CN117286440A - Heat treatment method for additive manufacturing of nickel-titanium alloy and application thereof - Google Patents

Heat treatment method for additive manufacturing of nickel-titanium alloy and application thereof Download PDF

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Publication number
CN117286440A
CN117286440A CN202311214641.2A CN202311214641A CN117286440A CN 117286440 A CN117286440 A CN 117286440A CN 202311214641 A CN202311214641 A CN 202311214641A CN 117286440 A CN117286440 A CN 117286440A
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China
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nickel
titanium alloy
pressure
heat treatment
additive manufacturing
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CN202311214641.2A
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Inventor
施麒
申正焱
刘辛
谭冲
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Institute of New Materials of Guangdong Academy of Sciences
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Institute of New Materials of Guangdong Academy of Sciences
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Priority to CN202311214641.2A priority Critical patent/CN117286440A/en
Publication of CN117286440A publication Critical patent/CN117286440A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing 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
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60Treatment of workpieces or articles after build-up
    • B22F10/64Treatment of workpieces or articles after build-up by thermal means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y40/00Auxiliary operations or equipment, e.g. for material handling
    • B33Y40/20Post-treatment, e.g. curing, coating or polishing
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Abstract

The invention discloses a heat treatment method for additive manufacturing of nickel-titanium alloy and application thereof, and relates to the technical field of heat treatment of metal materials. A heat treatment method for additive manufacturing of nickel-titanium alloy, comprising the following steps: (1) Heating and pressurizing nickel-titanium alloy in a closed container to 900-1200 ℃ and the pressure in the closed container is not lower than 120MPa; then preserving heat and pressure for more than 120min, and finally cooling to 250-500 ℃ at a cooling speed of 100-1000 ℃/min; (2) Preserving heat and pressure for 30-180min for the nickel-titanium alloy in the closed container, then cooling to room temperature and taking out the nickel-titanium alloy; the pressure of the closed container after the temperature is reduced in the step (1) and the step (2) is more than or equal to 80MPa. The method of the invention not only can eliminate residual pores and microcracks generated in the additive manufacturing process, but also can effectively regulate and control the material tissue performance and improve the preparation efficiency.

