CN114622110B - Preparation method of titanium-nickel alloy-based composite material with wide temperature range and high damping response - Google Patents

Preparation method of titanium-nickel alloy-based composite material with wide temperature range and high damping response Download PDF

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CN114622110B
CN114622110B CN202210263875.5A CN202210263875A CN114622110B CN 114622110 B CN114622110 B CN 114622110B CN 202210263875 A CN202210263875 A CN 202210263875A CN 114622110 B CN114622110 B CN 114622110B
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titanium
nickel alloy
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CN114622110A (en
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李响
常国
霍望图
董龙龙
李亮
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Northwest Institute for Non Ferrous Metal Research
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0008—Electrical discharge treatment, e.g. corona, plasma treatment; wave energy or particle radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/162—Cleaning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/16—Drying; Softening; Cleaning
    • B32B38/164—Drying
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
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    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00—Electrophoretic coating characterised by the process
    • C25D13/02—Electrophoretic coating characterised by the process with inorganic material
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00—Electrophoretic coating characterised by the process
    • C25D13/22—Servicing or operating apparatus or multistep processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B2038/0052—Other operations not otherwise provided for
    • B32B2038/0064—Smoothing, polishing, making a glossy surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/56—Damping, energy absorption

Abstract

The invention discloses a preparation method of a titanium-nickel alloy based composite material with wide temperature range and high damping response, which comprises the following steps: 1. cutting the titanium-nickel foil into slices and then pretreating to obtain a pretreated titanium-nickel foil; 2. dispersing graphene oxide into absolute ethyl alcohol, and adding aluminum nitrate to obtain electrophoretic deposition liquid; 3. placing the pretreated titanium-nickel foil in an electrophoretic deposition solution for deposition to obtain a titanium-nickel alloy deposited foil; 4. and stacking the titanium-nickel alloy deposition foil and sintering to obtain the titanium-nickel alloy based composite material. According to the invention, graphene oxide is introduced into the titanium-nickel alloy layer by layer to form a multi-scale hierarchical structure, the intrinsic multilayer structure of the graphene oxide is kept by controlling the interface reaction condition, and the titanium-nickel alloy-based composite material has the hybrid enhancement function of multiple damping enhancement mechanisms such as intrinsic damping, phase change damping and interface damping, so that the damping response of the titanium-nickel alloy-based composite material in a wide temperature range is improved, and the service condition is widened.

Description

Preparation method of titanium-nickel alloy-based composite material with wide temperature range and high damping response
Technical Field
The invention belongs to the technical field of design and preparation of damping materials, and particularly relates to a preparation method of a titanium-nickel alloy-based composite material with wide temperature range and high damping response.
Background
In recent years, with the change of science and technology, the development of aviation and aerospace technology is becoming a hard index for measuring the scientific and technological strength of the large country. The design and research and development of novel high-performance aerospace materials have become important pushers for promoting the aerospace technology. In the past, the research and development of aviation and aerospace materials mostly pursue to improve the strength. However, as aerospace metal, it is far from insufficient to seek high mechanical properties, and a spacecraft can generate serious broadband random vibration and noise environment due to engine operation, aerodynamic noise and the like in the flying process, so that the structure is fatigue-ineffective and dynamic unstable, and the working accuracy and reliability of equipment are seriously influenced. Therefore, aerospace materials are also important for damping performance, i.e., vibration damping and isolation characteristics.
Among numerous metal damping materials, titanium-nickel alloys have been widely used in aerospace devices, biomedicine and mechatronics due to their unique shape memory effect, superelasticity, high damping properties and excellent strong plastic matching. However, as a damping material, there is also a limit to the use of titanium-nickel alloys over a wide temperature range. The reason for this is that the titanium-nickel alloy is a twin crystal type damping alloy, and the structure thereof at low temperature is a B19' martensite phase of a monoclinic structure, and when the temperature is higher than the martensite reverse transformation start temperature, the martensite phase is transformed into a B2 austenite phase of a body-centered cubic structure. The austenite phase in the titanium-nickel alloy has low intrinsic damping performance due to the lack of energy consumption of interface motion between variants and low dislocation density. The use temperature environment of the aerospace material is complex, and how to enable the titanium-nickel alloy to realize high damping response in a wide temperature range is still the key point of the design of the current damping material.
