CN107761018B - Preparation method of TiNi shape memory alloy wire reinforced magnesium alloy composite material - Google Patents
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Abstract
The invention relates to a preparation method of a TiNi shape memory alloy wire reinforced magnesium alloy composite material, belonging to the technical field of metal matrix composite material preparation. The method comprises the following steps: firstly forming a composite material prefabricated part by the magnesium alloy plate and the TiNi shape memory alloy wire, and carrying out vacuum hot pressing to obtain a complex; and (3) carrying out deformation treatment on the composite to obtain the TiNi shape memory alloy wire reinforced magnesium alloy composite material. After the composite is deformed at low temperature, the temperature is raised to be higher than the martensite reverse phase transformation temperature, the TiNi shape memory alloy wire in the obtained TiNi shape memory alloy wire reinforced magnesium alloy composite generates martensite reverse phase transformation and recovers the original shape, and the shape of the TiNi shape memory alloy wire in the TiNi shape memory alloy wire reinforced magnesium alloy composite is difficult to recover due to the constraint of the matrix magnesium alloy, so that the pressure stress is generated in the composite, and the self-reinforcing effect of the composite is realized.
Description
Technical Field
The invention relates to a preparation method of a TiNi shape memory alloy wire reinforced magnesium alloy composite material, belonging to the technical field of metal matrix composite material preparation.
Background
The magnesium alloy is the lightest known metal structure material at present, has the advantages of high specific strength, high specific rigidity, good shock absorption performance and the like, and has good cutting processing performance and easy recycling environmental protection performance, and the magnesium alloy have wide application prospects in a plurality of fields of electronics, traffic, communication, aerospace, national defense and the like. However, when the magnesium alloy is used as a structural material, the high-temperature mechanical property, the wear resistance and the hardness of the magnesium alloy are still not ideal enough, so that the application of the magnesium alloy is greatly limited.
The preparation of the magnesium alloy composite material by adding the reinforcing phase into the magnesium alloy is an effective way for improving the mechanical property of the magnesium alloy and is one of the hot spots in the research field of the magnesium alloy. The TiNi shape memory alloy is widely concerned due to the unique characteristics of shape memory effect, super elasticity, large recovery stress when phase change occurs, stable performance and the like, and becomes an important component for preparing composite materials. At present, the room temperature mechanical property of the TiNi shape memory alloy wire reinforced magnesium-lithium alloy composite material prepared by a vacuum hot pressing method is not obviously improved compared with that of a base material; the room temperature mechanical property of the TiNi shape memory alloy wire reinforced magnesium alloy composite material prepared by the other pulse energization hot pressing method (PCHP) is not obviously improved, and the investment cost of the pulse energization hot pressing method is higher.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a TiNi shape memory alloy wire reinforced magnesium alloy composite material, and the TiNi shape memory alloy wire reinforced magnesium alloy composite material prepared by the method realizes a self-reinforcing effect.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a TiNi shape memory alloy wire reinforced magnesium alloy composite material comprises the following steps:
(1) forming a composite material prefabricated part: laying a layer of clean TiNi shape memory alloy wires between every two clean magnesium alloy plates, and fixing to form a composite material prefabricated part;
(2) vacuum hot pressing: putting the composite material prefabricated part into a mold, putting the mold into vacuum hot-pressing equipment, vacuumizing to below 2Pa, and introducing protective gas; heating and pressurizing, raising the temperature to 500-600 ℃, raising the pressure to more than 10MPa, keeping the temperature and the pressure for 3-4 h, releasing the pressure, and cooling along with the furnace to obtain a complex;
(3) deformation treatment: and cooling the composite body to be below the martensite phase transformation temperature of the TiNi shape memory alloy wire, carrying out deformation treatment on the composite body, and heating the deformed composite body to be above the martensite inverse phase transformation temperature of the TiNi shape memory alloy wire to obtain the TiNi shape memory alloy wire reinforced magnesium alloy composite material.
Preferably, the TiNi shape memory alloy wire is an alloy in an austenite state at normal temperature.
Preferably, the mold is a graphite mold or a 45 steel mold.
Preferably, the protective gas is argon or helium.
Preferably, the deformation process is stretching, pressing, bending or twisting.
