CN117403154A - Heat treatment process suitable for laser near-net forming nickel-titanium shape memory alloy - Google Patents
Heat treatment process suitable for laser near-net forming nickel-titanium shape memory alloy Download PDFInfo
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- CN117403154A CN117403154A CN202311045644.8A CN202311045644A CN117403154A CN 117403154 A CN117403154 A CN 117403154A CN 202311045644 A CN202311045644 A CN 202311045644A CN 117403154 A CN117403154 A CN 117403154A
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- 229910001000 nickel titanium Inorganic materials 0.000 title claims abstract description 113
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910001285 shape-memory alloy Inorganic materials 0.000 title claims abstract description 76
- 238000010438 heat treatment Methods 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 55
- 230000008569 process Effects 0.000 title claims abstract description 46
- 239000000956 alloy Substances 0.000 claims abstract description 22
- 238000005516 engineering process Methods 0.000 claims abstract description 9
- 238000004321 preservation Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 58
- 239000000758 substrate Substances 0.000 claims description 28
- 238000012545 processing Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000002356 single layer Substances 0.000 claims description 7
- 239000010410 layer Substances 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910001257 Nb alloy Inorganic materials 0.000 claims description 2
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 2
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910001055 inconels 600 Inorganic materials 0.000 claims description 2
- 229910001119 inconels 625 Inorganic materials 0.000 claims description 2
- 229910000816 inconels 718 Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000007493 shaping process Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 229910001566 austenite Inorganic materials 0.000 abstract description 6
- 229910000734 martensite Inorganic materials 0.000 abstract description 6
- 230000009466 transformation Effects 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 5
- 230000003446 memory effect Effects 0.000 abstract description 4
- 230000033228 biological regulation Effects 0.000 abstract description 2
- 238000007639 printing Methods 0.000 description 11
- 230000007704 transition Effects 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 244000137852 Petrea volubilis Species 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 239000011261 inert gas Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005498 polishing Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000011089 mechanical engineering Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
- 238000003852 thin film production method Methods 0.000 description 1
Classifications
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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
- C22F1/10—Changing 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/25—Direct deposition of metal particles, e.g. direct metal deposition [DMD] or laser engineered net shaping [LENS]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- 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
- B33Y80/00—Products made by additive manufacturing
-
- 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
- C22F1/006—Resulting in heat recoverable alloys with a memory effect
Abstract
The invention discloses a heat treatment process suitable for laser near-net forming nickel-titanium shape memory alloy, which comprises the following steps: forming a nickel-titanium shape memory alloy material by a laser near-net forming technology; and carrying out high-temperature heat treatment on the nickel-titanium shape memory alloy material to obtain the nickel-titanium shape memory alloy component. According to the invention, through the regulation and control of temperature and heat preservation time, the size and distribution of the precipitated phases in the nickel-titanium alloy can be effectively controlled, and the precipitated phases distributed near the grain boundary and in the crystal are obtained, so that the shape memory effect of the nickel-titanium alloy is improved; the content of the martensite phase and the austenite phase is controlled through heat treatment, and the phase transformation temperature of the material is improved, so that the nickel-titanium shape memory alloy exists in a mixed form of the martensite phase and the austenite phase at normal temperature; the invention has simple operation and easy control of conditions, eliminates the internal stress of the nickel-titanium shape memory alloy through a heat treatment process, so that the heat treated nickel-titanium alloy component has high strength and large strain, and the mechanical stability of the nickel-titanium alloy component is obviously improved.
Description
Technical Field
The invention relates to the technical field of nickel-titanium shape memory alloy, in particular to a heat treatment process suitable for laser near-net forming nickel-titanium shape memory alloy.
Background
Shape Memory Alloys (SMA) have the ability to directly convert thermal energy into mechanical work due to their high drive energy density and excellent functional properties, and are widely used in particular engineering applications including aerobiomedicine, microelectronics, and other applications. Among them, niTi alloys are widely used because of their excellent functional characteristics, and they can exhibit superelasticity and shape memory effects. To better reflect these properties, conventional methods, such as ingot metallurgy, powder metallurgy, thermal spraying, and thin film production methods, have severely limited the use of NiTi alloys, which affect the mechanical and functional properties of the material, resulting in lack of homogeneity of composition, high porosity, low surface finish, and unexpected second phases in processing. Furthermore, conventional casting processes cannot support the production of large complex structures.
