CN114669751A - Preparation method of crack-free nickel-titanium-copper alloy for additive manufacturing - Google Patents

Preparation method of crack-free nickel-titanium-copper alloy for additive manufacturing Download PDF

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CN114669751A
CN114669751A CN202210390755.1A CN202210390755A CN114669751A CN 114669751 A CN114669751 A CN 114669751A CN 202210390755 A CN202210390755 A CN 202210390755A CN 114669751 A CN114669751 A CN 114669751A
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titanium
nickel
copper alloy
substrate
crack
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CN114669751B (en
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张利军
李志诚
钟静
易旺
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Central South University
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Central South University
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    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20—Direct sintering or melting
    • B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • 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
    • B22F10/40—Structures for supporting workpieces or articles during manufacture and removed afterwards
    • 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
    • B22F10/80—Data acquisition or data processing
    • B22F10/85—Data acquisition or data processing for controlling or regulating additive manufacturing processes
    • 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
    • B33Y50/00—Data acquisition or data processing for additive manufacturing
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Abstract

A preparation method of crack-free nickel-titanium-copper alloy for additive manufacturing comprises the steps of firstly calculating the thermal cracking tendency in the range of target alloy components, selecting the alloy component with the lowest thermal cracking tendency for proportioning and smelting, and preparing nickel-titanium-copper alloy powder by a gas atomization method; designing a 'grid lapping' parameter optimization structure, modeling the structure of the 'grid lapping' parameter optimization structure and the part structure, designing a position and a support, and carrying out slicing treatment; then keeping the original coordinates of the model unchanged, setting a printing path and a scanning strategy, inputting process parameters, and copying the set engineering file into SLM equipment; then debugging equipment is debugged, printing the lamella to form a new substrate, and then printing parts; when the temperature of the substrate is reduced to below 70 ℃, taking down the substrate with the printing piece, and placing the substrate in a furnace for heat preservation; and finally, cutting the printed piece from the substrate and grinding to obtain the nickel-titanium-copper alloy. According to the invention, the printing cracks are eliminated through component design, process parameter optimization and structural design, and the nickel-titanium-copper alloy with high density, good formability and excellent comprehensive performance is prepared.

Description

Preparation method of crack-free nickel-titanium-copper alloy for additive manufacturing
Technical Field
The invention relates to the technical field of metal additive manufacturing, in particular to a preparation method of a crack-free nickel-titanium-copper alloy for additive manufacturing.
Background
Nickel titanium based alloys are the most widely used shape memory alloys at present. Among them, the nitinol thin film and the spring show a high power ratio, a high recoverable stress, and excellent fatigue properties, and are widely used in microactuator devices and spring brakes. However, the nickel-titanium-copper shape memory alloy prepared by the traditional processing technology has high cost and complex process, and is difficult to realize the manufacture of complex structures. Selective Laser Melting (SLM) is used as a 3D printing method for accurately controlling forming, the smoothness and the geometric accuracy of parts can be guaranteed, and the manufacture of the structure-function integrated shape memory alloy can be realized. Therefore, the SLM technology is considered as a key technology for the preparation of the new generation of nitinol.
However, as a rapid solidification process, the complicated thermal history (high temperature inside the molten pool and high cooling speed on the boundary of the molten pool) in the forming process of manufacturing some alloy parts by adopting the SLM technology can cause the non-equilibrium solidification to be intensified, and the alloy is repeatedly remelted, so that the residual stress in the printed alloy is high, thereby being easy to generate deformation and cracking and influencing the comprehensive performance of the alloy. Particularly, for the preparation of NiTiCu alloy by adopting SLM process, the Cu element has high reflectivity, and the precipitated phase generated in the solidification process can cause alloy embrittlement, so that the cracking problem becomes the biggest obstacle of the application of the NiTiCu alloy.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a crack-free nickel-titanium-copper alloy for additive manufacturing, which is characterized in that target alloy components with lower crack sensitivity are preferably selected through component design, process parameters and a scanning strategy are optimized on the basis of adopting a selective laser melting technology, and unique structural design is carried out, so that alloy cracks in a 3D printing forming process are effectively reduced, and the nickel-titanium-copper alloy with good formability and excellent comprehensive performance is prepared.
