CN113275600A - Heat treatment method for obtaining tri-state structure in SLM forming titanium alloy - Google Patents
Heat treatment method for obtaining tri-state structure in SLM forming titanium alloy Download PDFInfo
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Abstract
The invention belongs to the field of selective laser melting forming, and particularly discloses a heat treatment method for obtaining a tri-state structure in an SLM forming titanium alloy.
Description
Technical Field
The invention belongs to the field of selective laser melting and forming, and particularly relates to a heat treatment method for obtaining a tri-state structure in an SLM forming titanium alloy.
Background
The titanium alloy has the characteristics of small density, high specific strength, low elastic modulus, small heat conductivity coefficient, tensile strength close to yield strength, good heat resistance and low temperature resistance, good damping resistance and the like. Wherein the alpha + beta titanium alloy has excellent processing plasticity; the near-alpha titanium alloy has the advantages of both alpha titanium alloy and alpha + beta titanium alloy, excellent high temperature creep resistance, good heat strength, heat stability and weldability, and excellent processing plasticity. The long-term working temperature reaches more than 300 ℃, and the high-temperature-resistant material is widely applied to the fields of aerospace and navigation.
SLM (Selective laser melting) technology melts metal powder completely by a focused high-energy laser beam, cools and solidifies, and directly shapes metal pieces. Before the laser beam starts scanning in the device, the powder in the powder storage bin is firstly paved on a forming bin substrate through a horizontal scraper, and then the laser beam is controlled to selectively scan the powder on the outline of the powder layer slice according to a forming model designed by previous three-dimensional software, so that the powder is melted and solidified, and a continuous scanning line is formed, and the outline of the layer slice is formed. And then the lifting system is controlled to lower the forming platform by the height of one powder layer, and the powder storage bin is raised by the height of one powder layer. And then the scraper moves horizontally, powder with the height of one powder layer is flatly paved on the processed current layer, and scanning processing of the next layered slice is continued, so that the processing is performed circularly layer by layer until the whole formed part is processed. The SLM is an additive manufacturing technology which completely melts metal powder by using focused high-energy laser, and can directly form a metal part, thereby greatly reducing production steps, shortening production period and improving material utilization rate. In addition, due to the nature of layer-by-layer build-up manufacturing, there are great advantages to the formation of highly complex structures.
Under the action of a complex thermal force field in the SLM forming process, the formed near alpha and alpha + beta titanium alloy structure is in a coarse isometric crystal structure in the forming direction, is in a coarse columnar crystal structure penetrating through the whole plane in the direction vertical to the forming direction, is in a needle-like martensite structure inside the isometric crystal and the columnar crystal, and contains a large amount of deformation twin crystals and annealing twin crystals. Therefore, the SLM forming near alpha and alpha + beta titanium alloy shows extremely high tensile strength and poor plastic ductility in mechanical property, and the strength-plastic matching property is difficult to meet the use requirement.
It is known that the mechanical properties of the formed piece can be adjusted by changing the phase proportion, the grain size and the grain proportion of various shapes in the titanium alloy structure through heat treatment. Wu et Al studied the influence of heat treatment on the room temperature mechanical properties of SLM-formed near-alpha titanium alloy TA15(Ti-6Al-2Zr-1Mo-1V), found that the comprehensive mechanical properties obtained by holding at 750 ℃ for 2h and furnace cooling are optimal, and the tensile strength of the sample under the process conditions is reduced by 8.96% (up to 1123.6MPa) and the elongation is improved by 55% (up to 11.3 +/-0.7%) compared with that before heat treatment. Jiang et al studied the change in texture and properties of the SLM-formed TA15 titanium alloy before and after annealing, and found that the formed sample texture was lamellar with a 15.90% (up to 1090MPa) reduction in tensile strength and 60.3% (up to 10.3%) improvement in plastic ductility after heat preservation at 800 ℃ for 2h and then air cooling. Although the plastic ductility is improved to a certain extent through the traditional heat treatment mode, the level of the traditional forge piece is still difficult to achieve, and the strength-plastic matching property still hardly meets the application requirement.