The laser near-net forming technology is one directional energy depositing additive producing process capable of being produced in certain requirement, and has computer system to produce digital controlled bench motion track, high power continuous wave laser beam to form molten pool system with fast melting and solidification, and the near-net forming part is obtained through layer-by-layer superposition of points, lines and surfaces and the formed part may be used without need of small amount of machining. Therefore, the non-mould production and manufacture of the nickel-titanium shape memory alloy material can be realized by utilizing the laser near-net forming technology, a series of problems of difficult cutting processing, large material removal amount, serious cutter abrasion and the like of the complex curved surface part in the traditional manufacturing process are solved, and the adjustable porosity, adjustable size and shape are supported.
In additive manufacturing techniques, rapid cure rates can lead to the accumulation of residual stresses, which can reduce the ductility of the material. Ductility is restored by a suitable heat treatment process and anisotropy caused by the difference in orientation of the deposited layers is minimized. In addition, precipitates having different sizes and shapes are formed during the heat treatment, which have a great influence on the phase transformation and shape memory effects of the alloy, and studies have demonstrated that complex multiphase transformation occurs at different aging temperatures, which is related to the precipitates inside the NiTi alloy.
In view of this, it is necessary to adjust the size and distribution of the internal structure and precipitated phase of the laser near-net shape nickel-titanium alloy by a heat treatment process to improve the performance of the nickel-titanium shape memory alloy.
Disclosure of Invention
The invention aims to overcome the technical defects, provides a heat treatment process suitable for laser near-net-shape nickel-titanium shape memory alloy, and solves the technical problem of poor mechanical property caused by accumulation of residual stress of the laser near-net-shape nickel-titanium alloy in the prior art.
In a first aspect, the present invention provides a heat treatment process for a laser near net shape nickel titanium shape memory alloy, comprising the steps of:
forming a nickel-titanium shape memory alloy material by a laser near-net forming technology;
and (3) carrying out high-temperature heat treatment on the nickel-titanium shape memory alloy material, and then cooling to room temperature along with a furnace to obtain the nickel-titanium shape memory alloy component.
In a second aspect, the present invention provides a nickel-titanium shape memory alloy obtained by the heat treatment process for laser near net shape nickel-titanium shape memory alloy provided in the first aspect of the present invention.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, through the design of temperature and the regulation and control of heat preservation time, the size and distribution of the precipitated phases in the nickel-titanium alloy can be effectively controlled, and the precipitated phases distributed near the grain boundary and in the crystal are obtained, so that the shape memory effect of the nickel-titanium alloy is improved;
(2) According to the invention, the contents of the martensite phase and the austenite phase are controlled through heat treatment, so that the phase transformation temperature of the material is improved, and the nickel-titanium shape memory alloy exists in a mixed form of the martensite phase and the austenite phase at normal temperature;
(3) The heat treatment process is simple to operate, the conditions are easy to control, and the internal stress of the nickel-titanium shape memory alloy is eliminated through the heat treatment process, so that the heat treated nickel-titanium alloy component has high strength and large strain, and the mechanical stability of the nickel-titanium alloy component is obviously improved.
Drawings
FIG. 1 is a stress-strain curve of the nickel titanium shape memory alloy members prepared in examples 1-3;
FIG. 2 is a graph of the phase transition temperature of the nickel titanium shape memory alloy members prepared in examples 1-3;
FIG. 3 is a microstructure effect map of the nickel titanium shape memory alloy components prepared in examples 1-3;
FIG. 4 is a stress-strain plot of the nickel titanium shape memory alloy members prepared in comparative examples 1-2;
FIG. 5 is a graph of the phase transition temperature of the nickel titanium shape memory alloy member prepared in comparative examples 1-2;
in the figure, A is austenite phase, R is R phase, M is martensite phase, A s Is the temperature at which transformation begins from martensite to austenite phase transformation.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In a first aspect, the present invention provides a heat treatment process for a laser near net shape nickel titanium shape memory alloy, comprising the steps of:
s1, forming a nickel-titanium shape memory alloy material by a laser near-net forming technology;
s2, performing high-temperature heat treatment on the nickel-titanium shape memory alloy material, and then cooling to room temperature along with a furnace to obtain a nickel-titanium shape memory alloy member; wherein, in the high temperature heat treatment process, the heat treatment temperature is 300-1100 ℃, including but not limited to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ and the like, preferably 600-800 ℃; the incubation time is 1-3 hours, including but not limited to 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, etc.