In order to solve the technical problems, the invention adopts the following technical method: a preparation method of a crack-free nickel-titanium-copper alloy for additive manufacturing comprises the following steps:
step S1, component design: calculating the hot cracking tendency in the range of target alloy components based on a Hill solidification model and a crack sensitive factor calculation method, and selecting the alloy component with the lowest hot cracking tendency for batching;
step S2, preparing a powder: smelting and ingot casting are carried out according to the alloy components selected in the step S1 to obtain a nickel-titanium-copper alloy bar, then nickel-titanium-copper pre-alloy powder is prepared through an air atomization method, the nickel-titanium-copper pre-alloy powder is screened and then dried in vacuum to obtain nickel-titanium-copper alloy powder;
step S3, modeling the three-dimensional structure: designing a 'grid lapping' parameter optimization structure, respectively carrying out 3D modeling on the 'grid lapping' parameter optimization structure and a part structure by using NX-10 and Materialise-Magics3 software, designing a position, supporting, and carrying out slicing treatment, wherein the thickness of a sheet layer is layered according to the minimum layer thickness of 0.01 mm;
step S4, setting process parameters: keeping the original coordinates of the model constructed in the step S3 unchanged, setting a printing path as a branch melting channel for layer-by-layer printing, setting a scanning strategy as a strip division and interlayer rotation, inputting process parameters optimized by adopting a 'mesh lapping' parameter optimization structure model, and copying the set engineering file into SLM equipment;
step S5, print forming: firstly, debugging equipment, introducing argon, and preheating a substrate; printing a 1mm thick sheet layer with the same component as the part in advance to form a new substrate, and then finishing the part printing; cooling the substrate to below 70 ℃, taking down the substrate with the printing piece, placing the substrate in a furnace for heat preservation, and performing stress relief annealing; and finally, cutting the printed part from the substrate, and grinding the surface of the part to obtain the nickel-titanium-copper alloy part.
Further, in step S2, after obtaining the nickel-titanium-copper alloy bar, putting the nickel-titanium-copper alloy bar into a small vacuum induction gas atomization powder making device, controlling the oxygen content in the whole process within 600ppm, preparing nickel-titanium-copper pre-alloy powder through a gas atomization method, then sieving the nickel-titanium-copper pre-alloy powder through a 200-mesh screen to remove large-particle powder, and then putting the nickel-titanium-copper pre-alloy powder into a 100 ℃ vacuum drying oven to dry for more than 2 hours, so as to obtain the nickel-titanium-copper alloy powder with the particle size of 15-53 μm and the sphericity of more than 95%.
Further, in step S3, when the part structure is 3D modeled using NX-10 and materials-Magics 3 software, a "bullnose" structure is provided on the edge of the part, with a bullnose radius of 2-4 mm.
Further, in step S3, when the part structure is 3D modeled using NX-10 and materials-Magics 3 software, a "fillet" structure is provided at the contact portion of the part and the substrate, and the fillet radius is 2-4 mm.
Still further, in step S3, the method for designing the "mesh lapping" parameter optimization structure is as follows:
firstly, arranging the decomposed selective laser melting process parameters into an orthogonal table, constructing a 22mm multiplied by 29mm multiplied by 4mm cuboid with a 2mm chamfer angle, equally dividing the cuboid into 12 independent blocks with the size of 8mm multiplied by 4mm before slicing, wherein the adjacent grids contain a 1mm lap joint area, copying a module, reasonably arranging the modules, and assigning the process parameters in the orthogonal table to 24 independent blocks in sequence to obtain a 'grid lap joint' parameter optimization structure.
Still further, in step S3, when the "mesh lapping" parameter optimization structure is 3D modeled using NX-10 and material-Magics 3 software, process parameters are optimized in an orthogonal table form, three parameters among laser power, scanning speed, scanning pitch, and spot diameter are controlled to be constant values, and another parameter is changed to determine the optimal range of each parameter.
Further, in step S3, the optimized process parameters are: the laser power is 100-.
Further, in step S4, the stripe division plus interlayer rotation has a stripe width of 4-10mm, an interlayer rotation angle of 67 °, and an initial scan angle of 0-57 °.
Further, in step S5:
when debugging equipment, cleaning a powder bin of the SLM equipment, closing a bin door of a forming chamber, introducing argon, setting the preheating temperature of a substrate to be 180 ℃ when the oxygen content in the forming chamber is lower than 300ppm, when the temperature of the substrate is raised to 150 ℃, sending the nickel-titanium-copper alloy powder prepared in the step S2 into the SLM equipment, manually spreading the powder, and executing a printing program when the spreading is observed to be smooth and good in fluidity;
when printing a part, selecting a nickel-titanium alloy substrate as a printing substrate, firstly printing a 1mm thick sheet layer with the same components as the part on the substrate by SLM equipment, remelting the sheet layer twice on the upper layer, and cooling the sheet layer to the temperature of the substrate to be used as a new substrate; then, according to the slice data set in the step S4, automatic powder spreading scanning and printing of parts are started, when manufacturing of one layer is completed, the workbench is lowered by one powder spreading layer thickness, the scraper flattens the nickel-titanium-copper alloy powder again, manufacturing of the next layer is performed, the circulation is continuously carried out until the printing of the whole part is completed, if severe warping occurs, the printing of the corresponding process is stopped, in the printing process, argon is introduced into the forming chamber, the content of oxygen is reduced to be below 300ppm, the air pressure is kept to be 10-20mbar, convection air blowing is kept in the forming chamber, the air speed of an air outlet is changed according to the quantity of residues, and impurity residues are removed;
and after printing is finished, stopping heating the substrate, reducing the pressure in the forming chamber when the temperature of the substrate is reduced to below 70 ℃, removing residual powder, taking down the substrate with the printed piece, placing the substrate and the printed piece in a vacuum furnace or a 200 ℃ furnace filled with inert gas for heat preservation for 2h, performing stress relief annealing, then performing air cooling to room temperature, cutting the printed piece from the substrate by utilizing wire cutting, treating the surface of the part by using an automatic grinding machine, and grinding oxide skin formed by wire cutting to obtain the nickel-titanium-copper alloy part.