Description

Heat treatment method for additive manufacturing of nickel-titanium alloy and application thereof
Technical Field
The invention relates to the technical field of heat treatment of metal materials, in particular to a heat treatment method for manufacturing nickel-titanium alloy by additive and application thereof.
Background
The nickel-titanium alloy has the characteristics of shape memory effect, super elasticity, low rigidity, biocompatibility, damping characteristic, corrosion resistance and the like, and is widely applied to the fields of aerospace, medical equipment and the like. However, due to the reactivity and resilience of nickel-titanium alloys, conventional machining processes have difficulty in making nickel-titanium alloy articles, particularly parts of complex shape.
In recent years, the rapid development of additive manufacturing technology has provided a new path for forming technology for the manufacture of complex parts. For example, nickel-titanium alloy self-expanding vascular stents, orthodontic wires, interbody fusion devices, and the like manufactured by selective laser melting technology. It should be noted, however, that additive manufacturing nickel-titanium alloys typically require subsequent heat treatments, such as solution treatment, to eliminate the foreign phases generated during the forming process in order to obtain a single phase matrix; aging treatment is carried out to obtain second phase precipitation so as to obtain better comprehensive mechanical properties. In addition, internal voids and microcracks are inevitably generated in the additive manufacturing process, and the performance of the product is finally affected. Therefore, the development of the heat treatment method suitable for additive manufacturing of nickel-titanium alloy parts has the advantages that the internal defects are eliminated, meanwhile, the effective regulation and control of the microstructure of the materials are realized, and the method has important significance in improving the performance of the parts and the preparation efficiency.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a heat treatment method for additive manufacturing of nickel-titanium alloy and application thereof. The method of the invention not only can eliminate residual pores and microcracks generated in the additive manufacturing process, but also can effectively regulate and control the material tissue performance and improve the preparation efficiency.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
in a first aspect, the present invention provides a heat treatment method for additive manufacturing of nickel titanium alloy, comprising the steps of:
(1) Heating and pressurizing nickel-titanium alloy in a closed container to 900-1200 ℃ and the pressure in the closed container is not lower than 120MPa; then preserving heat and pressure for more than 120min, and finally cooling to 250-500 ℃ at a cooling speed of 100-1000 ℃/min;
(2) Preserving heat and pressure for 30-180min for the nickel-titanium alloy in the closed container, then cooling to room temperature and taking out the nickel-titanium alloy; the pressure in the closed container after the temperature is reduced in the step (1) and the step (2) is more than or equal to 80MPa.
The invention simultaneously completes densification and heat treatment of the additive manufacturing nickel-titanium alloy material in a closed container. The invention applies uniform isostatic pressure of not less than 120MPa to the nickel-titanium alloy at 900-1200 ℃, maintains the temperature and pressure for not less than 120min, and effectively eliminates residual internal pores and microcracks of the material in the additive manufacturing process. Meanwhile, the high-pressure solid solution treatment can fully dissolve the impurity phase generated in the additive manufacturing process in the matrix, so that a uniform single-phase matrix structure, namely NiTi phase, is obtained; and the precipitation of the second phase in the nickel-titanium alloy is regulated and controlled by regulating the cooling rate at the end of the solution treatment. In addition, the invention further regulates the extraction and growth of the second phase in the nickel-titanium alloy by regulating the temperature of aging treatment and the duration of heat preservation and pressure maintaining. In addition, as the solution treatment and the aging treatment are carried out under the pressure of not lower than 80MPa, the nickel-titanium alloy can effectively avoid the re-opening of pores in the heat treatment process. The invention not only can effectively improve the comprehensive mechanical property of the nickel-titanium alloy material, but also can combine the original multi-step heat treatment, thereby improving the production efficiency of nickel-titanium alloy parts.
Preferably, the temperature after heating and pressurizing in the step (1) is 1050-1200 ℃, and the air pressure of the closed container is 120-150MPa.
More preferably, the heating temperature in the step (1) is 1100 ℃, the air pressure is 130MPa, and the heat preservation and pressure maintaining time is 210min.
Preferably, the time of the heat preservation and pressure maintaining in the step (1) is 180-240min.
The temperature and the air pressure in the range and the heat preservation and pressure maintaining time are adopted in the invention, so that the residual internal pores and microcracks of the nickel-titanium alloy in the additive manufacturing process are better eliminated, thereby further improving the comprehensive mechanical property of the nickel-titanium alloy.
Preferably, the temperature at Wen Baoya in the step (2) is 350-500 ℃, and the air pressure of the closed container is 80-120MPa.
Preferably, the time of the heat preservation and pressure maintaining in the step (2) is 60-120min.
More preferably, the temperature at the time of Wen Baoya in the step (2) is 400 ℃, the air pressure of the closed container is 100MPa, and the heat preservation and pressure maintaining time is 80min.