The nickel-titanium shape memory alloy material formed by adopting the laser near-net forming technology has high density, almost no oxidation on the surface, no obvious defects such as holes, cracks and the like. According to the invention, through reasonably regulating and controlling the heat treatment time and temperature, more precipitated phases with different sizes and different distributions are generated in the nickel-titanium alloy, so that the mechanical properties and the phase transition temperature of the nickel-titanium alloy are further improved, and the application requirements of the nickel-titanium alloy in the fields of aerospace, mechanical engineering, biomedical and the like are met.
In this embodiment, the step of forming the nickel-titanium shape memory alloy material by the laser near net forming technique includes:
s11, guiding the three-dimensional model into a laser near net shaping technology operation system;
s12, loading nickel-titanium raw material powder into a raw material powder cylinder;
s13, adopting a high-energy laser beam, introducing inert atmosphere for protection, adjusting laser parameters of laser near-net forming equipment, and according to a processing scanning path, enabling nickel-titanium raw material powder to be deposited layer by layer for fast melting and solidification, and forming a nickel-titanium shape memory alloy material on the surface of the substrate.
The invention adopts high-energy laser beam to effectively melt NiTi powder, reduces the escape of the powder, realizes the accurate design of NiTi materials according to components, and effectively establishes the association between the restorable performance of NiTi and the components; by adopting a closed inert atmosphere environment, the formation of C, O impurities in the preparation process of NiTi can be effectively inhibited.
The invention adopts a laser near-net forming double-nozzle coaxial powder feeding system, the whole equipment comprises a building cabin and a powder feeding barrel, the powder is visible, the composition is adjustable, the laser and the powder are fed simultaneously, the equipment is stable, and the oxygen content is controllable.
Wherein the nickel-titanium raw material powder is Ni x Ti 100-x The value range of x is 45-55.
Wherein the particle size of the nickel titanium raw material powder is 30-150 mu m.
Wherein the substrate is one or more of nickel-titanium alloy, nickel alloy, niobium alloy, titanium alloy, inconel625, inconel600, inconel718, inconel750 substrate.
Wherein the inert atmosphere is at least one of argon, nitrogen and helium.
Wherein, the laser parameters are: the laser power is 250-400W, including but not limited to 250W, 300W, 350W, 400W, etc.; the powder feeding rate of the raw material powder is 3-8g/min, including but not limited to 3g/min, 4g/min, 5g/min, 6g/min, 7g/min, 8g/min, etc.; the scanning rate is 400-800mm/min, including but not limited to 400mm/min, 500mm/min, 600mm/min, 700mm/min, 800mm/min, etc.; spot sizes of 0.5-3mm, including but not limited to 0.5mm, 1mm, 2mm, 3mm, etc.; the thickness of the single layer is 0.050 mm to 0.50mm, including but not limited to 0.05mm, 0.1mm, 0.2mm, 0.3mm, 0.4mm, 0.5mm, etc., and the working distance of the lowest end of the laser processing head relative to the substrate surface is 1mm to 25mm, including but not limited to 1mm, 5mm, 10mm, 15mm, 20mm, 25mm, etc.
The invention does not limit the processing scanning path, and the person skilled in the art can select according to the actual situation, for example, the processing scanning path of bidirectional zigzag, single forward and cyclic reciprocation can be adopted, so that the laser moves back and forth along the whole sample without stopping or overlapping.
The invention is not limited to the type of equipment used for the high-temperature heat treatment, and a person skilled in the art can select the equipment according to actual conditions, and for example, the equipment can be a high-temperature furnace, a heat treatment furnace, a heating furnace, a box furnace, an aging furnace, an induction furnace, a pit furnace, a tempering furnace and the like.
