CN114101703A - 4D printing optimization method of TiZrNb high-temperature shape memory alloy based on selective laser melting - Google Patents
4D printing optimization method of TiZrNb high-temperature shape memory alloy based on selective laser melting Download PDFInfo
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Abstract
The invention discloses a 4D printing optimization method of TiZrNb high-temperature shape memory alloy based on selective laser melting, and relates to the technical field of additive manufacturing. The prealloying powder of the TiZrNb high-temperature shape memory alloy with the expected components is prepared by rotary electrode atomization; carrying out selective laser melting block forming on the powder of the high-temperature shape memory alloy, and then carrying out density analysis to obtain an optimal process parameter interval; performing shape memory performance analysis and mechanical performance analysis on the parameters in the optimal process parameter interval; the metallographic analysis and the microscopic morphology analysis are assisted to the experiment; and (4) obtaining optimal process parameters by integrating mechanical property analysis, shape memory property analysis and micro-morphology analysis. The invention realizes the high phase transition temperature and excellent shape memory performance of the 4D printing material, the maximum austenite forming temperature can reach more than 700K, the microhardness can reach 3.8GPa, and the shape memory recovery rate can reach 43 percent at most.
Description
Technical Field
The invention belongs to the technical field of additive manufacturing, and particularly relates to a 4D printing optimization method of TiZrNb high-temperature shape memory alloy based on selective laser melting.
Background
The additive manufacturing technology (commonly known as 3D printing technology) is a technology which is developed in the last thirty years and decomposes materials into layer-by-layer data based on digital model design software to realize the accumulative manufacturing of solid parts, has the advantages of high forming speed, short production period, high material utilization rate, good material adaptability, no need of drawings and tooling equipment, high digitization degree and the like, and is widely applied to the fields of mechanical manufacturing, aerospace, biomedical treatment and the like. With the gradual change of the center of gravity of high-end equipment in the intelligent development to the intelligent characteristic requirement, the 4D printing technology realizes the controllable change of the shape, the performance or the function along with the time by manufacturing a special component through the 3D printing technology, and is an effective means for realizing the manufacture of complex intelligent components or intelligent materials.
The shape memory alloy can automatically recover the shape before deformation after the temperature reaches the austenite transformation temperature after the phase transformation is carried out in the low-temperature martensite form through the crystallography corresponding relation between the austenite phase and the martensite phase, and is an intelligent material with wide application. The shape memory alloy which is most widely applied at present is the nickel titanium shape memory alloy with the approximate equal atomic ratio. However, the low martensitic transformation temperature (generally lower than 373K) and the poor machinability of NiTi shape memory alloys greatly limit their further applications. To cope with high temperature fields such as an aircraft engine tail nozzle, the concept of a high temperature shape memory alloy has been proposed and studied. At present, high-temperature shape memory alloys such as Cu-based NiTi-X (X ═ Hf, Zr), CoNiGa, NiMnGa and the like can realize shape memory phase transformation in a high-temperature environment higher than 373K, but all have various defects which are difficult to overcome, such as poor machinability, high price, difficult molding and the like, and limit the development and application of the alloys.
Ti-based high-temperature shape memory alloys have the advantages of excellent cold and hot processability, stable high phase transition temperature and low cost, and are widely concerned in the field of high-temperature shape memory, and novel Ti-based shape memory alloys comprising Ti-Zr base, Ti-Nb base, Ti-Ta base and Ti-Mo base are researched in the field of casting metallurgy. At present, the phase transition temperature of the Ti-Zr binary shape memory alloy can reach more than 800K at room temperature, and the phase transition behavior can be regulated and controlled by further adding third and fourth elements such as Nb, Fe, Ta, Al, B and the like, so that the martensite phase transition temperature and the shape memory effect are coordinated.
Disclosure of Invention
In view of the above, the invention aims to provide a method for optimizing a 4D printing preparation process based on selective laser melting of TiZrNb high-temperature shape memory alloy, which obtains an optimal process parameter interval through density analysis, and obtains an optimal process parameter by combining mechanical property analysis and shape memory property analysis and micro-morphology analysis.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention discloses a 4D printing preparation process optimization method based on selective laser melting of TiZrNb high-temperature shape memory alloy, which is realized by the following technical scheme:
the method comprises the following steps: prealloying powder of TiZrNb high-temperature shape memory alloy with expected components is prepared by rotary electrode atomization.