The Lianghe, Shazhenan, etc. at Nanjing university of rational engineering invent a triple heat treatment mode for obtaining SLM forming TC4(Ti-6Al-4V) titanium alloy with better strength-plasticity matching. Forming TC4 through specific forming process parameters, coating a high-temperature antioxidant coating on the surface of a sample, heating to 820-840 ℃ at a heating rate of 3-4 ℃/min, preserving heat for 2-4h, and cooling in air to room temperature; heating to 710-740 ℃ at the heating rate of 3-4 ℃/min, preserving heat for 2-4h, and then cooling to room temperature along with the furnace; heating to 500-540 ℃ at the heating rate of 3-4 ℃/min, preserving heat for 2-6h, cooling to room temperature in air, and then carrying out post-treatment. The SLM-formed TC4 sample with the tensile strength of 1100.92MPa (reduced by 2.62%), the yield strength of 971.62MPa (reduced by 9.99%), the elongation after fracture of 18.14% (improved by 42.50%) and the reduction of area of 20.85% is obtained, and a better strength-plasticity matching is obtained, but a tri-state structure which enables the titanium alloy to have excellent performance is not obtained.
Rushikesh Sabban and the like heat an SLM forming TC4 titanium alloy (beta transformation point temperature is 991 ℃) sample to 975 ℃ at a heating rate of 5 ℃/min, then carry out circulating heat treatment at 875-975 ℃, wherein the heating rate is 2.5 ℃/min, the cooling rate is 1 ℃/min, and air cooling is carried out after 9 times of circulation, so that an SLM forming TC4 sample which is matched with good strength-plasticity and has the tensile strength of 1017MPa (reduced by 20.17%), the yield strength of 865MPa (reduced by 17.38%) and the plastic ductility of 18% (improved by 80%) is obtained. However, the obtained structure is closer to a two-state structure, and a three-state structure which provides excellent properties to the titanium alloy has not been obtained.
The research on the structure and the mechanical property of the near-alpha titanium alloy in the traditional forging field is found that when the structure is a tri-state structure (composed of about 15-20% of equiaxial alpha and 50-60% of lamellar alpha and beta transformation structures), the high strength is ensured and the good plastic ductility is simultaneously achieved. The heat treatment as mentioned above, although providing some improvement in the strength-plasticity matching, does not achieve a tri-state structure that results in excellent mechanical properties of the titanium alloy. The invention aims to adjust the SLM forming near alpha and alpha + beta titanium alloy structure through heat treatment, so that the former acicular martensite structure (the forming direction is coarse isometric crystal, the vertical forming direction is coarse columnar crystal, the isometric crystal and the columnar crystal are internally acicular martensite and contain a large amount of twin crystals) is converted into a tristate structure to improve the characteristic of poor plasticity of the SLM forming near alpha and alpha + beta titanium alloy, and the tensile mechanical property with better matching strength and plasticity is obtained.
Disclosure of Invention
In order to solve the technical problem, the invention provides a heat treatment method for obtaining a tri-state structure in SLM forming titanium alloy. According to the method, the SLM forming near alpha and alpha + beta titanium alloy structure with the needle-shaped martensite as the initial structure is converted into the tri-state structure only through heat treatment, so that the strength of a formed part is ensured, and the formed part has high plasticity and reaches or even exceeds the level of a forged piece.