Preferably, the nickel-titanium-copper alloy powder comprises the following components in percentage by mass: nickel-45.04 wt.%, copper-10.01 wt.%, silicon-0.10 wt.%, oxygen-0.054 wt.%, aluminum-0.10 wt.%, iron-0.04 wt.%, chromium-0.05 wt.%, cobalt-0.008 wt.%, molybdenum-0.04 wt.%, zirconium-0.02 wt.%, unspecified further elements, each of ≦ 0.02 wt.%, total ≦ 0.10 wt.%, the balance titanium.
According to the preparation method of the crack-free nickel-titanium-copper alloy for additive manufacturing, provided by the invention, cracks in 3D printing are eliminated through component design, process parameter optimization and structural design, so that the nickel-titanium-copper alloy with the advantages of no cracks on the surface, high density, good formability and excellent comprehensive performance is prepared. Specifically, the invention provides an alloy component with low crack sensitivity by efficiently screening target alloy components based on a Hill solidification model and a crack sensitivity factor calculation method provided by Kou. In addition, the invention provides a frame for efficiently optimizing process parameters, which decomposes the process parameters by adopting an orthogonal table and is matched with an autonomously designed 'mesh lapping' parameter optimization structure, so that the energy density can be regulated and controlled in a large range in one-time printing, the quality of a printed sample is efficiently evaluated, and the optimal parameter range is obtained. Furthermore, the invention firstly provides a structural design method for reducing internal stress, avoiding warping and eliminating cracks, and the design of printing a substrate and rounding is introduced into the structure of the part, so that the stress concentration on the part can be obviously reduced on the premise of not changing the original process parameters, and the warping and cracking of the part can be effectively prevented. In conclusion, the invention firstly provides an efficient process optimization strategy and a structure design method based on the selective laser melting technology, which can effectively eliminate nickel-titanium-copper alloy cracks formed by 3D printing and prepare the nickel-titanium-copper alloy with good formability and excellent comprehensive performance. The invention provides a new feasible process for preparing the nickel-titanium-copper alloy with the complex structure, and is expected to expand the application range of the nickel-titanium-copper alloy.
Drawings
FIG. 1 is a flow chart of a method for preparing a crack-free nickel-titanium-copper alloy for additive manufacturing according to the present invention;
FIG. 2 is a schematic diagram showing the calculation results of crack sensitivity factors of nickel-titanium-copper alloys with different components in the preparation method of crack-free nickel-titanium-copper alloys for additive manufacturing according to the present invention;
FIG. 3 is a schematic diagram of a scanning strategy in the method for preparing a crack-free Ni-Ti-Cu alloy for additive manufacturing according to the present invention;
FIG. 4 is a schematic view of a nickel-titanium-copper alloy printed according to example 1 of the present invention;
FIG. 5 is a schematic view of a nickel-titanium-copper alloy printed according to example 2 of the present invention;
FIG. 6 is a schematic view of a nickel-titanium-copper alloy printed according to example 3 of the present invention;
FIG. 7 is a surface scanning electron micrograph of a shaped nickel-titanium-copper alloy prepared by SLM in examples 1 to 3 of the present invention (in the figures, (a), (c) are planar regions perpendicular to the manufacturing direction (X-Y) and parallel to the manufacturing direction (X-Z) in example 3-b, (b) is a planar region perpendicular to the manufacturing direction (X-Y) in example 2-a, and (d) is a planar region parallel to the manufacturing direction (X-Z) in example 3).
Detailed Description
In order to facilitate understanding of those skilled in the art, the present invention will be further described with reference to the following examples and drawings, which are not intended to limit the present invention.
The method mainly eliminates the cracks of the parts in the 3D printing process through component design, process parameter optimization and structure design, so that the nickel-titanium-copper alloy with good formability and excellent comprehensive performance is prepared, which is the key for expanding the application of the nickel-titanium-copper shape memory alloy and has wide practical value. The present invention will be described in detail with reference to examples.