Step two: and carrying out selective laser melting block forming on the powder of the high-temperature shape memory alloy, and then carrying out density analysis to obtain an optimal process parameter interval.
Step three: and (4) carrying out shape memory performance analysis and mechanical property analysis on the parameters in the optimal process parameter interval.
Step four: the above experiments were supplemented with metallographic analysis and microscopic morphology analysis.
Step five: and (4) obtaining optimal process parameters by integrating mechanical property analysis, shape memory property analysis and micro-morphology analysis.
In the technical scheme, in the step one, the nominal atomic ratio of the TiZrNb high-temperature shape memory alloy powder is 7:2: 1.
In the above technical solution, in the step one, the form of the TiZrNb high temperature shape memory alloy powder is pre-alloyed powder.
In the technical scheme, in the step one, the density analysis adopts an ST-100E full-automatic electronic densimeter, and the sample has high density in a process optimization interval of 35-300J/mm 3.
In the above technical solution, in the second step, the selective laser melting adopts RENISHAW-AM400 laser selective melting rapid prototyping equipment, and three variable parameters of the dot pitch, the exposure time, and the laser power are selected as orthogonal test factors to perform an experiment to prepare a sample.
In the technical scheme, in the third step, the mechanical property test adopts a Hysitron TI-Premier nanoindenter, the microhardness of the TiZrNb high-temperature shape memory alloy can reach 3.86GPa at most, and the modulus can reach 67.1GPa at most.
In the above technical solution, in the third step, the phase transition temperature test in the shape memory performance test adopts an STA449f3 comprehensive thermal analyzer, and the martensite phase transition temperature of the TiZrNb high temperature shape memory alloy can reach 707K.
In the above technical solution, in the third step, the shape memory recovery rate in the shape memory performance test is subjected to a nanoindentation point depth test before and after high temperature recovery by using a Dimension Icon atomic force microscope, and the shape memory recovery rate of the TiZrNb high temperature shape memory alloy can reach 25.1%.
In the technical scheme, in the third step, the shape memory recovery rate parameter in the electrochemical experiment parameters for testing the shape memory performance is the austenite transformation completion temperature plus 10 ℃, and the heat preservation time is 3 minutes.
Has the advantages that: TiZrNb is a shape memory alloy with high phase transition temperature, and is currently studied in the field of selective laser melting. Although density analysis is performed by using laser energy density as a parameter as a process optimization analysis method commonly used in the field of selective laser melting, the method has many advantages, and partial defects still exist when process optimization is actually performed. On the one hand, there are many parameters at the same energy density, and the properties of the samples manufactured by these parameters still have significant differences. On the other hand, under the condition of high density, the material has a larger laser energy density forming interval, and further scientific and reasonable process optimization is difficult to perform. The method determines the optimal process parameter interval by taking the laser energy density as the basic reference quantity, and then determines the optimal process parameter by combining mechanical property analysis and micro-morphology analysis. The Ti-20Zr-10Nb forming in a large laser energy density interval is successfully realized, the maximum austenite forming temperature can reach above 700K, the microhardness reaches 3.8GPa, and the shape memory recovery rate can reach 43% to the maximum. By the method, 4D printing manufacturing of the high-temperature shape memory alloy with high phase transition temperature and excellent shape memory performance based on the selective laser melting process is successfully realized, and the method has important significance.