Advantageous effects
(1) Preparing a TiNi shape memory alloy wire reinforced magnesium alloy composite material by using a vacuum hot pressing method, softening a base body and a reinforcing body in the heating and heat preservation processes, and performing element diffusion on the magnesium alloy base body and the TiNi shape memory alloy wire at an interface joint under the action of pressure to form metallurgical bonding; the vacuum hot pressing method can reduce the requirements on experimental equipment and the process complexity, and effectively reduce the experimental cost.
(2) And (2) carrying out deformation treatment on the composite under a low-temperature condition, unloading and heating to a temperature above the martensite reverse phase transformation temperature, wherein the TiNi shape memory alloy wire in the obtained TiNi shape memory alloy wire reinforced magnesium alloy composite has martensite reverse phase transformation and recovers the original shape, and the shape of the TiNi shape memory alloy wire in the TiNi shape memory alloy wire reinforced magnesium alloy composite is difficult to recover due to the constraint of the matrix magnesium alloy, so that the compressive stress is generated in the composite, and the composite realizes a self-reinforcing effect.
(3) The TiNi shape memory alloy wire in an austenite state at room temperature is used as a reinforcement, and the characteristic that the TiNi shape memory alloy can be spontaneously recovered when the TiNi shape memory alloy is deformed is utilized, after the composite is deformed below the martensite phase transition temperature, the TiNi shape memory alloy wire in the composite is subjected to martensite reverse phase transition by heating, and meanwhile, the TiNi shape memory alloy wire can be recovered to the original shape above the martensite reverse phase transition temperature, and the process is difficult to perform due to the constraint of a magnesium alloy matrix, so that the compressive stress is generated in the composite, and the self-reinforcement of the composite can be realized due to the existence of residual compressive stress.
(4) The volume fraction of the TiNi shape memory alloy wires in the composite material can be adjusted by changing the diameter of the TiNi shape memory alloy wires or changing the interval between the TiNi shape memory alloy wires, so that the mechanical property of the composite material is enhanced.
Drawings
FIG. 1 is a schematic representation of the lay-up of a composite preform of example 1;
FIG. 2 is a Scanning Electron Microscope (SEM) image of a cross section of the TiNi shape memory alloy wire reinforced magnesium alloy composite material prepared in example 1, which is perpendicular to the TiNi shape memory alloy wire;
FIG. 3 is a Scanning Electron Microscope (SEM) image of the interface of the TiNi shape memory alloy wire reinforced magnesium alloy composite prepared in example 1;
FIG. 4 is an enlarged Scanning Electron Microscope (SEM) image of a local area of the interface of the TiNi shape memory alloy wire reinforced magnesium alloy composite prepared in example 1;
FIG. 5 is an X-ray diffraction (XRD) pattern of the TiNi shape memory alloy wire reinforced magnesium alloy composite material prepared in example 1;
FIG. 6 is a Differential Scanning Calorimetry (DSC) graph of the TiNi shape memory alloy wire in the TiNi shape memory alloy wire reinforced magnesium alloy composite material prepared in example 1;
FIG. 7 is a graph of true stress-strain curve of quasi-static tensile of the TiNi shape memory alloy wire-reinforced magnesium alloy composite material prepared in example 1;
FIG. 8 is a graph of quasi-static tensile true stress-strain curve of the TiNi shape memory alloy wire reinforced magnesium alloy composite prepared in example 2;
fig. 9 is a quasi-static tensile true stress-strain curve diagram of the TiNi shape memory alloy wire reinforced magnesium alloy composite material prepared in example 3.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The tests were as follows:
(1) scanning Electron Microscopy (SEM): cutting samples of 5 multiplied by 4mm from the TiNi shape memory alloy wire reinforced magnesium alloy composite material along two directions which are vertical to the TiNi shape memory alloy wire and parallel to the TiNi shape memory alloy wire, polishing, and observing the interface of the TiNi shape memory alloy wire reinforced magnesium alloy composite material by using a HITACHI-S4800 scanning electron microscope.
(2) X-ray diffraction analysis (XRD) method for preparing the Mg-alloy reinforced TiNi-shaped memory alloy wire includes such steps as cutting the TiNi-shaped memory alloy wire into rectangular blocks (10X 3 mm) along the longitudinal cross-section of said wire, polishing, and using CuK α ray source with wavelength (1.5406A), scan rate (6 deg/min) and scan angle (20-120 deg).