Graphene oxide is a natural layered material composed of stacked graphene, the distance between layers is 0.34nm, and the graphene oxide and graphene oxide are connected with each other by weak van der waals force, so that the layers are easy to slip and absorb vibration energy under the action of alternating load. In addition, d.lahiri (ACS Nano (2012) 3992-4000) and y.j.su (CARBON 50 (2012) 2804-2809) also find in research that the damping performance of graphene improves with the increase of the number of layers, and has more excellent damping characteristics at higher temperatures, which provides a basis for the feasibility of graphene oxide as a multilayer interface damping mechanism reinforcing phase. However, the improvement of the damping performance of the titanium-nickel alloy by utilizing the graphene oxide multi-scale hierarchical structure is not reported.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a titanium-nickel alloy based composite material with wide temperature range and high damping response aiming at the defects of the prior art. According to the method, graphene oxide is introduced into the titanium-nickel alloy in a layered manner, a multi-scale hierarchical structure is formed in the titanium-nickel alloy base composite material, the intrinsic multilayer structure of the graphene oxide is reserved to the greatest extent by controlling interface reaction conditions, and the titanium-nickel alloy base composite material has hybrid enhancement effects of multiple damping enhancement mechanisms such as intrinsic damping, phase change damping and interface damping, so that the damping response of the titanium-nickel alloy base composite material in a wide temperature range is greatly improved, and the service conditions of the titanium-nickel alloy base composite material are fully expanded.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of a titanium-nickel alloy based composite material with wide temperature range and high damping response is characterized by comprising the following steps:
step one, pretreatment of a titanium-nickel foil: cutting the titanium-nickel foil into slices by adopting linear cutting, sequentially polishing the surfaces of the slices by adopting 500-mesh, 1000-mesh and 1500-mesh metallographic abrasive paper, sequentially pickling in an acid solution, washing in deionized water, neutralizing the residual pickling solution, ultrasonically cleaning by adopting absolute ethyl alcohol, and drying to obtain the pretreated titanium-nickel foil;
step two, preparing electrophoretic deposition liquid: adding graphene oxide into absolute ethyl alcohol for ultrasonic dispersion to obtain a stable graphene oxide/absolute ethyl alcohol turbid liquid, then adding aluminum nitrate particles into the graphene oxide/absolute ethyl alcohol turbid liquid, and uniformly stirring to obtain an electrophoretic deposition liquid;
step three, preparing the titanium-nickel alloy deposition foil: placing the pretreated titanium-nickel foil obtained in the step one in the electrophoretic deposition solution obtained in the step two for deposition, and depositing a graphene oxide layer on the surface of the pretreated titanium-nickel foil to obtain a titanium-nickel alloy deposition foil;
step four, preparing the titanium-nickel alloy based composite material: the titanium-nickel alloy deposited foil obtained in the third step is tiled and stacked layer by layer along the same direction of the graphene oxide layers, the pretreated titanium-nickel foil obtained in the first step is tiled and stacked on the outermost graphene oxide layer to obtain a laminated foil, and then the laminated foil is placed in a graphite mold to be subjected to discharge plasma sintering to obtain a titanium-nickel alloy-based composite material; the damping factors of the titanium-nickel alloy based composite material at-20 ℃, 25 ℃ and 200 ℃ respectively reach 0.089, 0.128 and 0.034.