The temperature and the air pressure in the range and the heat preservation and pressure maintaining time are adopted in the invention, so that pores of the nickel-titanium alloy are not easy to reopen in the heat treatment process, and the comprehensive mechanical property of the nickel-titanium alloy is further improved.
Preferably, the cooling speed in the step (1) is 800-1000 ℃/min.
More preferably, the cooling rate in step (1) is 900 ℃/min.
Preferably, the closed vessel is a hot isostatic pressing cylinder.
In a second aspect, the invention provides an additive manufacturing nickel-titanium alloy, which is obtained after being treated by the above heat method.
In a third aspect, the invention provides an application of additive manufacturing nickel-titanium alloy in the field of aerospace and biomedical.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention applies uniform isostatic pressure of not less than 120MPa to the material at 900-1200 ℃, keeps the temperature and pressure for not less than 120min, and effectively eliminates residual internal pores and microcracks of the material in the additive manufacturing process.
(2) According to the invention, the temperature of aging treatment and the duration of heat preservation and pressure maintaining are adjusted, so that the second phase in the nickel-titanium alloy is favorably regulated and controlled to be lifted and grown. In addition, as the solution treatment and the aging treatment are carried out under the pressure of not lower than 80MPa, the pores of the nickel-titanium alloy material can be effectively prevented from being opened again in the heat treatment process.
Drawings
FIG. 1 is a scanning electron micrograph of the microstructure of example 1 of the present invention prior to heat treating an additive manufactured nickel titanium alloy.
FIG. 2 is a scanning electron micrograph of the microstructure of the additive manufactured nickel-titanium alloy of example 1 of the present invention after heat treatment.
FIG. 3 is a scanning electron microscope image of the microstructure of example 2 of the present invention after heat treatment of the additive manufactured nickel titanium alloy.
Detailed Description
For better illustrating the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples, but the scope and embodiments of the present invention are not limited thereto.
Materials, reagents and the like used in the following examples are commercially available ones unless otherwise specified.
Example 1
A heat treatment method for additive manufacturing of nickel-titanium alloy, comprising the following steps:
(1) High-pressure solution treatment: placing nickel-titanium alloy in a hot isostatic pressing cylinder, simultaneously heating and pressurizing under the condition of initial air pressure of 30MPa, heating to 900 ℃, keeping the cylinder air pressure at 120MPa, preserving heat and pressure for 120min, and then cooling to 250 ℃ at a speed of 100 ℃/min under the condition of no pressure relief;
(2) High-pressure aging treatment: and (3) keeping the temperature and pressure for 30min at 250 ℃ and 80MPa, and finally cooling to room temperature, and taking out the nickel-titanium alloy, wherein the nickel-titanium alloy is always placed in the hot isostatic pressing cylinder body during high-pressure solid solution treatment and high-pressure aging treatment.
As can be seen from the comparison of FIG. 1 and FIG. 2, after the nickel-titanium alloy material is treated by the method of the invention, the density of the nickel-titanium alloy is improved, and the pores are basically eliminated.
Example 2
A heat treatment method for additive manufacturing of nickel-titanium alloy, comprising the following steps:
(1) High-pressure solution treatment: placing nickel-titanium alloy in a hot isostatic pressing cylinder, simultaneously heating and pressurizing under the condition of initial air pressure of 30MPa, heating to 1200 ℃, keeping the cylinder air pressure at 120MPa, preserving heat and pressure for 120min, and then cooling to 500 ℃ at the speed of 1000 ℃/min under the condition of no pressure relief;
(2) High-pressure aging treatment: and (3) keeping the temperature and pressure for 180min at 500 ℃ and 80MPa, and finally cooling to room temperature, and taking out the nickel-titanium alloy, wherein the nickel-titanium alloy is always placed in the hot isostatic pressing cylinder body during high-pressure solid solution treatment and high-pressure aging treatment.
Example 3
A heat treatment method for additive manufacturing of nickel-titanium alloy, comprising the following steps:
(1) High-pressure solution treatment: placing nickel-titanium alloy in a hot isostatic pressing cylinder, simultaneously heating and pressurizing under the condition of initial air pressure of 30MPa, heating to 1050 ℃, keeping the cylinder air pressure at 120MPa, preserving heat and pressure for 180min, and then cooling to 350 ℃ at the speed of 1000 ℃/min under the condition of no pressure relief;
(2) High-pressure aging treatment: and (3) keeping the temperature and pressure for 60min at 350 ℃ and 80MPa, and finally cooling to room temperature, and taking out the nickel-titanium alloy, wherein the nickel-titanium alloy is always placed in the hot isostatic pressing cylinder body during high-pressure solid solution treatment and high-pressure aging treatment.
Example 4
A heat treatment method for additive manufacturing of nickel-titanium alloy, comprising the following steps:
(1) High-pressure solution treatment: placing nickel-titanium alloy in a hot isostatic pressing cylinder, simultaneously heating and pressurizing under the condition of initial air pressure of 30MPa, heating to 1200 ℃, keeping the cylinder air pressure at 150MPa, preserving heat and pressure for 240min, and then cooling to 500 ℃ at the speed of 1000 ℃/min under the condition of no pressure relief;
(2) High-pressure aging treatment: and (3) keeping the temperature and pressure for 120min at 500 ℃ and 120MPa, and finally cooling to room temperature, and taking out the nickel-titanium alloy, wherein the nickel-titanium alloy is always placed in the hot isostatic pressing cylinder body during high-pressure solid solution treatment and high-pressure aging treatment.
Example 5
