combining the metallographic structure microscopic images and the mechanical property test results of the titanium alloy workpiece shown in fig. 4-12, it can be seen that the titanium alloy grain structure can be effectively refined under the condition of not changing the material composition by the friction stir additive manufacturing technology, and the grains can be stably kept in the workpiece by utilizing a preposed hydrogen placing process. As can be seen from the metallographic micrographs of the comparative examples and comparative examples, when the hydrogen-containing solution treatment was not employed, even though the titanium alloy formed fine-grain strengthening by plastic deformation, partial columnar grains were formed in the structure under the effect of high temperature.
According to the invention, the structure of the titanium alloy material is changed and the thermal deformation flow stress of the titanium alloy is reduced by the combined regulation and control of hydrogen placement and heat treatment of the titanium alloy bar, so that the hydrogen placement titanium or the titanium alloy is easy to deform at high temperature, meanwhile, hydrogen is a beta-phase stable element, the (alpha+beta)/beta transition temperature can be effectively reduced, the stirring temperature can be reduced, and the refinement, homogenization and densification of the microstructure of the material can be realized by combining with a friction stir additive manufacturing technology, so that a powerful guide is provided for the powerful development of the titanium alloy bar in the friction stir additive manufacturing in the future.
While the invention has been described with reference to preferred embodiments, it is not intended to be limiting. Those skilled in the art will appreciate that various modifications and adaptations can be made without departing from the spirit and scope of the present invention. Accordingly, the scope of the invention is defined by the appended claims.
Claims (7)
1. A process for improving the metallurgical structure of a titanium alloy bar friction stir additive manufacturing comprising the steps of:
sequentially carrying out hydrogen placing treatment and high-temperature solution treatment on the first titanium alloy bar to obtain a second titanium alloy bar; the hydrogen placing treatment is to place the first titanium alloy bar in a heat treatment furnace, introduce hydrogen with a certain percentage of the weight of the first titanium alloy bar, then heat-preserving the bar, and cool the bar to room temperature;
taking a second titanium alloy bar as a raw material, adopting a friction stir additive manufacturing process, and depositing layer by layer in an upward growth mode from a first layer according to a preset program until a last layer is deposited to obtain a titanium alloy workpiece intermediate;
annealing and dehydrogenation heat treatment are carried out on the intermediate of the titanium alloy workpiece, so that the required titanium alloy workpiece is obtained;
wherein, the processing stress of the titanium alloy is reduced by hydrogen placing treatment and high-temperature solution treatment.
2. The process for improving the metallurgical structure of friction stir additive manufacturing of titanium alloy bars according to claim 1, characterized in that the specific process of the hydrogen placing treatment comprises:
placing the first titanium alloy bar into a tubular hydrogen-placing heat treatment furnace, and vacuumizing to 1.5 x 10 -3 Heating to 700-800 ℃ at the speed of 10-20 ℃/min after Pa, introducing hydrogen after 10-30 min of heat preservation, and cooling to room temperature at the speed of 5-15 ℃/min after 1-4h of heat preservation.
3. Process for improving the metallurgical structure of a friction stir additive manufacturing of titanium alloy bars according to claim 1 or 2, characterized in that 0.1-0.8% of hydrogen is filled according to the weight percentage of the titanium alloy bars.
4. The process for improving the metallurgical structure of a titanium alloy bar friction stir additive manufacturing of claim 1, wherein the specific process of high temperature solution treatment comprises:
placing the first titanium alloy bar after hydrogen placement into a heat treatment furnace, and heating to the transformation temperature T at a speed of 10-20 ℃/min p- Preserving heat for 20-40 min at the temperature of +10 ℃, and then quenching.
5. The process for improving the metallurgical structure of a titanium alloy bar friction stir additive manufacturing process of claim 1, wherein the friction stir additive manufacturing process is configured to determine the titanium alloy bar feed rate based on titanium alloy workpiece parameters, and the operating parameters of the stirring head, and to set a printing program based thereon to perform a printing of the workpiece.
6. The process for improving the metallurgical structure of a titanium alloy bar friction stir additive manufacturing of claim 1, wherein the process parameters of friction stir additive manufacturing include:
the rotation speed of the stirring head ranges from 200r/min to 3000r/min, the advancing speed of the stirring head ranges from 1 mm/min to 200mm/min, the pressing amount is 0.1 mm/min to 8mm/min, the pressing force ranges from 10 KN to 500KN, and the feeding speed is 1 mm/min to 100mm/min.
7. The process for improving the metallurgical structure of a friction stir additive manufacturing of a titanium alloy bar of claim 1, wherein the annealing and dehydrogenation heat treatment process comprises:
placing the titanium alloy workpiece intermediate into a vacuum heat treatment furnace, and vacuumizing to 1.5 x 10 -3 Pa, heating to 700-800 ℃ at a speed of 10-20 ℃/min, regulating the vacuum degree in the furnace, and keeping the vacuum degree in the furnace higher than 3 x 10 -3 Pa, preserving heat for 2-4 h, and cooling to room temperature at 5-15 ℃/min.
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