The design of the existing damping material emphasizes on improving the damping performance at a specific temperature by using a certain mechanism in the reinforcing phase intrinsic damping or the structural damping, so that the high damping response in a wide temperature range is difficult to realize. In order to make up for the defects, firstly, the method of electrophoretic deposition is adopted to uniformly deposit graphene oxide on the surface of the pretreated titanium-nickel foil to obtain a titanium-nickel alloy deposited foil, then the titanium-nickel alloy deposited foil is tiled and stacked layer by layer along the same direction of the graphene oxide layer, and the pretreated titanium-nickel foil is tiled and stacked on the graphene oxide layer at the outermost layer to obtain a laminated foil, so that the bottom layer and the top layer of the laminated foil are both the titanium-nickel foil, and the titanium-nickel alloy-based composite material is obtained after sintering. According to the invention, graphene oxide is introduced into the titanium-nickel alloy layer by layer, the intrinsic multilayer structure of the graphene oxide is retained to the greatest extent by controlling interface reaction conditions, and under alternating load, the intrinsic multilayer structure of the graphene oxide can slide between layers and absorb vibration energy, so that high damping response of the titanium-nickel alloy based composite material in a wide temperature range is realized; meanwhile, the titanium-nickel alloy-based composite material obtained by the invention has a multi-scale hierarchical structure, namely an atomic hierarchical structure among single-layer carbon atoms in graphene oxide, a nano hierarchical structure among adjacent graphene oxide in a deposition layer and a micron hierarchical structure among adjacent titanium-nickel foil, and the damping performance of the titanium-nickel alloy-based composite material can be further improved by the coordination effect of a multi-scale hierarchical structure interface in the vibration process; therefore, the titanium-nickel alloy-based composite material prepared by the invention has high damping response in a wide temperature range, and the service conditions of the titanium-nickel alloy-based composite material are fully expanded.
The preparation method of the titanium-nickel alloy-based composite material with the wide temperature range and the high damping response is characterized in that in the step one, the titanium-nickel foil has the superelasticity characteristic at room temperature, and the recoverable strain is larger than 6%. The titanium-nickel alloy-based composite material with the superelasticity property is adopted, so that the prepared titanium-nickel alloy-based composite material has excellent damping performance and tensile yield strength at room temperature.
The preparation method of the titanium-nickel alloy based composite material with wide temperature range and high damping response is characterized in that in the step one, the shape of the sheet is rectangular, circular or triangular; the acid solution is prepared from HF and HNO 3 And H 2 O is composed according to the volume ratio of 1; the ultrasonic cleaning time is 5-10 min. The optimized acid solution and the acid washing time can effectively and completely eliminate the oxide film on the surface of the sheet, are beneficial to subsequent sintering combination, and avoid the influence of excessive corrosion of the sheet on the adsorption of the graphene oxide in the electrophoretic deposition process; the preferred ultrasonic cleaning time is sufficient to neutralize the acid solution on the surface of the sheet, which helps to uniformly deposit the graphene oxide. In addition, the shape of the thin sheet can be adjusted according to the requirements of the titanium-nickel alloy based composite material, and the thin sheet can be in the shapes of circles, triangles and the like besides the shapes of rectangles.
The preparation method of the titanium-nickel alloy based composite material with the wide temperature range and the high damping response is characterized in that in the second step, the graphene oxide has the sheet diameter of 1-3 mu m and the thickness of 1-5 nm and has a multilayer structure. The graphene oxide with the sheet diameter and the thickness is preferably adopted, so that the titanium-nickel alloy based composite material contains more movable interfaces under the action of alternating load, and the damping characteristic of the titanium-nickel alloy based composite material is favorably improved.
The preparation method of the titanium-nickel alloy based composite material with the wide temperature range and the high damping response is characterized in that in the second step, the ratio of the mass of the graphene oxide to the volume of the absolute ethyl alcohol in the electrophoretic deposition solution is 0.25-0.75, the unit of the mass is mg, the unit of the volume is mL, and the mass ratio of the graphene oxide to the aluminum nitrate particles is 1. The optimized proportion of the electrophoretic deposition liquid ensures that the graphene oxide is rapidly and uniformly deposited on the surface of the titanium-nickel foil.