A heat treatment method for additive manufacturing of nickel-titanium alloy, comprising the following steps:
(1) High-pressure solution treatment: placing nickel-titanium alloy in a hot isostatic pressing cylinder, simultaneously heating and pressurizing under the condition of initial air pressure of 30MPa, heating to 1100 ℃, keeping the cylinder air pressure at 130MPa, preserving heat and pressure for 210min, and then cooling to 400 ℃ at the speed of 1000 ℃/min under the condition of no pressure relief;
(2) High-pressure aging treatment: and (3) keeping the temperature and pressure for 80 minutes at 400 ℃ and 100MPa, and finally cooling to room temperature, and taking out the nickel-titanium alloy, wherein the nickel-titanium alloy is always placed in the hot isostatic pressing cylinder body during high-pressure solid solution treatment and high-pressure aging treatment.
Example 6
The difference from example 1 was that the cooling rate at the end of the solution treatment in step (1) was 800℃per minute, and the other steps were the same as in example 1.
Example 7
The difference from example 1 was that the cooling rate at the end of the solution treatment in step (1) was 900℃per minute, and the other steps were the same as in example 1.
Comparative example 1
The difference from example 1 was that the temperature after heating and pressurizing in the solution treatment in step (1) was 800℃and the other steps were the same as in example 1.
Comparative example 2
The difference from example 1 is that the temperature after heating and pressurizing in the solution treatment in the step (1) was 1500℃and the other steps were the same as in example 1.
Comparative example 3
The difference from example 1 is that the cylinder gas pressure in the solution treatment in step (1) was 60MPa, and the other steps were the same as in example 1.
Comparative example 4
The difference from example 1 is that the holding time for the solution treatment in step (1) was 100 minutes, and the other steps were the same as in example 1.
Comparative example 5
The difference from example 1 is that in step (1), the cooling rate at the end of the solution treatment was 80℃per minute, and the other steps were the same as in example 1.
Comparative example 6
The difference from example 1 is that in step (1), the cooling rate at the end of the solution treatment was 1200 ℃/min, and the other steps were the same as in example 1.
Comparative example 7
The difference from example 1 is that the temperature at the time of heat and pressure maintaining in the aging treatment in the step (2) was 200℃and the other steps were the same as in example 1.
Comparative example 8
The difference from example 1 is that the temperature at the time of heat and pressure maintaining in the aging treatment in the step (2) was 600℃and the other steps were the same as in example 1.
Comparative example 9
The difference from example 1 is that the cylinder pressure in the aging treatment in step (2) was 50MPa, and the other steps were the same as those in example 1.
Comparative example 10
The difference from example 1 is that in step (2), the holding time for the aging treatment was 200min, and the other steps were the same as those in example 1.
Comparative example 11
The difference from example 1 is that in step (2), the holding time for the aging treatment was 10 minutes, and the other steps were the same as those in example 1.
Comparative example 12
The difference from example 1 is that in step (1), after heat preservation and pressure maintaining for 120min, the nickel-titanium alloy is naturally cooled to room temperature and taken out.
Experiment
The nickel-titanium alloy after heat treatment of the above examples and comparative examples was subjected to performance testing by the following method:
density: density measurement method GB/T3850-2015 for compact sintered metal material and hard alloy;
tensile strength: metal material tensile test GB/T228.1-2010;
elongation percentage: metallic material tensile test GB/T228.1-2010.
TABLE 1
According to Table 1, when the heating temperature, air pressure and heat preservation and pressure maintaining time during solution treatment, the temperature, air pressure and heat preservation and pressure maintaining time during aging treatment are not in the range protected by the application, the performance of the nickel-titanium alloy can be affected to a certain extent, so that the invention can effectively improve the comprehensive mechanical property of the nickel-titanium alloy material and combine the original multi-step heat treatment by adjusting the heating temperature, air pressure and heat preservation and pressure maintaining time during solution treatment in the range protected by the application, and simultaneously, the temperature, air pressure and heat preservation and pressure maintaining time during aging treatment are controlled, thereby improving the production efficiency of nickel-titanium alloy products.
In conclusion, the invention applies uniform isostatic pressure of not less than 120MPa to the nickel-titanium alloy at 900-1200 ℃, maintains the temperature and pressure for not less than 120min, and effectively eliminates residual internal pores and microcracks of the nickel-titanium alloy material in the additive manufacturing process. Meanwhile, the high-pressure solid solution treatment can fully dissolve the impurity phase generated in the additive manufacturing process in the matrix, so that a uniform single-phase matrix structure is obtained; and the precipitation of the second phase in the nickel-titanium alloy is regulated and controlled by regulating the cooling rate at the end of the solution treatment. In addition, the invention further regulates the extraction and growth of the second phase in the nickel-titanium alloy by regulating the temperature of aging treatment and the duration of heat preservation and pressure maintaining. In addition, as the solution treatment and the aging treatment are carried out under the pressure of not lower than 80MPa, the nickel-titanium alloy material can effectively avoid the re-opening of pores in the heat treatment process.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.