The technical scheme of the invention comprises the following steps: a heat treatment method for obtaining a tri-modal microstructure in an SLM formed titanium alloy, comprising the steps of:
step 1), sub-beta phase transition point temperature heat preservation furnace cooling:
placing the sample in a crucible and placing the crucible in a heat treatment furnace, heating the heat treatment furnace to a sub-beta transformation point temperature which is 15-30 ℃ lower than the beta transformation point temperature of the near alpha and alpha + beta titanium alloy at the heating rate of 5-15 ℃/min, and keeping the temperature for 0.5-2 h; after the heat preservation is finished, closing the set heat treatment program, cooling the sample along with the furnace, and cooling the sample to room temperature in a furnace cooling mode to convert the structure of the sample into a beta-transformation matrix + isometric alpha + short rod-shaped alpha;
step 2), temperature preservation and air cooling of a two-phase region:
placing the sample subjected to primary heat treatment in a crucible and placing the crucible in a heat treatment furnace, heating the heat treatment furnace at a heating rate of 5-15 ℃/min to a two-phase region temperature which is 40-80 ℃ lower than the beta transformation point temperature of the alpha and alpha + beta titanium alloy, and preserving heat for 2-4 h; after the heat preservation is finished, taking out the sample and the crucible together, exposing the sample and the crucible in the air for air cooling, and cooling the sample to room temperature in an air cooling mode to convert the structure of the sample into a beta-transition matrix + isometric alpha + lamellar alpha;
step 3) aging:
placing the sample subjected to the two heat treatments in a crucible and placing the crucible in a heat treatment furnace, heating the heat treatment furnace to the aging temperature of 500-650 ℃ at the heating rate of 5-15 ℃/min, and preserving heat for 3-10 h; and after the heat preservation is finished, taking out the sample and the crucible together, exposing the sample and the crucible to the air for air cooling, and cooling the sample to room temperature in an air cooling mode to obtain the near alpha and alpha + beta titanium alloy with the tri-state structure.
Compared with the prior art, the invention has the following advantages:
1. the invention has the advantage that the SLM forming near alpha and alpha + beta titanium alloy (high strength and low plasticity) structure with the original structure of acicular martensite can be converted into the tri-state structure (excellent strength-plasticity matching) only by heat treatment, so that the strength-plasticity mismatch of the SLM forming near alpha and alpha + beta titanium alloy is improved.
2. The difficulty in transforming the SLM-formed near alpha and alpha + beta titanium alloy structure into the tri-state structure is the equiaxial transformation of crystal grains. The invention innovatively adopts a furnace cooling mode in the primary annealing of the triple annealing. And (3) enabling the SLM to form a near alpha and alpha + beta titanium alloy structure to be converted from an acicular martensite structure into a beta transformation matrix + isometric alpha + short rod-shaped alpha. Thus, only the transformation of the redundant equiaxed crystals and short rod crystals into lamellar crystal grains and a beta transformation matrix needs to be considered subsequently. As shown in fig. 2, if the primary annealing cooling method is air cooling or water cooling, it will present a great challenge to the equiaxial transformation of the crystal grains. The primary annealing water-cooled structure is acicular martensite and does not change much from the original structure, while the air-cooled structure is in a complete lamellar shape, and it is difficult to equiaxe the crystal grains.
3. The primary annealing of the invention is the temperature holding of sub-beta transformation point and furnace cooling, and at such high temperature, the dislocation can be completely activated by sliding or climbing. In contrast to conventional stress relief annealing, isothermally held at 15-30 ℃ below the sub-beta transus point, some dislocations may polygon and form many sub-grains. This will provide a precondition for the spheroidization of the SLM martensitic microstructure. Furthermore, below the β -transus temperature, some primary α will be retained and form intragranular α nuclei. These alpha nuclei will further promote the growth of equiaxed alpha during subsequent continuous cooling.
4. Compared with the inventions of Nanjing Liaojie, Xiaozhennan and the like in the background art, the invention has obvious differences: the primary annealing temperature of the furnace is a middle-temperature stage (820-840 ℃) of an alpha + beta phase region, the secondary annealing temperature is a low-temperature stage (710-740 ℃) of the alpha + beta phase region, and the tertiary annealing temperature is 500-540 ℃. The primary annealing temperature of the invention is sub-beta phase transition temperature (15-30 ℃ below the beta phase transition temperature), the secondary annealing temperature is the high temperature stage of alpha + beta phase region (40-70 ℃ below the beta phase transition point), the tertiary annealing temperature is the aging temperature (550-650 ℃), and the functions of each stage are different. The first annealing makes equiaxed crystal appear in the structure, the second annealing adjusts the proportion of equiaxed crystal and lamellar crystal, and the third annealing stabilizes the structure.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings.
FIG. 1 is a flow chart of the method of the present invention.
FIG. 2 shows the structure morphology formed after different cooling modes after primary annealing. (a) Furnace cooling FC, (b) air cooling AC, and (c) water cooling WC.