The preparation method of the titanium-nickel alloy based composite material with wide temperature range and high damping response is characterized in that in the second step, the ultrasonic dispersion time is 4-6 hours, and the stirring time is more than 10min. The optimized ultrasonic dispersion time ensures that the graphene oxide is fully dispersed in the absolute ethyl alcohol, is beneficial to uniform deposition of the graphene oxide, avoids the problem of poor bonding effect of the graphene oxide and the titanium-nickel alloy foil due to serious agglomeration of the graphene oxide, and improves the preparation efficiency of the titanium-nickel alloy deposited foil; the above preferred stirring time ensures sufficient dissolution of aluminum nitrate particles, contributes to improving the deposition rate of graphene oxide, and improves the preparation efficiency of the titanium-nickel alloy deposited foil.
The preparation method of the titanium-nickel alloy based composite material with wide temperature range and high damping response is characterized in that the voltage of deposition in the step three is 120V, the current is 0.03A, and the deposition time is 3-5 min.
The preparation method of the titanium-nickel alloy based composite material with wide temperature range and high damping response is characterized in that the sintering temperature of the spark plasma sintering in the fourth step is 700-900 ℃, the sintering pressure is 30MPa, the heat preservation time is 10-20 min, and the vacuum degree is 1Pa. The optimized sintering process parameters ensure that a large number of nano-level structures are still remained after the titanium-nickel alloy based composite material is sintered, and the interface high-damping response in a wide temperature range is favorably realized.
The preparation method of the titanium-nickel alloy based composite material with wide temperature range and high damping response is characterized in that the titanium-nickel alloy based composite material in the fourth step contains 50-220 layers of graphene oxide. The graphene oxide with the layers can ensure that the damping performance of the titanium-nickel alloy based composite material is effectively improved, and the interface bonding quality is not reduced.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, graphene oxide is introduced into the titanium-nickel alloy in a layered manner, a multi-scale hierarchical structure is formed in the titanium-nickel alloy-based composite material, and the titanium-nickel alloy-based composite material has hybrid enhancement effects of multiple damping enhancement mechanisms such as intrinsic damping, phase change damping and interface damping, so that the damping response of the titanium-nickel alloy-based composite material in a wide temperature range is greatly improved, and the service conditions of the titanium-nickel alloy-based composite material are fully broadened.
2. Compared with the traditional blocky damping alloy, the titanium-nickel alloy-based composite material prepared by the invention has a multi-scale hierarchical structure, and the mechanical property of the titanium-nickel alloy-based composite material can be improved through the effects of crack deflection, bridging and the like in the failure process.
3. Compared with the traditional high-molecular damping material, the titanium-nickel alloy-based composite material prepared by the invention takes the metal material as the matrix, has more excellent mechanical property, and can be more suitable for the harsh service environments of low temperature, high pressure and the like of materials for aviation and aerospace.
4. The invention changes the layer number of the graphene oxide layer deposited on the surface of the pretreated titanium-nickel foil by adjusting the process parameters of electrophoretic deposition, effectively adjusts the damping response characteristics of the titanium-nickel alloy-based composite material in different temperature intervals, and prepares the structure-function integrated damping material meeting different service environments by adjusting the size and sintering process parameters of the titanium-nickel foil.
5. The titanium-nickel alloy-based composite material obtained by adopting the metal foil metallurgy method and the one-step sintering molding through the spark plasma sintering technology has high density, does not need subsequent densification treatment, has simple process flow and short preparation time, saves energy consumption and is beneficial to industrial development.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is an SEM image of a titanium-nickel alloy based composite material prepared in example 1 of the present invention.
FIG. 2 is an SEM image of the interface of the Ti-Ni alloy based composite material prepared in example 1 of the present invention.