Example 1
A preparation method of a crack-free nickel-titanium-copper alloy for additive manufacturing is shown in figure 1 and comprises the following steps:
step S1, designing components: based on the Hill coagulation model and Kou et al [ S.Kou Acta Materialia 88(2015) 366-]The proposed method for calculating the crack sensitivity factor uses the thermodynamic calculation software Pandat https:// computherm]Calculating the thermal cracking tendency in the range of the target alloy components, as shown in fig. 2, as the calculation result of the crack sensitive factors of the nitinol with different components, selecting the alloy component with the lowest thermal cracking tendency for batching, specifically, in this embodiment 1, the selected alloy component is calculated by mass percentage: nickel-45.04 wt.%, copper-10.01 wt.%, silicon-0.10 wt.%, oxygen-0.054 wt.%, aluminum-0.10 wt.%, iron-0.04 wt.%, chromium-0.05 wt.%, cobalt-0.008 wt.%, molybdenum-0.04 wt.%, zirconium-0.02 wt.%, unspecified further elements, each of ≦ 0.02 wt.%, total ≦ 0.10 wt.%, the balance titanium. Wherein the main component titanium has a purity of 99.995% and
Figure BDA0003595397940000053
the nickel is 99.995% pure and
Figure BDA0003595397940000051
the purity of the high-purity nickel columnar particles and the copper is 99.99 percent
Figure BDA0003595397940000052
The pure copper particles of (1).
Step S2, preparing a powder: and (4) carrying out smelting and ingot casting according to the alloy components selected in the step S1 to obtain the nickel-titanium-copper alloy bar with uniform components. Then putting the nickel-titanium-copper alloy bar into a small-sized vacuum induction gas atomization powder preparation device, controlling the oxygen content in the whole process within 600ppm, preparing nickel-titanium-copper prealloying powder by a gas atomization method, then sieving the nickel-titanium-copper prealloying powder through a 200-mesh screen to remove large-particle powder, and then putting the nickel-titanium-copper prealloying powder into a 100 ℃ vacuum drying oven to be dried for more than 2 hours to obtain the nickel-titanium-copper alloy powder with the particle size of 15-53 mu m and the sphericity of more than 95%, wherein the nickel-titanium-copper alloy powder has good fluidity.
Step S3, modeling three-dimensional structure
S31, designing a 'mesh lapping' parameter optimization structure: the decomposed selective laser melting process parameters are listed in an orthogonal table, as shown in table 1 and table 2, a cuboid with 2mm rounded corners and the size of 22mm multiplied by 29mm multiplied by 4mm is constructed, the cuboid is equally divided into 12 independent blocks with the size of 8mm multiplied by 4mm before slicing, 1mm lap joint areas are contained between adjacent grids, modules are copied and reasonably arranged, the process parameters in the orthogonal table are sequentially assigned to the 24 independent blocks, and a set of efficient 'grid lap joint' parameter optimization structure is obtained.
Table 1 parameter optimization orthogonal table a
Figure BDA0003595397940000061
TABLE 2 parameter optimization orthogonal Table b
Figure BDA0003595397940000062
Figure BDA0003595397940000071
S32, structural design: the structure combining the printing substrate and the fillet is adopted.
Selecting a nickel-titanium alloy substrate as a printing substrate, firstly printing four 1 mm-thick sheet layers with the same component as the part on the substrate by SLM equipment, remelting the sheet layers twice on the upper layer, and cooling the sheet layers to the temperature of the substrate to be used as a new substrate, wherein the new substrate can reduce the internal stress between the substrate and the printing part and prevent warping; a10 mm x 5mm part is formed on each new substrate, and a fillet with a radius of 2mm is provided at the contact portion of the part and the new substrate. On the base plate, the four parts are rotated clockwise by 15 ° forming an inclination with the direction of travel of the scraper.
S33, modeling: and respectively carrying out 3D modeling on the grid lapping parameter optimization structure and the part structure by using NX-10 and Materialise-Magics3 software, designing positions and supports, and carrying out slicing treatment, wherein the thickness of the sheet layer is layered according to the minimum layer thickness of 0.01 mm.
When NX-10 and Materialise-Magics3 software are used for carrying out 3D modeling on a 'grid lapping' parameter optimization structure, process parameters are optimized in an orthogonal table form, 48 process parameters are printed at one time during optimization, the quality of a printed sample is efficiently evaluated, specifically, three parameters of laser power, scanning speed, scanning distance and spot diameter are controlled to be constant values, the other parameter is changed, the optimal range of the other parameter is determined, and the optimized process parameter range is as follows: the laser power is 100-.