FIG. 3 is a graph of the original acicular martensite structure of TA15 titanium alloy with a beta transformation point of 995 ℃.
Fig. 4 is a microstructure diagram of a near α titanium alloy (TA15) after heat treatment in step one.
Fig. 5 shows a tri-state structure of the near α titanium alloy (TA15) after triple heat treatment.
Detailed Description
In order to make the objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Example one
The powder particles of TA15(Ti-6Al-2Zr-1Mo-1V) having an average particle diameter of 43.6 μm and the composition shown in the attached table were used as a molding material, and a bar stock having a size of phi 12mm x 83mm was molded according to the process parameters shown in the attached table.
Parameter attached table 1
Parameter attached table two
TA15 titanium alloy powder (transformation point temperature 995 ℃) was printed using a selective laser melting device to obtain a bar with phi 12mm x 83 mm. Separating the bar stock from the substrate by linear cutting, and then putting the bar stock into a vacuum heat treatment furnace for heat treatment.
Firstly, heating a bar stock to 970 ℃ at a heating rate of 10 ℃/min, preserving heat for 1.5h, closing a heating program, and cooling to room temperature along with a furnace; heating the bar stock subjected to the primary heat treatment to 930 ℃ at the same heating rate, preserving the heat for 2h, taking out a sample, exposing the sample in air, and cooling the sample in air to room temperature; and finally, heating the bar stock subjected to the secondary heat treatment to 600 ℃ at the same heating rate, preserving the heat for 3h, taking out the sample, exposing the sample in air, and cooling the sample in air to room temperature.
And (3) performing line cutting on the heat-treated bar, cutting a cubic sample block with the size of 8mm x 7mm from the core part of the bar, observing the microstructure, machining the rest part, and processing into a tensile sample with the gauge length of 25mm and the diameter of a working section of 5 mm. The tensile property test is carried out on the sample, and after the formed TA15 titanium alloy is treated by the process, the tensile strength is 1026MPa (reduced by 20.69%), the yield strength is 913MPa (reduced by 18.70%), the plastic ductility is 15.49% (improved by 90.29%), the reduction of area is 33% (improved by 106.25%), a tri-state structure is obtained, and the tri-state structure is shown in FIG. 5 and has excellent strength-plastic matching property.
Example two
The powder particles of TA15(Ti-6Al-2Zr-1Mo-1V) having an average particle diameter of 43.6 μm and the composition shown in the attached table were used as a molding material, and a bar stock having a size of phi 12mm x 83mm was molded according to the process parameters shown in the attached table.
Parameter attached table 1
Parameter attached table two
TA15 titanium alloy powder (transformation point temperature 995 ℃) was printed using a selective laser melting device to obtain a bar with phi 12mm x 83 mm. Separating the bar stock from the substrate by linear cutting, and then putting the bar stock into a vacuum heat treatment furnace for heat treatment.
Firstly, heating a bar stock to 970 ℃ at a heating rate of 10 ℃/min, preserving heat for 1h, closing a heating program, and cooling to room temperature along with a furnace; heating the bar stock subjected to the primary heat treatment to 930 ℃ at the same heating rate, preserving the heat for 3h, taking out a sample, exposing the sample in air, and cooling the sample in air to room temperature; and finally, heating the bar stock subjected to the secondary heat treatment to 600 ℃ at the same heating rate, preserving the heat for 5 hours, taking out the sample, exposing the sample in air, and cooling the sample in air to room temperature.
And (3) performing line cutting on the heat-treated bar, cutting a cubic sample block with the size of 8mm x 7mm from the core part of the bar, observing the microstructure, machining the rest part, and processing into a tensile sample with the gauge length of 25mm and the diameter of a working section of 5 mm. The tensile property test is carried out on the test sample, and after the formed TA15 titanium alloy is treated by the process, the tensile strength is 1004MPa (reduced by 21.62%), the yield strength is 897MPa (reduced by 20.12%), the plastic ductility is 16.13% (improved by 98.16%), and the excellent strength-plastic matching property is achieved.
EXAMPLE III
The powder particles of TA15(Ti-6Al-2Zr-1Mo-1V) having an average particle diameter of 43.6 μm and the composition shown in the attached table were used as a molding material, and a bar stock having a size of phi 12mm x 83mm was molded according to the process parameters shown in the attached table.