Fig. 3 is an SEM image of a titanium-nickel alloy laminate prepared in comparative example 1 of the present invention.
Fig. 4 is a graph showing damping performance of the titanium-nickel alloy based composite material prepared in example 1 of the present invention and the titanium-nickel alloy laminate prepared in comparative example 1.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, pretreatment of a titanium nickel foil: cutting the titanium nickel foil into rectangular sheets by adopting linear cutting, sequentially polishing the surfaces of the rectangular sheets by adopting 500-mesh, 1000-mesh and 1500-mesh metallographic abrasive paper, then sequentially putting the rectangular sheets into an acid solution for acid cleaning for 8s, putting the rectangular sheets into deionized water for washing, neutralizing the residual acid cleaning solution, putting the neutralized acid cleaning solution into absolute ethyl alcohol, putting the neutralized acid cleaning solution into an ultrasonic cleaning machine for ultrasonic cleaning for 8min, and drying the neutralized acid cleaning solution to obtain a pretreated titanium nickel foil; the acid solution is prepared from HF and HNO 3 And H 2 The volume ratio of O to the component (1); the titanium nickel foil has super elasticity characteristic at room temperature, and the recoverable strain is more than 6%;
step two, preparing electrophoretic deposition liquid: adding 200mg of graphene oxide with a sheet diameter of 1-3 mu m and a thickness of 1-5 nm and a multilayer structure into a beaker filled with 400mL of absolute ethyl alcohol for ultrasonic dispersion for 6 hours to obtain a stable graphene oxide/absolute ethyl alcohol suspension, and then adding 200mg of aluminum nitrate particles into the graphene oxide/absolute ethyl alcohol suspension to stir uniformly for 10min to obtain an electrophoretic deposition solution;
step three, preparing the titanium-nickel alloy deposition foil: placing the pretreated titanium-nickel foil obtained in the first step into the electrophoretic deposition solution obtained in the second step for deposition, and depositing a graphene oxide layer on the surface of the pretreated titanium-nickel foil to obtain a titanium-nickel alloy deposited foil; the deposition voltage is 120V, the current is 0.03A, and the deposition time is 4min;
step four, preparing the titanium-nickel alloy based composite material: tiling and stacking the titanium-nickel alloy deposited foil obtained in the third step layer by layer along the same graphene oxide layer direction, tiling and stacking the pretreated titanium-nickel alloy foil obtained in the first step on the outermost graphene oxide layer to obtain a laminated foil, and then placing the laminated foil in a rectangular graphite mold for spark plasma sintering at the sintering temperature of 800 ℃, the sintering pressure of 30MPa, the heat preservation time of 15min and the vacuum degree of 1Pa to obtain the titanium-nickel alloy-based composite material; the titanium-nickel alloy based composite material contains 150 layers of graphene oxide on average.
Fig. 1 is an SEM image of the titanium-nickel alloy based composite material prepared in this embodiment, and as can be seen from fig. 1, the titanium-nickel alloy based composite material is in a layered structure, and a graphene oxide layer is located between titanium-nickel alloy layers.
Fig. 2 is an interface SEM image of the titanium-nickel alloy based composite material prepared in this example, and the results of the corresponding micro-area EDS composition analysis are shown in table 1 below.
TABLE 1
Figure BDA0003550897630000071
Figure BDA0003550897630000081
As can be seen from fig. 2, the interface bonding of the titanium-nickel alloy-based composite material prepared in this embodiment is good, and has no obvious visible defect, and the thickness of the interface bonding layer is moderate, which indicates that no excessive reaction occurs between the titanium-nickel alloy matrix and the graphene oxide in the sintering process of the present invention, which is beneficial to maintaining the excellent performance of the graphene oxide, and the EDS component analysis result in table 1 indicates that the compound generated at the interface of the titanium-nickel alloy-based composite material is rich in titanium, nickel and carbon elements, and the element content is in gradient distribution, further demonstrating that the interface bonding of the titanium-nickel alloy-based composite material is good.