Step S4, setting process parameters: keeping the original coordinates of the model constructed in the step S3 unchanged, setting a printing path to be a melting channel layer-by-layer printing, and setting a scanning strategy to be a strip division and interlayer rotation, as shown in fig. 3, wherein the strip width is 4mm, the interlayer rotation angle is 67 °, the initial scanning included angle is 0 °, and the process parameters optimized in the step S33 are selected as follows:
(a) the laser power is 140W, the scanning speed is 1000mm/s, the scanning interval is 60 mu m, the spot diameter is 60 mu m, and the powder layer thickness is 50 mu m;
(b) the method comprises the following steps The laser power is 130W, the scanning speed is 1000mm/s, the scanning interval is 80 μm, the spot diameter is 60 μm, and the powder layer thickness is 50 μm;
(c) the method comprises the following steps The laser power is 135W, the scanning speed is 1000mm/s, the scanning interval is 80 mu m, the spot diameter is 60 mu m, and the powder layer thickness is 50 mu m;
(d) the method comprises the following steps The laser power is 160W, the scanning speed is 1000mm/s, the scanning interval is 100 μm, the spot diameter is 60 μm, and the powder layer thickness is 50 μm.
And copying the set engineering file into SLM equipment, wherein the SLM equipment selects a BLT-A320 selective laser melting metal 3D printer.
Step S5, print forming
S51, debugging the equipment: cleaning a powder bin of the SLM equipment, closing a bin door of a forming chamber, introducing argon, setting the preheating temperature of a substrate to be 180 ℃ when the oxygen content in the forming chamber is lower than 300ppm, feeding the nickel-titanium-copper alloy powder prepared in the step S2 into the SLM equipment when the temperature of the substrate rises to 150 ℃, manually spreading the powder, and executing a printing program when the spreading of the powder is flat and good in fluidity;
s52, print part: after the SLM equipment prints a new substrate, automatic powder spreading scanning and printing of parts are started according to slice data set in the step S4, when manufacturing of one layer is completed, the workbench descends by one powder spreading layer thickness, namely 50 micrometers, the scraper flattens nickel-titanium-copper alloy powder again, here, the scraper selects a 40-steel hard scraper to manufacture the next layer, the manufacturing is continuously and circularly performed until the printing of the whole part is completed, if severe warping occurs, the printing of the corresponding process is stopped, and it is noted that in the printing process, argon gas is introduced into the forming chamber, in order to protect the argon gas, the content of oxygen needs to be reduced to be below 300ppm, the air pressure is kept to be 10-20mbar, in addition, convection air blowing is kept in the forming chamber, the air outlet air speed is changed according to the quantity of residues, and impurity residues are removed.
S53, post-processing: after printing is finished (as shown in fig. 4), stopping heating the substrate, reducing the pressure in the forming chamber when the temperature of the substrate is reduced to below 70 ℃, removing residual powder, taking down the substrate with the printing piece, placing the substrate and the printing piece in a vacuum furnace or a 200 ℃ furnace filled with inert gas for heat preservation for 2 hours, removing stress, annealing, and then air cooling to room temperature. And cutting the printed part from the base plate by using wire cutting, processing the surface of the part by using an automatic grinding machine, and grinding the oxide skin formed by the wire cutting to obtain the nickel-titanium-copper alloy part with a smooth and bright surface.
And (5) cutting off part of the part obtained in the step S53, grinding and polishing the part, then shooting the surface appearance, and testing the mechanical property and the phase transformation behavior. The scanning topography of the nitinol alloy obtained by the process parameter (b) in the embodiment 1 is shown in fig. 7(a, c), and the alloy properties are as follows: vickers Hardness (HV) of 302.1HV5.0The compressive strength (. sigma.) was 683.42MPa, the elongation (. delta.) was 6.21%, and the phase change hysteresis was 12.1 ℃.
Example 2
A preparation method of a crack-free nickel-titanium-copper alloy for additive manufacturing is disclosed, which is different from example 1 only in that:
1) the structure designed in step S32 is: the structure combining the 'external fillet' and the 'internal fillet' is adopted. Specifically, in step S33, when the part structure is 3D modeled by using NX-10 and material-Magics 3 software, four parts are constructed on a substrate, wherein three parts are truncated pyramids with an upper surface of 25mm × 25mm, a lower surface of 30mm × 30mm and a height of 8mm, and a fillet with a radius of 3mm is constructed on the edges of the three parts, and another part is a common truncated cone with an upper surface radius of 12mm and a lower surface radius of 15mm, and all parts are provided with fillets with a radius of 3mm at contact parts with the substrate. On the base plate, the four parts are rotated 15 ° clockwise, forming an inclination with the direction of travel of the blade.
2) When the process parameters are set in step S4: keeping the original coordinates of the model constructed in the step S3 unchanged, setting a printing path as a branch melt channel for layer-by-layer printing, and setting a scanning strategy as a strip division and interlayer rotation, wherein the strip width is 4mm, the interlayer rotation angle is 67 degrees, the initial scanning included angle is 57 degrees, and the process parameters optimized in the step S33 are selected as follows:
a) the method comprises the following steps The laser power is 130W, the scanning speed is 1000mm/s, the scanning interval is 80 μm, the spot diameter is 60 μm, and the powder layer thickness is 50 μm;
(b) the method comprises the following steps The laser power is 135W, the scanning speed is 1000mm/s, the scanning interval is 80 mu m, the spot diameter is 60 mu m, and the powder layer thickness is 50 mu m;
(c) the method comprises the following steps The laser power is 140W, the scanning speed is 1000mm/s, the scanning interval is 80 μm, the spot diameter is 60 μm, and the powder layer thickness is 50 μm;
(d) the method comprises the following steps The laser power is 150W, the scanning speed is 1100mm/s, the scanning interval is 80 μm, the spot diameter is 60 μm, and the powder layer thickness is 50 μm.