Drawings
FIG. 1 is a diagram of a Ti-20Zr-10Nb high temperature shape memory alloy obtained by selective laser melting;
FIG. 2 is a fitting curve of sample density and laser energy density obtained by block molding;
FIG. 3 is a room temperature nanoindentation load depth curve (left) and a trend (right) of room temperature hardness and modulus with laser energy density of the Ti-20Zr-10Nb high-temperature shape memory alloy;
FIG. 4 is a DSC curve of Ti-20Zr-10Nb high temperature shape memory alloys of different laser energy densities;
FIG. 5 is a graph of the shape memory recovery of Ti-20Zr-10Nb high temperature shape memory alloys at different laser energy densities;
FIG. 6 is an SEM microstructure of samples of parts at different laser energy densities, wherein (a) No. 1; (b) the method comprises the following steps Number 2; (c) the method comprises the following steps Number 3; (d) the method comprises the following steps Number 4; (e) no. 5;
FIG. 7 is a TEM microstructure of samples of various parts at different laser energy densities, wherein (a): a TEM image and a SEAD image of the structure of the mother phase and the precipitated phase; (b) the method comprises the following steps A dark field image of the omega phase; (c) the method comprises the following steps A precipitated phase inside the crystal grains; (d) the method comprises the following steps Grain boundary precipitated phase of sample No. 2; (e) the method comprises the following steps The grain boundary precipitated phase of sample No. 5.
Detailed Description
Example 1
Atomizing by a rotary electrode to obtain Ti-20Zr-10Nb high-temperature shape memory alloy prealloying powder; then, performing selective laser melting block forming on the original powder, and then performing density analysis to obtain an optimal process parameter interval; molding sample pieces with different performances according to parameters in the optimal process parameter interval, and analyzing mechanical properties and shape memory properties; analyzing the micro-morphology of the experiment; obtaining optimal process parameters by comprehensive mechanical property analysis, shape memory property analysis and micro-morphology analysis
First, selective laser ablation
And collecting the mixed powder in a powder cylinder, cleaning the substrate, blasting sand, removing a surface oxide layer, and then installing, and finally finishing the replacement and installation of the scraper. Opening the air extractor, filling argon to protect, ensuring the oxygen content in the equipment to be below 100ppm, and preheating the TC4 substrate to 130 ℃. Completion of 5 x 5mm using QuantAM software3Building a cube model and setting process parameters, importing model data into equipment, and automatically starting sample manufacturing by the equipment system after preparation conditions are ready. Three variable parameters of laser line spacing, exposure time and laser power are selected as orthogonal test factors in the experiment, and the experiment is carried out to prepare the sample. And selecting parameters in the optimal process parameter interval obtained after the density analysis, and repeatedly printing a mechanical property sample and a shape memory property sample used in a subsequent experiment.
Second, density analysis
Putting the sample after wire cutting into absolute ethyl alcohol, cleaning and removing impurities adhered to the surface, drying, putting the sample on a measuring table, weighing, recording data by pressing a key after the number is stable, then weighing the sample in a hanging basket in a water tank, and directly obtaining a result and recording data by pressing the key after the number is stable. Each sample is guaranteed at least three measurements, averaged to reduce errors
Third, mechanical property test
And selecting the formed block as a nano indentation test sample, and directly polishing and washing the sample with alcohol until the surface of the sample has no scratch. Room temperature nanoindentation test is carried out by adopting a Hysitron TI-Premier nanoindentor, and microhardness and modulus of Ti-20Zr-10Nb high-temperature shape memory alloy with different laser energy densities prepared in an optimal SLM process parameter interval are researched. The loading load is 10 mN, the loading time is 10s, the load-holding time is 10s, the unloading time is 10s, and in order to keep the accuracy of data and facilitate the next shape memory performance test, the average value of four points with the square shape measuring interval of 1mm is taken for each sample.
Shape memory performance test
The method comprises the following two aspects: phase transition temperature test and shape memory recovery test
Phase transition temperature testing the heat absorption and heat release behaviors of the samples during slow temperature rise and fall were characterized using a STA449f3 comprehensive thermal analyzer. Taking the size of 1.5X 1.5mm3The test sample is placed in a special crucible for an instrument to be tested, the test atmosphere is an argon environment, the temperature of the sample is slowly increased from 100 ℃ to 700 ℃ and then is decreased to 100 ℃, and the temperature increasing rate and the temperature decreasing rate are both 10 ℃/min.