Comparative example 1
This comparative example comprises the following steps:
step one, pretreatment of a titanium-nickel foil: by means of wiresCutting a titanium nickel foil into rectangular thin sheets, sequentially polishing the surfaces of the rectangular thin sheets by using 500-mesh, 1000-mesh and 1500-mesh metallographic abrasive paper, sequentially putting the rectangular thin sheets into an acid solution for pickling for 8 seconds, putting the rectangular thin sheets into deionized water for washing, neutralizing the residual pickling solution, putting the neutralized pickling solution into absolute ethyl alcohol, putting the neutralized pickling solution into an ultrasonic cleaning machine for ultrasonic cleaning for 8 minutes, and drying the neutralized pickling solution to obtain a pretreated titanium nickel foil; the acid solution is prepared from HF and HNO 3 And H 2 The volume ratio of O to the component (1); the titanium nickel foil has super elasticity characteristic at room temperature, and the recoverable strain is more than 6%;
step two, preparing a titanium-nickel alloy laminated board: and (2) tiling and stacking the pretreated titanium-nickel foil obtained in the step one layer by layer, and then placing the laminated foil in a rectangular graphite mold for spark plasma sintering at the sintering temperature of 800 ℃, the sintering pressure of 30MPa, the heat preservation time of 15min and the vacuum degree of 1Pa to obtain the titanium-nickel alloy layer pressing plate.
Fig. 3 is an SEM image of the titanium-nickel alloy laminate prepared in the present comparative example, and it can be seen from fig. 3 that the microstructure of the titanium-nickel alloy laminate is dense and free of defects, and the original boundaries of the adjacent titanium-nickel alloy foils are completely disappeared, indicating that sufficient diffusion reaction occurs between the interfaces.
Fig. 4 is a damping performance curve diagram of the titanium-nickel alloy-based composite material prepared in example 1 of the present invention and the titanium-nickel alloy laminate prepared in comparative example 1, and it can be seen from fig. 4 that the damping factor of the titanium-nickel alloy laminate prepared in comparative example 1 is low, and the damping factors at-20 ℃, 25 ℃ and 200 ℃ are 0.057, 0.099 and 0.021, respectively, while the damping factors at-20 ℃, 25 ℃ and 200 ℃ of the titanium-nickel alloy-based composite material prepared in example 1 by introducing the graphene oxide layer respectively reach 0.089, 0.128 and 0.034, that is, the damping factors at corresponding temperatures are increased by 56%, 29.3% and 62%, respectively, and particularly, the damping performance of the titanium-nickel alloy-based composite material is increased to the highest level by introducing the graphene into the titanium-nickel alloy, which indicates that the present invention successfully improves the damping performance of the titanium-nickel alloy-based composite material by introducing the graphene into the titanium-nickel alloy, and realizes a high damping response in a wide temperature range.