In a second aspect, the present invention provides a nickel-titanium shape memory alloy obtained by the heat treatment process for laser near net shape nickel-titanium shape memory alloy provided in the first aspect of the present invention.
In the invention, the tensile strength of the nickel-titanium shape memory alloy obtained after heat treatment is more than or equal to 550MPa, the elongation is more than or equal to 10 percent, and the phase transition temperature is more than or equal to 0 ℃.
Example 1
The nickel-titanium shape memory alloy specifically comprises the following steps:
(1) Ni is selected for 51.73 Ti 48.27 Shape memory alloy powder of the components is used as printing material;
(2) Selecting a nickel-titanium plate as a substrate, firstly polishing the surface of the substrate by using sand paper, and then cleaning the surface oil stain by using absolute ethyl alcohol;
(3) Firstly, filling high-purity inert gas in a building cabin to prevent a sample from being oxidized in the printing process; then, weighing a proper amount of nickel-titanium powder (the average particle diameter is 83.15 mu m), putting the nickel-titanium powder into a powder feeding barrel, and setting the working distance of the lowest end of the laser processing head relative to the surface of the substrate to be 9mm; parameters such as laser power, powder feeding speed, scanning speed and the like of laser near-net forming equipment are set, powder is directly injected into a molten pool system formed by a high-power continuous wave laser beam on a substrate, the powder is rapidly melted and solidified, the laser power is 350W, the powder feeding speed is 5g/min, the scanning speed is 600mm/min, the light spot size is 2.0mm, and the thickness of each single layer is 0.25mm.
(4) And (3) placing the prepared nickel-titanium shape memory alloy material into a high-temperature furnace, heating to 600 ℃, preserving heat for 2 hours, and cooling to room temperature along with the furnace.
In the method, the nickel-titanium shape memory alloy is prepared by adopting a laser near net forming process and a heat treatment process. Referring to FIGS. 1-2, the resulting product has a tensile strength of 582MPa, an elongation of 11.19%, and a phase transition temperature A s Is 0.57 ℃.
Example 2
The nickel-titanium shape memory alloy specifically comprises the following steps:
(1) Ni is selected for 50.93 Ti 49.07 Shape memory alloy powder of the components is used as printing material;
(2) Selecting a Nb plate as a substrate, polishing the surface of the substrate by sand paper, and cleaning the surface with absolute ethyl alcohol;
(3) Firstly, filling high-purity inert gas in a building cabin to prevent a sample from being oxidized in the printing process; then, weighing a proper amount of nickel-titanium powder (the average particle diameter is 76.89 mu m), putting the nickel-titanium powder into a powder feeding barrel, and setting the working distance of the lowest end of the laser processing head relative to the surface of the substrate to be 10mm; laser parameters such as laser power, powder feeding speed, scanning speed and the like of laser near-net forming equipment are set, powder is directly injected into a molten pool system formed by a high-power continuous wave laser beam on a substrate, rapid melting and solidification are carried out, the laser power is 350W, the powder feeding speed of the nickel-titanium shape memory alloy is 4g/min, the scanning speed is controlled at 600mm/min, the light spot size is 1mm, and the thickness of each single layer is 0.27mm.
(4) And (3) placing the formed nickel-titanium shape memory alloy material into a heating furnace to heat to 800 ℃, preserving heat for 2 hours, and cooling to room temperature along with the furnace.
In the method, the nickel-titanium shape memory alloy is prepared by adopting a laser near net forming process and a heat treatment process. Referring to FIGS. 1-2, the resulting product had a tensile strength of 686MPa, an elongation of 11.50%, and a phase transition temperature A s 1.44 ℃.