(3) Differential scanning thermal test (DSC): cutting a sample which contains the TiNi shape memory alloy wire and has the size of 3 multiplied by 1.5mm from the TiNi shape memory alloy wire reinforced magnesium alloy composite material, polishing the sample until only the TiNi shape memory alloy wire is contained, and then carrying out phase change test, wherein pure argon is adopted for protection during the test, liquid nitrogen is adopted for cooling, the DSC test temperature range is-50 to 100 ℃, and the heating and cooling speed in the test is 10 ℃/min.
(4) Room temperature quasi-static stretching: cutting a tensile sample from the TiNi shape memory alloy wire reinforced magnesium alloy composite material along the direction parallel to the TiNi shape memory alloy wire, wherein the gauge length of the sample is 20mm, the tensile test is carried out on an INSTRON universal testing machine, and the loading strain rate is 10-3s-1。
In the embodiment, the composite material preform is laid in a manner shown in fig. 1, and a layer of TiNi shape memory alloy wire is laid between two magnesium alloy plates.
Example 1
A preparation method of a TiNi shape memory alloy wire reinforced magnesium alloy composite material comprises the following specific steps:
(1) pretreatment: processing two AZ31 plates with the size of 50 multiplied by 3mm by AZ31 magnesium alloy, cutting TiNi shape memory straight wires with the diameter of 1mm into small sections with the size of 55mm, sequentially polishing the surfaces of the AZ31 plates and the TiNi shape memory alloy wires with sand paper of 400#, 600#, 800#, and 1000#, ultrasonically cleaning the plates in absolute ethyl alcohol for 30min, and drying the plates by cold air; storing the TiNi shape memory alloy wires in a clean self-sealing bag, and putting an AZ31 plate into alcohol for storage to prevent oxidation;
(2) forming a composite material prefabricated part: placing an AZ31 plate on a flat and clean table top, paving 50 TiNi shape memory alloy wires densely on the surface of the table top, paving a second AZ31 plate on the paved TiNi shape memory alloy wire layer, finely adjusting the position of the second AZ31 plate to align the second AZ31 plate with the first AZ31 plate, and fixing the second AZ31 plate by using a transparent adhesive tape to obtain a composite material prefabricated part;
(3) vacuum hot pressing: graphite paper is laid on each side within the graphite mold and the composite preform is placed into the mold. Putting the mould into a vacuum hot-pressing furnace chamber, firstly pumping the vacuum degree of the vacuum hot-pressing furnace to be below 2Pa, introducing argon, heating to 600 ℃, boosting the pressure to 12MPa, preserving heat and pressure for 3h, unloading the pressure, and cooling along with the furnace to obtain a complex.
(4) Deformation treatment: and cutting a tensile sample on the composite body along the direction parallel to the TiNi shape memory alloy wires, wherein the tensile sample is divided into a clamping section at two ends, a parallel section in the middle and a fillet transition section between the clamping section and the parallel section, putting the tensile sample into a self-sealing bag filled with purified water, and freezing the tensile sample in a refrigerator (0 ℃). The ice-sealed tensile specimen was quickly mounted on an INSTRON Universal testing machine at 10 ° in a direction parallel to the TiNi shape memory alloy wire-3s-1Applying 1% tensile deformation to the strain rate, taking down the sample, and heating the sample after deformation treatment to room temperature to obtain the TiNi shape memory alloy wire reinforced magnesium alloy composite material.
SEM analysis is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material, and the result is shown in figures 2, 3 and 4, the cross section of the TiNi shape memory alloy wire is still cylindrical as shown in figure 2, which shows that the TiNi shape memory alloy wire is not deformed in the hot pressing process, good interface combination is formed between a magnesium alloy matrix and the TiNi shape memory alloy wire in the composite material as shown in figure 3, no defects such as cracks, holes and the like exist, metallurgical combination is formed between the TiNi shape memory alloy wire and the magnesium alloy matrix as shown in figure 4, and a diffusion layer with the thickness of about 2 mu m exists at the interface.