Example 2
The embodiment comprises the following steps:
step one, pretreatment of a titanium-nickel foil: cutting the titanium-nickel foil into round slices by adopting linear cutting, sequentially polishing the surfaces of the round slices by adopting 500-mesh, 1000-mesh and 1500-mesh metallographic abrasive paper, sequentially putting the round slices into an acid solution for pickling for 5 seconds, putting the round slices into deionized water for washing, neutralizing the residual pickling solution, putting the round slices into absolute ethyl alcohol, putting the round slices into an ultrasonic cleaner for ultrasonic cleaning for 5 minutes, and drying to obtain the pretreated titanium-nickel foil; the acid solution is prepared from HF and HNO 3 And H 2 The volume ratio of O to the component (1); the titanium nickel foil has super elasticity characteristic at room temperature, and the recoverable strain is more than 6%;
step two, preparing electrophoretic deposition liquid: adding 100mg of graphene oxide with a sheet diameter of 1-3 mu m and a thickness of 1-5 nm and a multilayer structure into a beaker filled with 400mL of absolute ethyl alcohol for ultrasonic dispersion for 4 hours to obtain a stable graphene oxide/absolute ethyl alcohol suspension, and then adding 100mg of aluminum nitrate particles into the graphene oxide/absolute ethyl alcohol suspension to stir uniformly for 10min to obtain an electrophoretic deposition solution;
step three, preparing the titanium-nickel alloy deposition foil: placing the pretreated titanium-nickel foil obtained in the step one in the electrophoretic deposition solution obtained in the step two for deposition, and depositing a graphene oxide layer on the surface of the pretreated titanium-nickel foil to obtain a titanium-nickel alloy deposition foil; the deposition voltage is 120V, the current is 0.03A, and the deposition time is 5min;
step four, preparing the titanium-nickel alloy based composite material: tiling and stacking the titanium-nickel alloy deposited foil obtained in the third step layer by layer along the same graphene oxide layer direction, tiling and stacking the pretreated titanium-nickel alloy foil obtained in the first step on the outermost graphene oxide layer to obtain a laminated foil, and then placing the laminated foil in a circular graphite mold for spark plasma sintering, wherein the sintering temperature is 700 ℃, the sintering pressure is 30MPa, the heat preservation time is 10min, and the vacuum degree is 1Pa, so as to obtain the titanium-nickel alloy-based composite material; the titanium-nickel alloy based composite material contains 65 layers of graphene oxide on average.
Through tests, the damping factors of the titanium-nickel alloy-based composite material prepared in the embodiment at-20 ℃, 25 ℃ and 200 ℃ are 0.071, 0.112 and 0.027 respectively.
Example 3
The embodiment comprises the following steps:
step one, pretreatment of a titanium-nickel foil: cutting the titanium-nickel foil into triangular slices by adopting linear cutting, sequentially polishing the surfaces of the triangular slices by adopting 500-mesh, 1000-mesh and 1500-mesh metallographic abrasive paper, sequentially putting the triangular slices into an acid solution for pickling for 10 seconds, putting the triangular slices into deionized water for washing, neutralizing the residual pickling solution, putting the triangular slices into absolute ethyl alcohol, putting the triangular slices into an ultrasonic cleaner for ultrasonic cleaning for 10 minutes, and drying to obtain the pretreated titanium-nickel foil; the acid solution is prepared from HF and HNO 3 And H 2 The volume ratio of O to the component (1); the titanium nickel foil has super elasticity characteristic at room temperature, and the recoverable strain is more than 6%;
step two, preparing electrophoretic deposition liquid: adding 300mg of graphene oxide with a sheet diameter of 1-3 mu m and a thickness of 1-5 nm and a multilayer structure into a beaker filled with 400mL of absolute ethyl alcohol for ultrasonic dispersion for 5 hours to obtain a stable graphene oxide/absolute ethyl alcohol suspension, and then adding 300mg of aluminum nitrate particles into the graphene oxide/absolute ethyl alcohol suspension to stir uniformly for 10min to obtain an electrophoretic deposition solution;
step three, preparing the titanium-nickel alloy deposition foil: placing the pretreated titanium-nickel foil obtained in the step one in the electrophoretic deposition solution obtained in the step two for deposition, and depositing a graphene oxide layer on the surface of the pretreated titanium-nickel foil to obtain a titanium-nickel alloy deposition foil; the deposition voltage is 120V, the current is 0.03A, and the deposition time is 3min;
step four, preparing the titanium-nickel alloy based composite material: tiling and stacking the titanium-nickel alloy deposited foil obtained in the third step layer by layer along the same graphene oxide layer direction, tiling and stacking the pretreated titanium-nickel alloy foil obtained in the first step on the outermost graphene oxide layer to obtain a laminated foil, and then placing the laminated foil in a triangular graphite mold for spark plasma sintering, wherein the sintering temperature is 900 ℃, the sintering pressure is 30MPa, the heat preservation time is 20min, and the vacuum degree is 1Pa, so as to obtain the titanium-nickel alloy-based composite material; the titanium-nickel alloy based composite material contains 110 layers of graphene oxide on average.