Parameter attached table 1
Parameter attached table two
TA15 titanium alloy powder (transformation point temperature 995 ℃) was printed using a selective laser melting device to obtain a bar with phi 12mm x 83 mm. Separating the bar stock from the substrate by linear cutting, and then putting the bar stock into a vacuum heat treatment furnace for heat treatment.
Firstly, heating a bar stock to 970 ℃ at a heating rate of 10 ℃/min, preserving heat for 2h, closing a heating program, and cooling to room temperature along with a furnace; heating the bar stock subjected to the primary heat treatment to 950 ℃ at the same heating rate, preserving the heat for 3 hours, taking out a sample, exposing the sample in air, and cooling the sample in air to room temperature; and finally, heating the bar stock subjected to the secondary heat treatment to 600 ℃ at the same heating rate, preserving the heat for 4h, taking out the sample, exposing the sample in air, and cooling the sample in air to room temperature.
And (3) performing line cutting on the heat-treated bar, cutting a cubic sample block with the size of 8mm x 7mm from the core part of the bar, observing the microstructure, machining the rest part, and processing into a tensile sample with the gauge length of 25mm and the diameter of a working section of 5 mm. The tensile property test is carried out on the test sample, and after the formed TA15 titanium alloy is treated by the process, the tensile strength is 1017MPa (reduced by 20.61%), the yield strength is 909MPa (reduced by 19.06%), the plastic ductility is 15.87% (improved by 94.96%), and the test sample has excellent strength-plastic matching property.
The invention adopts three stages of multiple heat treatment with different temperature intervals: firstly, heating a sample to 15-30 ℃ below the sub-beta transformation point temperature at the heating rate of 10 ℃/min, preserving heat for 0.5-2h, then closing the heating program of a heat treatment furnace, and cooling along with the furnace until the temperature is reduced to room temperature, so that the original acicular martensite structure is converted into a structure containing a beta transformation matrix, equiaxial alpha and short rod-shaped alpha, the equiaxial structure in the tri-state structure is prepared, and conditions are provided for the equiaxial transformation of subsequent grains. Heating the sample to 40-80 ℃ below the beta transformation point temperature at the heating rate of 10 ℃/min through the second step, preserving the heat for 2-4h, taking out the sample, exposing the sample in air, and cooling the sample in air to room temperature to reduce the medium axial crystal in the tissue to 15-25% and form 40-60% of lamellar crystal and beta transformation matrix. Heating the sample to the aging temperature of 500-650 ℃ at the heating rate of 10 ℃/min, preserving the heat for 3-10h, taking out the sample, exposing the sample in the air, air-cooling to the room temperature, ensuring that the change of the structure morphology is not large, and playing a role in stabilizing the structure, thereby finally obtaining the tri-state structure which causes the near alpha and alpha + beta titanium alloy to have excellent performance. The technology has the advantage that the SLM forming near alpha and alpha + beta titanium alloy (high strength and low plasticity) structure with the original structure of acicular martensite can be converted into the tri-state structure (excellent strength-plasticity matching) only by heat treatment, so that the current situation of strength-plasticity mismatching of the SLM forming near alpha and alpha + beta titanium alloy is improved.