XRD analysis is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material sample, and the result is shown in figure 5, so that the composite material mainly contains α magnesium and B2 austenite phases, and Ti, Ni precipitated phases and other intermetallic compounds do not appear, which indicates that a magnesium alloy matrix and the TiNi shape memory alloy wire do not have serious reaction in the hot pressing process, and the TiNi shape memory alloy wire does not generate excessive precipitated phases.
The results of DSC analysis of the sample of the TiNi shape memory alloy wire-reinforced magnesium alloy composite material are shown in fig. 6, when B2 transforms from austenite to B19 'martensite, the corresponding martensite transformation starting temperature Ms is 33.7 ℃, the martensite transformation ending temperature Mf is 11.7 ℃, when B19' transforms from martensite to B2 austenite, the martensite reverse transformation starting temperature As is 4.9 ℃, and the martensite reverse transformation ending temperature Af is 37.4 ℃, so that the present experiment applies 1% tensile strain at 0 ℃ to realize the deformation of the TiNi shape memory alloy wire in the martensite state, and the temperature is raised to room temperature (above the martensite reverse transformation temperature) after the deformation, the TiNi shape memory alloy wire generates reverse transformation, generates compressive stress on the magnesium alloy matrix, and realizes the self-reinforcement of the composite material.
The room temperature quasi-static tensile test is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material, and the result is shown in figure 7, and the room temperature tensile strength of the composite material reaches 275 MPa.
Example 2
A preparation method of a TiNi shape memory alloy wire reinforced magnesium alloy composite material comprises the following specific steps:
(1) pretreatment: processing two AZ31 plates with the size of 50 multiplied by 3mm by AZ31 magnesium alloy, cutting a TiNi shape memory alloy straight wire with the diameter of 0.5mm into small sections with the size of 55mm, sequentially polishing the stains and oxidation layers on the surfaces of the AZ31 plate and the TiNi shape memory alloy wire by 400#, 600#, 800# and 1000#, ultrasonically cleaning for 30min in absolute ethyl alcohol, and drying by cold air. Storing the TiNi shape memory alloy wires in a clean self-sealing bag, and putting an AZ31 plate into alcohol for storage to prevent oxidation;
(2) forming a composite material prefabricated part: placing an AZ31 plate on a flat and clean table top, laying 100 prepared TiNi shape memory alloy wires on the surface of the table top one by one in a close-packed manner, laying a second AZ31 plate on the laid TiNi shape memory alloy wires, finely adjusting the position of the second AZ31 plate to align the second AZ31 plate with a first AZ31 plate close to the table top, and fixing the plates by using a transparent adhesive tape to obtain a composite material prefabricated part;
(3) vacuum hot pressing: graphite paper was laid on each side within the graphite mold and the composite preform was placed into the mold. Putting the mould into a vacuum hot-pressing furnace chamber, firstly pumping the vacuum degree of the equipment to be below 2Pa, heating to 550 ℃, boosting the pressure to 12MPa, preserving heat and pressure for 4h, unloading the pressure, and cooling along with the furnace to obtain a complex.
(4) Deformation treatment: and processing the composite into a regular cuboid sample, putting the regular cuboid sample into a self-sealing bag filled with purified water, and freezing in a refrigerator. The composite specimen enclosed in ice was quickly mounted on an INSTRON universal tester, at 10 ° in a direction parallel to the TiNi shape memory alloy wire-3s-1Applying 2% tensile deformation to the strain rate, taking down the sample, and heating the sample after deformation treatment to room temperature to obtain the TiNi shape memory alloy wire reinforced magnesium alloy composite material.
SEM analysis is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material, and the result is similar to that of the embodiment 1, and the interface combination of the TiNi shape memory alloy wire and the magnesium alloy matrix is good.
XRD analysis is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material sample, and the result is similar to that of example 1, the composite material only contains α magnesium and B2 austenite phases, and other precipitated phases do not appear.
DSC analysis is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material sample, and the result is similar to that of the example 1.
Tensile test is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material, the result is shown in figure 8, and the tensile strength of the composite material at room temperature reaches 290 MPa.