In the shape memory recovery rate test, a Dimension Icon atomic force microscope is used for scanning indentation points after the nano indentation test to obtain indentation depth information before high-temperature recovery; then, carrying out high-temperature recovery on the sample in an atmosphere furnace, wherein the selected shape memory recovery temperature is the austenite transformation completion temperature plus 10 ℃, the heat preservation time is 3 minutes, and the whole process is protected in an argon atmosphere; and after high-temperature recovery, carrying out atomic force microscope scanning on the indentation point to obtain indentation depth information after high-temperature recovery. The shape memory recovery of the sample was calculated by the following formula:
wherein R is the shape memory recovery rate, Da is the indentation depth after high temperature recovery, and Db is the indentation depth before high temperature recovery.
Fourth, micro-topography determination
And (3) obtaining the phase composition and the micro morphology of the selected area laser melting block under different laser energy densities under an X-ray diffractometer, a scanning electron microscope and a projection electron microscope.
Fifth, analysis of experimental results
As can be seen visually from FIG. 2, as the laser energy density increases, the density increases rapidly and then becomes stable, and the laser energy density is 75J/mm3When the density is lower than the reference density, the density is greatly influenced by the laser energy density, and the density of the sample is rapidly increased along with the increase of the laser energy density; then, along with the increase of the laser energy density, the density of the sample is firstly reduced and then fluctuates in a certain range, and the influence of the laser energy density is small; the sample can reach a higher density level within a wide range of laser energy density intervals. The Ti-20Zr-10Nb high-temperature shape memory alloy has wide forming process range and needs higher-level process optimization analysis.
Selecting 35-300J/mm3The next analysis was performed on 5 samples of different energy density levels within the excellent process optimization interval. As can be seen from FIG. 3, when the phase composition of Ti-20Zr-10Nb high temperature shape memory alloys prepared at different SLM laser energy densities was analyzed, the main phase of all samples was the beta phase, and as the laser energy density increased, the alpha 'and omega phases were gradually generated, but when the energy density reached the highest, the alpha' and omega phases were inversely suppressed. Because of the very low content of alpha "and omega phases, the XRD data lacks further persuasion and further analysis of the microscopic morphology of the sample is required.
As can be seen from fig. 4, the load-displacement curves for the samples of different laser energy densities are similar in general shape and level, all having a higher level of microhardness, the highest microhardness level occurring in sample No. 1, up to 3.6GPa, and the lowest hardness of sample No. 2. Similar regularity in the modulus distribution was observed in addition to sample No. 5, which exhibited high microhardness and modulus at low energy density. Neglecting the extremely high energy density, the hardness and modulus of Ti-20Zr-10Nb high temperature shape memory alloy show a negative correlation with the laser energy density. The samples No. 3 and No. 4 have relatively excellent microhardness and modulus.
From FIG. 5, the DSC curve shapes of the Ti-20Zr-10Nb samples with different laser energy densities are similar, which shows that all the samples maintain the same phase transformation process during the temperature rising and lowering processes. Two endothermic peaks appear in the temperature rise curve, the first peak representing the precipitation of the ω phase, and the second peak representing the reverse transformation of α "martensite to β phase in the conventional martensitic transformation, the temperature of which represents the martensitic transformation temperature. No exothermic peak occurs during cooling due to the partial transformation of the beta phase to the alpha "martensite phase or the low enthalpy of the martensite phase transformation. Aiming at the relation between the martensite transformation characteristic temperature and the laser energy density, no obvious dependence is generated; on the other hand, the highest martensitic transformation characteristic temperature appears in sample No. 5, and the temperature exceeds 707K, and the lowest martensitic transformation temperature reaches 700K, which is far more than 373K specified for high-temperature shape memory alloys.
From FIG. 6, the AFM scanning depth of the Ti-20Zr-10Nb samples with different laser energy densities after high temperature recovery is obviously reduced, which shows that the samples generate obvious shape memory recovery effect after being heated to the phase transition temperature. The specific AFM scanning depth change data before and after high-temperature recovery and the shape memory recovery rate obtained by calculation are shown in FIG. 6, the shape memory recovery rates under different laser energy densities are between 16.9% and 25.1%, and are approximately in a similar level, so that the shape memory effect is obvious, and the shape memory effects of the samples No. 3 and No. 4 are excellent.