Example 3
The nickel-titanium shape memory alloy specifically comprises the following steps:
(1) Ni is selected for 51.15 Ti 48.85 Shape memory alloy powder of the components is used as printing material;
(2) Selecting a nickel-titanium plate as a substrate, firstly polishing the surface of the substrate by using sand paper, and then cleaning the surface oil stain by using absolute ethyl alcohol;
(3) Firstly, filling high-purity inert gas in a building cabin to prevent a sample from being oxidized in the printing process; then, weighing a proper amount of nickel-titanium powder (the average particle diameter is 87.65 mu m), putting the powder into a powder feeding barrel, and setting the working distance between the lowest end of the laser processing head and the surface of the substrate to be 9.5mm; by setting laser parameters such as laser power, powder feeding speed, scanning speed and the like of laser near-net forming equipment, powder is directly injected into a molten pool system formed by a high-power continuous wave laser beam on a substrate, and is rapidly melted and solidified, the laser power is 370W, the powder feeding speed of the nickel-titanium shape memory alloy is 6g/min, the scanning speed is controlled at 550mm/min, the light spot size is 1.2mm, and the thickness of each single layer is 0.27mm.
(4) And (3) placing the formed nickel-titanium shape memory alloy material into a heating furnace, heating to 600 ℃, preserving heat for 2 hours, and cooling to room temperature along with the furnace.
In the method, the nickel-titanium shape memory alloy is prepared by adopting a laser near net forming process and a heat treatment process. Referring to FIGS. 1-2, the resulting product has a tensile strength of 570MPa, an elongation of 13.78%, and a phase transition temperature A s 6.96 ℃.
Referring to fig. 3, fig. 3 is a microstructure effect diagram of the nickel-titanium shape memory alloy members prepared in examples 1-3. As can be seen from FIG. 3, the small size NiTi in example 1 2 The precipitated phase is distributed at the grain boundary; in example 2, niTi 2 The size of the precipitated phase increases and is distributed in the crystal, and at the same time, slender Ni can be observed 4 Ti 3 The precipitated phase is uniformly distributed in the crystal; in example 3, a precipitated phase of micron order size distributed near the grain boundary and inside the crystal was obtained, and the diffraction pattern could confirm the presence of the precipitated phase. Therefore, the size and the distribution of the precipitated phases in the nickel-titanium alloy can be effectively controlled by regulating and controlling the temperature and the heat preservation time of the heat treatment process.
Comparative example 1
The nickel-titanium shape memory alloy specifically comprises the following steps:
(1) Ni is selected for 51.73 Ti 48.27 Shape memory alloy powder of the components is used as printing material;
(2) Selecting a nickel-titanium plate as a substrate, firstly polishing the surface of the substrate by using sand paper, and then cleaning the surface oil stain by using absolute ethyl alcohol;
(3) Firstly, filling high-purity inert gas in a building cabin to prevent a sample from being oxidized in the printing process; then, weighing a proper amount of nickel-titanium powder (the average particle diameter is 83.15 mu m), putting the nickel-titanium powder into a powder feeding barrel, and setting the working distance of the lowest end of the laser processing head relative to the surface of the substrate to be 9mm; parameters such as laser power, powder feeding speed, scanning speed and the like of laser near-net forming equipment are set, powder is directly injected into a molten pool system formed by a high-power continuous wave laser beam on a substrate, the powder is rapidly melted and solidified, the laser power is 350W, the powder feeding speed is 5g/min, the scanning speed is 600mm/min, the light spot size is 2.0mm, and the thickness of each single layer is 0.25mm.
(4) And (3) placing the formed nickel-titanium shape memory alloy material into a heating furnace, heating to 1200 ℃, preserving heat for 2 hours, and cooling to room temperature along with the furnace.
In the method, the nickel-titanium shape memory alloy is prepared by adopting a laser near net forming process and a heat treatment process. Referring to FIGS. 4-5, the resulting product had a tensile strength of 352MPa, an elongation of 3.80% and a phase transition temperature of-13.88 ℃. It can be seen that the post-treatment of the comparative example adopts a high-temperature heat treatment process, namely, the heat treatment is carried out for 2 hours at 1200 ℃, the rest operation methods and processes are unchanged, the mechanical properties of the obtained product are obviously reduced, and the phase transition temperature is reduced.