Example 3
A preparation method of a TiNi shape memory alloy wire reinforced magnesium alloy composite material comprises the following specific steps:
(1) pretreatment: processing three AZ31 plates with the size of 50 multiplied by 3mm by AZ31 magnesium alloy, cutting TiNi shape memory straight wires with the diameter of 1mm into small sections with the size of 55mm, polishing the surfaces of the AZ31 plates and the TiNi shape memory alloy wires with sand paper of 400#, 600#, 800#, and 1000#, ultrasonically cleaning the plates in absolute ethyl alcohol for 30min, and drying the plates by cold air. Storing the TiNi shape memory alloy wires in a clean self-sealing bag, and putting an AZ31 plate into alcohol for storage to prevent oxidation;
(2) forming a composite material prefabricated part: placing an AZ31 plate on a flat and clean table top, laying 50 prepared TiNi shape memory alloy wires on the surface of the table top one by one in a close-packed manner, laying a second AZ31 plate on the laid TiNi shape memory alloy wires, laying a layer of TiNi shape memory alloy wires on the second AZ31 plate, laying an AZ31 plate on the second AZ31 plate, and fixing the plate by using a transparent adhesive tape to obtain a composite material prefabricated part;
(3) vacuum hot pressing: graphite paper was laid on each side within the graphite mold and the composite preform was placed into the mold. And (3) putting the die into a vacuum hot pressing furnace chamber, pumping the vacuum degree to be below 2Pa, heating to 600 ℃, boosting the pressure to 12MPa, preserving heat and maintaining pressure for 4h, unloading the pressure, and cooling along with the furnace to obtain a complex.
(4) Deformation treatment: and processing the composite into a regular cuboid sample, putting the regular cuboid sample into a self-sealing bag filled with purified water, and freezing in a refrigerator. The composite sample sealed in ice was quickly mounted on an INSTRON universal tester, running parallel to the TiNi shape memory alloy wire at 10-3s-1Applying 2% tensile deformation to the strain rate, taking down the sample, and heating the sample after deformation treatment to room temperature to obtain the TiNi shape memory alloy wire reinforced magnesium alloy composite material.
SEM analysis is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material, and the result is similar to that of the embodiment 1, and the TiNi shape memory alloy wire and the interface of the matrix magnesium alloy are well combined.
XRD analysis is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material sample, and the result is similar to that of example 1, and the composite material contains α magnesium and B2 austenite phases.
DSC analysis is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material sample, and the measured result is similar to that of the example 1.
Tensile test is carried out on the TiNi shape memory alloy wire reinforced magnesium alloy composite material, the result is shown in figure 9, and the tensile strength of the composite material at room temperature reaches 310 MPa.
The invention includes, but is not limited to, the above embodiments, and any equivalent substitutions or partial modifications made under the spirit and principle of the invention are deemed to be within the scope of the invention.
Claims (4)
1. A preparation method of a TiNi shape memory alloy wire reinforced magnesium alloy composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) forming a composite material prefabricated part: laying a layer of clean TiNi shape memory alloy wires between every two clean magnesium alloy plates, and fixing to form a composite material prefabricated part;
(2) vacuum hot pressing: putting the composite material prefabricated part into a mold, putting the mold into vacuum hot-pressing equipment, vacuumizing to below 2Pa, and introducing protective gas; heating and pressurizing, raising the temperature to 500-600 ℃, boosting the pressure to 12MPa, preserving heat and pressure for 3-4 h, releasing pressure, and cooling along with a furnace to obtain a complex;
(3) deformation treatment: cooling the composite body to below the martensitic transformation temperature of the TiNi shape memory alloy wire, carrying out deformation treatment on the composite body, wherein the strain capacity is 1% or 2%, and heating the deformed composite body to above the martensitic reverse transformation temperature of the TiNi shape memory alloy wire to obtain a TiNi shape memory alloy wire reinforced magnesium alloy composite material;
wherein, the TiNi shape memory alloy wire is an alloy in an austenite state at normal temperature.
2. The method for preparing the TiNi shape memory alloy wire reinforced magnesium alloy composite material of claim 1, wherein the method comprises the following steps: the mould is a graphite mould or a 45 steel mould.
3. The method for preparing the TiNi shape memory alloy wire reinforced magnesium alloy composite material of claim 1, wherein the method comprises the following steps: the protective gas is argon or helium.
4. The method for preparing the TiNi shape memory alloy wire reinforced magnesium alloy composite material of claim 1, wherein the method comprises the following steps: the deformation process is stretching, squeezing, bending or twisting.
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