And copying the set engineering file into SLM equipment, wherein the SLM equipment selects a BLT-A320 selective laser melting metal 3D printer.
3) In step S53, the finished nitinol is printed as shown in fig. 5.
4) In this example 2, the scanning topography of the nitinol alloy obtained by using the process parameters (b) is shown in fig. 7(b), and the alloy properties are as follows: vickers Hardness (HV) 317.5HV5.0The compressive strength (. sigma.) was 847.75MPa, the elongation (. delta.) was 7.46%, and the phase change hysteresis was 11.1 ℃.
Example 3
A preparation method of a crack-free nickel-titanium-copper alloy for additive manufacturing is disclosed, which is different from example 1 only in that:
1) the structure designed in step S32 is: the method comprises the following steps of adopting a combined structure of a printing substrate, an excircle corner and an inner fillet corner, selecting a nickel-titanium alloy substrate as the printing substrate, firstly printing a sheet layer which is 1mm thick, 80mm long and 80mm wide and has a fillet and the same component as a part on the substrate by SLM equipment, remelting the sheet layer twice on the upper layer, and cooling the sheet layer to the temperature of the substrate to serve as a new substrate, wherein the new substrate can reduce the internal stress between the substrate and the printing part and prevent warping; a part is constructed on a new substrate, the part is a frustum with an upper surface of 50mm multiplied by 50mm, a lower surface of 60mm multiplied by 60mm and a height of 8mm, a fillet of 4mm is arranged on the edge of the part, and a fillet of 4mm is arranged at the contact part of the part and the substrate.
2) When the process parameters are set in step S4: keeping the original coordinates of the model constructed in the step S3 unchanged, setting a printing path as a branch melt channel layer-by-layer printing, and setting a scanning strategy as a strip division and interlayer rotation, wherein the strip width is 4mm, the interlayer rotation angle is 67 degrees, the initial scanning included angle is 57 degrees, the optimized process parameters in the step S33 are selected, namely the laser power is 135W, the scanning speed is 1000mm/S, the scanning interval is 80 mu m, the spot diameter is 60 mu m, the powder laying layer thickness is 50 mu m, and the energy density is 33.75J/mm3。
3) In step S53, the finished nitinol is printed as shown in fig. 6.
4) The scanning topography of the nitinol alloy obtained in this example 3 is shown in fig. 7(d), and the alloy properties are as follows: vickers Hardness (HV) 310.5HV5.0The compressive strength (. sigma.) was 885.76MPa, the elongation (. delta.) was 7.21%, and the phase change hysteresis was 12.7 ℃.
The following table 3 shows the density comparison of the nickel-titanium-copper alloy obtained by the printing and the process parameters used in each of examples 1 to 3.
Table 3 process parameters and density comparisons used in examples 1-3
Figure BDA0003595397940000101
Figure BDA0003595397940000111
As can be seen from the comparison of Table 3 and FIG. 4, the scanning strategy of example 1The initial angle is 0 degrees, and because the scanning path needs to avoid the direction of the air outlet, only 2 scanning directions are mutually overlapped in the actual printing process, so that the stress concentration occurs on the part corners, and the warping is caused. Example 2-3 the initial angle in the scanning strategy was 57 °, 5 scan directions were present during the actual printing process, and saw-tooth grain boundaries could be formed between the layers, hindering crack propagation, and significantly improving the ductility of SLM-formed NiTiCu alloys. The process parameters have great influence on the formability and the compactness of the alloy in a printing state, and the energy density is more than 33.5J/mm3Can obtain a printing sample with the density meeting the requirement.
FIG. 7 is a scanning electron micrograph of the surface of a shaped nickel-titanium-copper alloy prepared by SLM, wherein (a) and (c) are the planar regions perpendicular to the manufacturing direction (X-Y) and parallel to the manufacturing direction (X-Z) of example 3-b, respectively; (b) is the planar area of example 2-a perpendicular to the direction of manufacture (X-Y); (d) example 3 is a planar area parallel to the direction of manufacture (X-Z). Wherein, no crack exists on the X-Y plane, a small amount of pores can be seen, a small amount of component segregation exists, and the whole structure is uniform. No crack on the X-Z plane, less pores and component segregation along the bottom of the molten pool, good integral formability and uniform structure. As can be seen from the figure 7, the method adopts the selective laser melting technology, and introduces the component design, the process optimization and the structure design method, so that the prepared nickel-titanium-copper alloy has no crack and good formability.