As can be seen in FIG. 7, the SEM images of the high temperature shape memory alloy samples with different laser energy densities of Ti-20Zr-10Nb are shown in the figure. Although the laser energy density of the formed samples is different, the microstructure of the prepared samples is composed of columnar crystals, the austenite crystal boundary is clear, and no obvious defect exists in the forming process. In the austenite grain boundary, a large number of nano-scale precipitated phases are observed, and the precipitated phases are granular in the intragranular morphology and are connected with each other at the grain boundary and are closely distributed on the grain boundary. The cause of substructure generation within the grains is the effect of corrosion because these structures cross the grain boundaries. The TEM morphology proves the analysis result of XRD, the main phase is beta phase, the dispersed and distributed fine omega phase in the matrix phase can be observed through the dark field image, the density of the precipitated phase in the sample gradually rises along with the rise of the laser energy density, the precipitated phase on the grain boundary gradually grows, the grain boundary is seriously coarsened, and the sample with low energy density is selected for reducing the influence of the precipitated phase.
The Ti-20Zr-10Nb high-temperature shape memory alloy has wide forming process range, and can realize high-density printing in the process optimization range of 35-300J/mm 3. In the interval, 5 samples with different energy density levels are selected to carry out mechanical property tests and shape memory property tests, and the microhardness and the shape memory effect of the No. 3 sample and the No. 4 sample are determined by combining microscopic analysis. On the basis, the sample No. 3 has more excellent martensitic transformation temperature, the optimal 4D printing laser energy density of the Ti-20Zr-10Nb high-temperature shape memory alloy under the experimental condition is determined to be about 150J/mm3, and the sample printed under the experimental condition has high transformation temperature, high shape memory effect and excellent mechanical property.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. An optimization method of a 4D printing preparation process of TiZrNb high-temperature shape memory alloy based on selective laser melting is characterized by comprising the following steps:
the method comprises the following steps: preparing prealloying powder of TiZrNb high-temperature shape memory alloy with expected components by rotary electrode atomization;
step two: carrying out selective laser melting block forming on the pre-alloyed powder, and then carrying out density analysis to obtain an optimal process parameter interval;
step three: and performing shape memory performance analysis, mechanical performance analysis, metallographic analysis and micro-morphology analysis on the parameters in the optimal process parameter interval, and performing comprehensive mechanical performance analysis, shape memory performance analysis and micro-morphology analysis to obtain optimal process parameters.
2. The optimization method according to claim 1, characterized in that: in the first step, the nominal atomic ratio of the TiZrNb high temperature shape memory alloy is 7:2: 1.
3. the optimization method according to claim 1, characterized in that: in the second step, the density analysis adopts an ST-100E full-automatic electronic densitometer, and the density is 35-300J/mm3The process optimization interval of (2) has a high density of samples.
4. The optimization method according to claim 1, characterized in that: in the second step, the selective laser melting adopts a RENISHAW-AM400 laser selective melting rapid prototyping device.
5. The optimization method according to claim 4, wherein when the selected area laser melting is performed by using a RENISHAW-AM400 laser selected area melting rapid prototyping device, three variable parameters of point distance, exposure time and laser power are selected as orthogonal test factors to perform experimental preparation of a sample.
6. The optimization method according to claim 1, characterized in that: in the third step, the mechanical property test adopts a Hysitron TI-Premier nanoindenter.
7. The optimization method according to claim 1, characterized in that: in step three, the phase transition temperature test in the shape memory performance test adopts an STA449f3 comprehensive thermal analyzer.
8. The optimization method according to claim 1, characterized in that: in the third step, the shape memory recovery rate in the shape memory performance test adopts a Dimension Icon atomic force microscope to perform the depth test of the nano indentation point before and after high-temperature recovery.
9. The optimization method according to claim 1, characterized in that: in the third step, the shape memory recovery rate parameter in the electrochemical experiment parameters of the shape memory performance test is the austenite transformation completion temperature plus 10 ℃, and the heat preservation time is 3 minutes.
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