While the embodiments of the present invention have been described in detail with reference to the drawings, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (1)
1. A heat treatment method for obtaining a tri-modal microstructure in SLM formed titanium alloys, characterised by the following steps:
step 1), sub-beta phase transition point temperature heat preservation furnace cooling:
placing the sample in a crucible and placing the crucible in a heat treatment furnace, heating the heat treatment furnace to a sub-beta transformation point temperature which is 15-30 ℃ lower than the beta transformation point temperature of the near alpha and alpha + beta titanium alloy at the heating rate of 5-15 ℃/min, and keeping the temperature for 0.5-2 h; after the heat preservation is finished, closing the set heat treatment program, cooling the sample along with the furnace, and cooling the sample to room temperature in a furnace cooling mode to convert the structure of the sample into a beta-transformation matrix + isometric alpha + short rod-shaped alpha;
step 2), temperature preservation and air cooling of a two-phase region:
placing the sample subjected to primary heat treatment in a crucible and placing the crucible in a heat treatment furnace, heating the heat treatment furnace at a heating rate of 5-15 ℃/min to a two-phase region temperature which is 40-80 ℃ lower than the beta transformation point temperature of the alpha and alpha + beta titanium alloy, and preserving heat for 2-4 h; after the heat preservation is finished, taking out the sample and the crucible together, exposing the sample and the crucible in the air for air cooling, and cooling the sample to room temperature in an air cooling mode to convert the structure of the sample into a beta-transition matrix + isometric alpha + lamellar alpha;
step 3) aging:
placing the sample subjected to the two heat treatments in a crucible and placing the crucible in a heat treatment furnace, heating the heat treatment furnace to the aging temperature of 500-650 ℃ at the heating rate of 5-15 ℃/min, and preserving heat for 3-10 h; and after the heat preservation is finished, taking out the sample and the crucible together, exposing the sample and the crucible to the air for air cooling, and cooling the sample to room temperature in an air cooling mode to obtain the near alpha and alpha + beta titanium alloy with the tri-state structure.
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| CN113981346A (en) * | 2021-09-16 | 2022-01-28 | 攀枝花容则钒钛有限公司 | Heat treatment method of titanium alloy with beta-phase columnar crystal TC18 |
| CN113996812A (en) * | 2021-10-15 | 2022-02-01 | 中国航发北京航空材料研究院 | Heat treatment method for improving fatigue performance of laser selective melting alpha-beta type titanium alloy |
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| CN115446329A (en) * | 2022-09-08 | 2022-12-09 | 辽宁五寰特种材料与智能装备产业技术研究院有限公司 | SLM (selective laser melting) technology-based high-strength Ti-Al-V-based alloy 3D printing manufacturing method |
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| CN113981346A (en) * | 2021-09-16 | 2022-01-28 | 攀枝花容则钒钛有限公司 | Heat treatment method of titanium alloy with beta-phase columnar crystal TC18 |
| CN113996812A (en) * | 2021-10-15 | 2022-02-01 | 中国航发北京航空材料研究院 | Heat treatment method for improving fatigue performance of laser selective melting alpha-beta type titanium alloy |
| CN114216763A (en) * | 2021-10-25 | 2022-03-22 | 北京星航机电装备有限公司 | Method for evaluating laser selective melting forming performance of titanium alloy material |
| CN114273673A (en) * | 2021-12-14 | 2022-04-05 | 攀枝花容则钒钛有限公司 | Preparation method of TC18 titanium alloy part |
| CN114273673B (en) * | 2021-12-14 | 2024-03-15 | 攀枝花容则钒钛有限公司 | Preparation method of TC18 titanium alloy part |
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| CN114618970A (en) * | 2022-03-14 | 2022-06-14 | 江西景航航空锻铸有限公司 | Forging process for improving strength of thick-section TA15 titanium alloy forging |
| CN115125462A (en) * | 2022-05-13 | 2022-09-30 | 上海航翼高新技术发展研究院有限公司 | Heat treatment method for improving stability of structure and performance of titanium alloy manufactured by laser additive |
| CN115305425A (en) * | 2022-07-15 | 2022-11-08 | 武汉大学 | Toughening heat treatment method for laser additive manufacturing titanium alloy |
| CN115446329A (en) * | 2022-09-08 | 2022-12-09 | 辽宁五寰特种材料与智能装备产业技术研究院有限公司 | SLM (selective laser melting) technology-based high-strength Ti-Al-V-based alloy 3D printing manufacturing method |
| CN115446329B (en) * | 2022-09-08 | 2024-04-19 | 辽宁五寰特种材料与智能装备产业技术研究院有限公司 | High-strength Ti-Al-V based alloy 3D printing manufacturing method based on SLM technology |
| CN115846867A (en) * | 2022-10-28 | 2023-03-28 | 哈尔滨焊接研究院有限公司 | High-ductility, high-toughness and high-strength welding joint based on Ti-6Al-4V titanium alloy and tissue regulation method and application thereof |
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