Generally, the nickel-titanium-copper alloy block printed by the method has the density as high as 99.1 +/-0.1%, no surface crack, no obvious large-size defect (such as a hole, a crack or an inclusion), uniform tissue and good formability. The phase transition temperature range of the nickel-titanium-copper alloy block is 12.1-40.0 ℃, the phase transition lag (Af-Ms) is 11.1-12.7 ℃, and the narrow phase transition lag effect is good. In addition, the hardness of the nickel-titanium-copper alloy block can reach 317.5 +/-7.6 HV5.0The compression strength is 885.76 +/-20.3 MPa, the compression strain is 7.36 +/-0.34 percent, and the mechanical property is good.
The above embodiments are preferred implementations of the present invention, and the present invention can be implemented in other ways without departing from the spirit of the present invention.
Some of the drawings and descriptions of the present invention have been simplified to facilitate the understanding of the improvements over the prior art by those skilled in the art, and other elements have been omitted from this document for the sake of clarity, and it should be appreciated by those skilled in the art that such omitted elements may also constitute the subject matter of the present invention.

Claims (10)

1. A preparation method of a crack-free nickel-titanium-copper alloy for additive manufacturing is characterized by comprising the following steps:
step S1, component design: calculating the hot cracking tendency in the range of target alloy components based on a Hill solidification model and a crack sensitive factor calculation method, and selecting the alloy component with the lowest hot cracking tendency for batching;
step S2, preparing a powder: smelting and ingot casting are carried out according to the alloy components selected in the step S1 to obtain a nickel-titanium-copper alloy bar, then nickel-titanium-copper pre-alloy powder is prepared through an air atomization method, the nickel-titanium-copper pre-alloy powder is screened and then dried in vacuum to obtain nickel-titanium-copper alloy powder;
step S3, modeling the three-dimensional structure: designing a 'grid lapping' parameter optimization structure, respectively carrying out 3D modeling on the 'grid lapping' parameter optimization structure and a part structure by using NX-10 and Materialise-Magics3 software, designing a position, supporting, and carrying out slicing treatment, wherein the thickness of a sheet layer is layered according to the minimum layer thickness of 0.01 mm;
step S4, setting process parameters: keeping the original coordinates of the model constructed in the step S3 unchanged, setting a printing path as a branch melting channel for layer-by-layer printing, setting a scanning strategy as a strip division and interlayer rotation, inputting process parameters optimized by adopting a 'mesh lapping' parameter optimization structure model, and copying the set engineering file into SLM equipment;
step S5, print forming: firstly, debugging equipment, introducing argon, and preheating a substrate; printing a 1mm thick sheet layer with the same component as the part in advance to form a new substrate, and then finishing the part printing; cooling the substrate to below 70 ℃, taking down the substrate with the printing piece, placing the substrate in a furnace for heat preservation, and performing stress relief annealing; and finally, cutting the printed part from the substrate, and grinding the surface of the part to obtain the nickel-titanium-copper alloy part.
2. The method for preparing the crack-free nickel-titanium-copper alloy for additive manufacturing according to claim 1, wherein the crack-free nickel-titanium-copper alloy for additive manufacturing comprises the following steps: in step S2, after obtaining the nickel-titanium-copper alloy bar, placing the nickel-titanium-copper alloy bar into a small vacuum induction gas atomization powder making device, controlling the oxygen content in the whole process within 600ppm, preparing nickel-titanium-copper pre-alloy powder by a gas atomization method, then sieving the nickel-titanium-copper pre-alloy powder through a 200-mesh sieve to remove large-particle powder, and then placing the nickel-titanium-copper pre-alloy powder into a 100 ℃ vacuum drying oven to dry for more than 2 hours, thereby obtaining the nickel-titanium-copper alloy powder with the particle size of 15-53 μm and the sphericity of more than 95%.
3. The method for preparing the crack-free nickel-titanium-copper alloy for additive manufacturing according to claim 2, wherein the crack-free nickel-titanium-copper alloy for additive manufacturing comprises the following steps: in step S3, when the part structure is subjected to 3D modeling by using NX-10 and materials-Magics 3 software, a 'bullnose' structure is arranged on the edge of the part, and the radius of the bullnose is 2-4 mm.
4. The method for preparing the crack-free nickel-titanium-copper alloy for additive manufacturing according to claim 2 or 3, wherein the crack-free nickel-titanium-copper alloy for additive manufacturing comprises the following steps: in step S3, when the part structure is 3D modeled using NX-10 and materials-Magics 3 software, a fillet structure is provided at the contact portion of the part and the substrate, and the radius of the fillet is 2-4 mm.