Comparative example 2
The nickel-titanium shape memory alloy specifically comprises the following steps:
(1) Ni is selected for 51.73 Ti 48.27 Shape memory alloy powder of the components is used as printing material;
(2) Selecting a nickel-titanium plate as a substrate, firstly polishing the surface of the substrate by using sand paper, and then cleaning the surface oil stain by using absolute ethyl alcohol;
(3) Firstly, filling high-purity inert gas in a building cabin to prevent a sample from being oxidized in the printing process; then, weighing a proper amount of nickel-titanium powder (the average particle diameter is 83.15 mu m), putting the nickel-titanium powder into a powder feeding barrel, and setting the working distance of the lowest end of the laser processing head relative to the surface of the substrate to be 9mm; parameters such as laser power, powder feeding speed, scanning speed and the like of laser near-net forming equipment are set, powder is directly injected into a molten pool system formed by a high-power continuous wave laser beam on a substrate, the powder is rapidly melted and solidified, the laser power is 350W, the powder feeding speed is 5g/min, the scanning speed is 600mm/min, the light spot size is 2.0mm, and the thickness of each single layer is 0.25mm. The heat treatment process is not performed subsequently.
In the method, the nickel-titanium shape memory alloy is prepared by adopting a laser near net forming process. Referring to FIGS. 4-5, the resulting product had a tensile strength of 586MPa, an elongation of 5.66% and a phase transition temperature of-24.09 ℃. It can be seen that the subsequent process of the comparative example does not use a heat treatment process, and the mechanical properties and the phase transition temperature of the comparative example are obviously reduced by directly performing the performance test after printing by the LENS equipment.
The above-described embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made in accordance with the technical idea of the present invention shall be included in the scope of the claims of the present invention.
Claims (10)
1. A heat treatment process suitable for laser near-net forming nickel-titanium shape memory alloy, which is characterized by comprising the following steps:
forming a nickel-titanium shape memory alloy material by a laser near-net forming technology;
and carrying out high-temperature heat treatment on the nickel-titanium shape memory alloy material, and then cooling to room temperature along with a furnace to obtain the nickel-titanium shape memory alloy component.
2. The heat treatment process for the near-net-shape nickel-titanium shape memory alloy according to claim 1, wherein in the process of the high-temperature heat treatment, the heat treatment temperature is 300-1100 ℃, and the heat preservation time is 1-3h.
3. The heat treatment process for the near-net shape nickel-titanium shape memory alloy according to claim 2, wherein the heat treatment temperature is 600-800 ℃ during the high temperature heat treatment.
4. The heat treatment process for a laser near net shape nickel titanium shape memory alloy according to claim 1, wherein the step of forming the nickel titanium shape memory alloy material by a laser near net shape forming technique comprises:
the three-dimensional model is imported into a laser near net shaping technology operating system;
loading nickel-titanium raw material powder into a raw material powder cylinder;
the high-energy laser beam is adopted, inert atmosphere is introduced for protection, laser parameters of laser near-net forming equipment are adjusted, nickel titanium raw material powder is deposited layer by layer according to a processing scanning path to be quickly melted and solidified, and nickel titanium shape memory alloy materials are formed on the surface of a substrate.
5. The heat treatment process for a laser near-net shape nickel-titanium shape memory alloy according to claim 4, wherein said nickel-titanium raw material powder is Ni x Ti 100-x The value range of x is 45-55.
6. The heat treatment process for a laser near net shape nickel titanium shape memory alloy as claimed in claim 4, wherein the particle size of the nickel titanium raw material powder is 30-150 μm.
7. The heat treatment process for a laser near net shape nickel titanium shape memory alloy of claim 4, wherein the substrate is one or more of nickel titanium alloy, nickel alloy, niobium alloy, titanium alloy, inconel625, inconel600, inconel718, inconel750 substrates.
8. The heat treatment process for a laser near net shape nickel titanium shape memory alloy as claimed in claim 4, wherein the inert atmosphere is at least one of argon, nitrogen and helium.
9. The heat treatment process for a laser near net shape nickel titanium shape memory alloy according to claim 4, wherein the laser parameters are: the laser power is 250-400W, the powder feeding rate of the raw material powder is 3-8g/min, the scanning rate is 400-800mm/min, the light spot size is 0.5-3mm, the single-layer thickness is 0.050-0.50mm, and the working distance of the lowest end of the laser processing head relative to the surface of the substrate is 1-25mm.
10. A nickel titanium shape memory alloy, characterized in that it is obtained by a heat treatment process according to any one of claims 1-9, suitable for laser near net shape nickel titanium shape memory alloys.
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