Through tests, the damping factors of the titanium-nickel alloy-based composite material prepared by the embodiment at-20 ℃, 25 ℃ and 200 ℃ are respectively 0.080, 0.120 and 0.031.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.

Claims (4)

1. A preparation method of a titanium-nickel alloy based composite material with wide temperature range and high damping response is characterized by comprising the following steps:
step one, pretreatment of a titanium-nickel foil: cutting the titanium-nickel foil into slices by adopting linear cutting, sequentially polishing the surfaces of the slices by adopting 500-mesh, 1000-mesh and 1500-mesh metallographic abrasive paper, sequentially pickling in an acid solution, washing in deionized water, neutralizing the residual pickling solution, ultrasonically cleaning by adopting absolute ethyl alcohol, and drying to obtain the pretreated titanium-nickel foil; the titanium nickel foil has super elasticity characteristic at room temperature, and the recoverable strain is more than 6%;
step two, preparing electrophoretic deposition liquid: adding graphene oxide into absolute ethyl alcohol for ultrasonic dispersion to obtain a stable graphene oxide/absolute ethyl alcohol turbid liquid, then adding aluminum nitrate particles into the graphene oxide/absolute ethyl alcohol turbid liquid, and uniformly stirring to obtain an electrophoretic deposition liquid; the graphene oxide has a sheet diameter of 1-3 μm and a thickness of 1nm-5nm, and has a multilayer structure; the ratio of the mass of the graphene oxide to the volume of the absolute ethyl alcohol in the electrophoretic deposition solution is 0.25-0.75, the unit of the mass is mg, the unit of the volume is mL, and the mass ratio of the graphene oxide to the aluminum nitrate particles is 1;
step three, preparing the titanium-nickel alloy deposition foil: placing the pretreated titanium-nickel foil obtained in the step one in the electrophoretic deposition solution obtained in the step two for deposition, and depositing a graphene oxide layer on the surface of the pretreated titanium-nickel foil to obtain a titanium-nickel alloy deposition foil; the deposition voltage is 120V, the current is 0.03A, and the deposition time is 3min to 5min;
step four, preparing the titanium-nickel alloy based composite material: the titanium-nickel alloy deposited foil obtained in the third step is tiled and stacked layer by layer along the direction of the same graphene oxide layer, the pretreated titanium-nickel foil obtained in the first step is tiled and stacked on the outermost graphene oxide layer to obtain a laminated foil, and then the laminated foil is placed in a graphite mold to be subjected to discharge plasma sintering to obtain a titanium-nickel alloy-based composite material; the sintering temperature of the spark plasma sintering is 700-900 ℃, the sintering pressure is 30MPa, the heat preservation time is 10-20min, and the vacuum degree is 1Pa; the titanium-nickel alloy based composite material contains 50-220 layers of graphene oxide.
2. The method for preparing the titanium-nickel alloy based composite material with the wide temperature range and the high damping response according to claim 1, wherein the shape of the sheet in the step one is rectangular, circular or triangular; the acid solution is prepared from HF and HNO 3 And H 2 O is composed of the following components in a volume ratio of 1; the ultrasonic cleaning time is 5min to 10min.
3. The preparation method of the titanium-nickel alloy based composite material with the wide temperature range and the high damping response according to claim 1, wherein the ultrasonic dispersion time in the second step is 4h to 6h, and the stirring time is more than 10min.
4. The method for preparing the titanium-nickel alloy based composite material with the wide temperature range and the high damping response according to claim 1, wherein the damping factors of the titanium-nickel alloy based composite material at-20 ℃, 25 ℃ and 200 ℃ in the fourth step are 0.089, 0.128 and 0.034 respectively.
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