5. The method for preparing the crack-free nickel-titanium-copper alloy for additive manufacturing according to claim 4, wherein the crack-free nickel-titanium-copper alloy for additive manufacturing comprises the following steps: in step S3, the method for designing the "mesh lapping" parameter optimization structure is as follows:
firstly, arranging the decomposed selective laser melting process parameters into an orthogonal table, constructing a 22mm multiplied by 29mm multiplied by 4mm cuboid with a 2mm chamfer angle, equally dividing the cuboid into 12 independent blocks with the size of 8mm multiplied by 4mm before slicing, wherein the adjacent grids contain a 1mm lap joint area, copying a module, reasonably arranging the modules, and assigning the process parameters in the orthogonal table to 24 independent blocks in sequence to obtain a 'grid lap joint' parameter optimization structure.
6. The method for preparing the crack-free nickel-titanium-copper alloy for additive manufacturing according to claim 5, wherein the crack-free nickel-titanium-copper alloy for additive manufacturing comprises the following steps: in step S3, when 3D modeling is performed on the "mesh lapping" parameter optimization structure using NX-10 and Materialise-Magics3 software, process parameters are optimized in an orthogonal table form, three parameters among laser power, scanning speed, scanning pitch, and spot diameter are controlled to be constant values, and the other parameter is changed to determine the optimal range of each parameter.
7. The method for preparing the crack-free nickel-titanium-copper alloy for additive manufacturing according to claim 6, wherein the crack-free nickel-titanium-copper alloy for additive manufacturing comprises the following steps: in step S3, the optimized process parameters are: the laser power is 100-.
8. The method for preparing the crack-free nickel-titanium-copper alloy for additive manufacturing according to claim 7, wherein the crack-free nickel-titanium-copper alloy for additive manufacturing comprises the following steps: in step S4, the width of the stripe in the stripe division and interlayer rotation is 4-10mm, the interlayer rotation angle is 67 °, and the initial scan angle is 0-57 °.
9. The method for preparing the crack-free nickel-titanium-copper alloy for additive manufacturing according to claim 8, wherein the crack-free nickel-titanium-copper alloy for additive manufacturing comprises the following steps: in step S5:
when debugging equipment, cleaning a powder bin of the SLM equipment, closing a bin door of a forming chamber, introducing argon, setting the preheating temperature of a substrate to be 180 ℃ when the oxygen content in the forming chamber is lower than 300ppm, when the temperature of the substrate rises to 150 ℃, sending the nickel-titanium-copper alloy powder prepared in the step S2 into the SLM equipment, manually spreading the powder, and executing a printing program when the spreading of the powder is flat and good in fluidity;
when printing a part, selecting a nickel-titanium alloy substrate as a printing substrate, firstly printing a 1mm thick sheet layer with the same components as the part on the substrate by SLM equipment, remelting the sheet layer twice on the upper layer, and cooling the sheet layer to the temperature of the substrate to be used as a new substrate; then, according to the slice data set in the step S4, automatic powder spreading scanning and printing of parts are started, when manufacturing of one layer is completed, the workbench is lowered by one powder spreading layer thickness, the scraper flattens the nickel-titanium-copper alloy powder again, manufacturing of the next layer is performed, the circulation is continuously carried out until the printing of the whole part is completed, if severe warping occurs, the printing of the corresponding process is stopped, in the printing process, argon is introduced into the forming chamber, the content of oxygen is reduced to be below 300ppm, the air pressure is kept to be 10-20mbar, convection air blowing is kept in the forming chamber, the air speed of an air outlet is changed according to the quantity of residues, and impurity residues are removed;
and after printing is finished, stopping heating the substrate, reducing the pressure in the forming chamber when the temperature of the substrate is reduced to below 70 ℃, removing residual powder, taking down the substrate with the printed piece, placing the substrate and the printed piece in a vacuum furnace or a 200 ℃ furnace filled with inert gas for heat preservation for 2h, performing stress relief annealing, then performing air cooling to room temperature, cutting the printed piece from the substrate by utilizing wire cutting, treating the surface of the part by using an automatic grinding machine, and grinding oxide skin formed by wire cutting to obtain the nickel-titanium-copper alloy part.
10. The method for preparing the crack-free nickel-titanium-copper alloy for additive manufacturing according to claim 9, wherein the crack-free nickel-titanium-copper alloy for additive manufacturing comprises the following steps: the nickel-titanium-copper alloy powder comprises the following components in percentage by mass: nickel-45.04 wt.%, copper-10.01 wt.%, silicon-0.10 wt.%, oxygen-0.054 wt.%, aluminum-0.10 wt.%, iron-0.04 wt.%, chromium-0.05 wt.%, cobalt-0.008 wt.%, molybdenum-0.04 wt.%, zirconium-0.02 wt.%, unspecified further elements, each of ≦ 0.02 wt.%, total ≦ 0.10 wt.%, the balance titanium.
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