Claims (10)

1. A heat treatment method for additive manufacturing of nickel-titanium alloy, which is characterized by comprising the following steps:
(1) Heating and pressurizing nickel-titanium alloy in a closed container to 900-1200 ℃ and the pressure in the closed container is not lower than 120MPa; then preserving heat and pressure for more than 120min, and finally cooling to 250-500 ℃ at a cooling speed of 100-1000 ℃/min;
(2) Preserving heat and pressure for 30-180min for the nickel-titanium alloy in the closed container, then cooling to room temperature and taking out the nickel-titanium alloy;
the pressure of the closed container after the temperature is reduced in the step (1) and the step (2) is more than or equal to 80MPa.
2. The heat treatment method for manufacturing nickel-titanium alloy by additive material according to claim 1, wherein the temperature after heating and pressurizing in the step (1) is 1050-1200 ℃, and the air pressure of the closed container is 120-150MPa.
3. The heat treatment method for additive manufacturing of nickel-titanium alloy according to claim 1, wherein the time for maintaining the temperature and pressure in the step (1) is 180-240min.
4. The heat treatment method for additive manufacturing of nickel-titanium alloy according to claim 1, wherein the temperature of Wen Baoya in the step (2) is 350-500 ℃, and the air pressure of the closed container is 80-120MPa.
5. The heat treatment method for additive manufacturing of nickel-titanium alloy according to claim 1, wherein the time for maintaining the temperature and pressure in the step (2) is 60-120min.
6. The method of heat treating an additive manufactured nickel titanium alloy according to claim 1, wherein the cooling rate in step (1) is 800-1000 ℃/min.
7. The method of heat treating an additive manufactured nickel titanium alloy according to claim 6, wherein the cooling rate in step (1) is 900 ℃/min.
8. The method of claim 1, wherein the containment vessel is a hot isostatic pressing cylinder.
9. An additive manufactured nickel-titanium alloy, characterized in that it is obtained after treatment by the heat treatment method of additive manufactured nickel-titanium alloy according to any one of claims 1-8.
10. Use of the additive manufactured nickel-titanium alloy of claim 9 in aerospace, biomedical applications.
CN202311214641.2A 2023-09-19 2023-09-19 Heat treatment method for additive manufacturing of nickel-titanium alloy and application thereof Pending CN117286440A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117286438A (en) * 2023-11-24 2023-12-26 常州钢研极光增材制造有限公司 Solution treatment method and heat treatment method for GH4099 part with cavity structure

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117286438A (en) * 2023-11-24 2023-12-26 常州钢研极光增材制造有限公司 Solution treatment method and heat treatment method for GH4099 part with cavity structure
CN117286438B (en) * 2023-11-24 2024-01-30 常州钢研极光增材制造有限公司 Solution treatment method and heat treatment method for GH4099 part with cavity structure

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