CN112109393B - Aluminum oxide/nickel-titanium alloy/aluminum oxide composite material prepared by diffusion bonding and method thereof - Google Patents

Aluminum oxide/nickel-titanium alloy/aluminum oxide composite material prepared by diffusion bonding and method thereof Download PDF

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CN112109393B
CN112109393B CN202010768576.8A CN202010768576A CN112109393B CN 112109393 B CN112109393 B CN 112109393B CN 202010768576 A CN202010768576 A CN 202010768576A CN 112109393 B CN112109393 B CN 112109393B
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nickel
titanium alloy
aluminum oxide
alumina
composite material
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CN112109393A (en
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李烨飞
牛瑞霞
李海生
李书文
郑巧玲
亦雨奇
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Xian Jiaotong University
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    • 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
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • 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
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • 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
    • B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
    • 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
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • 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
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • 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
    • B32B38/18—Handling of layers or the laminate
    • B32B38/1808—Handling of layers or the laminate characterised by the laying up of the layers
    • B32B38/1816—Cross feeding of one or more of the layers
    • 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
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B9/041—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
    • 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
    • B32B38/0036—Heat treatment
    • B32B2038/0048—Annealing, relaxing
    • 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
    • B32B2250/00—Layers arrangement
    • B32B2250/03—3 layers
    • 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
    • B32B2250/00—Layers arrangement
    • B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
    • 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
    • B32B2307/558—Impact strength, toughness

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
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Abstract

The invention discloses an alumina/nickel-titanium alloy/alumina composite material prepared by diffusion bonding and a method thereof, wherein a nickel-titanium alloy sheet and an alumina sheet are used as raw materials, and the nickel-titanium alloy sheet is placed between the two alumina sheets to prepare a sample with a sandwich structure; placing the obtained sandwich structure sample in a graphite mold and fastening; and putting the graphite mold into a vacuum carbon tube furnace, and annealing to obtain the aluminum oxide/nickel-titanium alloy/aluminum oxide sandwich layered composite material. The invention improves Al2O3Toughness of the ceramic of (1), realization of Al2O3Reliable connection of ceramic and metal.

Description

Aluminum oxide/nickel-titanium alloy/aluminum oxide composite material prepared by diffusion bonding and method thereof
Technical Field
The invention belongs to the technical field of ceramic matrix composite materials, and particularly relates to an alumina/nickel-titanium alloy/alumina composite material prepared by diffusion bonding and a method thereof.
Background
Alumina (Al)2O3) Is a well-known ceramic which has been widely used in many aspects due to its excellent heat resistance, high electrical conductivity, ultra-high hardness, light weight and excellent wear resistance. However, its inherent brittleness makes Al2O3It is extremely difficult to form large-sized or complex-geometry structural components for engineering applications. In contrast, Al2O3The workpiece is usually combined with metal to form a multi-phase composite material which reconciles the thermal stability and wear resistance of the ceramic with the toughness of the metal, thereby enlarging the bulk Al2O3The ceramic is used as an important engineering ceramic.
Until now, ceramics have rarely used nickel bases containing active elementsThe binary alloy connects the workpieces. Al (Al)2O3Relatively high melting point and low vapor pressure of Ni-Ti alloy, and Ni-Ti alloy and Al2O3The close thermal expansion coefficient is beneficial to interface connection, and the equiatomic Ni-Ti alloy becomes combined Al2O3Promising bonding alloys for ceramic workpieces.
Disclosure of Invention
The technical problem to be solved by the invention is to provide an alumina/nickel-titanium alloy/alumina composite material prepared by diffusion bonding and a method thereof, aiming at the defects in the prior art, so as to optimize the interface structure, further improve the mechanical property of the metal ceramic composite material and prepare the alumina/nickel-titanium alloy/alumina sandwich layered composite material with excellent performance.
The invention adopts the following technical scheme:
a method for preparing an alumina/nickel-titanium alloy/alumina composite material by diffusion bonding comprises the following steps:
s1, placing the nickel-titanium alloy sheet between two aluminum oxide sheets to prepare a sandwich-structured sample by taking the nickel-titanium alloy sheet and the aluminum oxide sheets as raw materials;
s2, placing the sandwich structure sample obtained in the step S1 in a graphite mold and fastening;
s3, placing the graphite mould into a vacuum carbon tube furnace, and annealing to obtain the aluminum oxide/nickel-titanium alloy/aluminum oxide sandwich layered composite material.
Specifically, in step S1, the shape of the surface of the nitinol sheet is square, the size of the nitinol sheet is 10-20 mm × 0.1-1 mm, and the size of the oxidized aluminum sheet is 10-20 mm × 1-5 mm.
Specifically, in step S2, a pressure of 1 to 5kPa is applied to perform fastening.
Specifically, in step S3, the temperature rise rate of the annealing treatment is 5-10 ℃/min, the reaction temperature is 1250-1500 ℃, and the heat preservation time is 2-6 h.
Specifically, in step S3, argon gas is introduced into the vacuum carbon tube furnace.
Specifically, an alumina/nitinol/alumina sandwich layerIn the composite material, nickel-titanium alloy and alumina react chemically to produce AlNi2Ti and TiO, AlNi2The thickness of the interface layer of Ti is 18-22 μm, and the thickness of the interface layer of TiO is 4-18 μm.
The invention also provides an alumina/nickel-titanium alloy/alumina composite material prepared by the method.
Compared with the prior art, the invention has at least the following beneficial effects:
the method for preparing the aluminum oxide/nickel-titanium alloy/aluminum oxide composite material by diffusion bonding selects the sheet material as the raw material, and is convenient, quick and simple; meanwhile, the sandwich structure sample is uniformly diffused, is slightly influenced by external materials, and has less introduced impurity elements and excellent mechanical property; and finally, sintering by using a graphite mold in a tube furnace, so that the efficiency is high and the cost is low.
Furthermore, the purpose of selecting the sheet material with smaller size and surface area is to save materials and dies, and the experimental effect is best.
Furthermore, the pressure is applied to the graphite mould to mainly promote the plastic deformation of the connecting surface to reach a close contact state, so that the diffusion is accelerated.
Furthermore, the annealing reaction temperature is 1250-1500 ℃, the solid-liquid phase change exists in the temperature range, the reaction between the aluminum oxide and the nickel-titanium alloy can be well researched, the annealing heat preservation time is 2-6 h, and the short-time heat preservation, the homogenization of joint components and the long-time heat preservation are considered from the viewpoint of improving the productivity.
Furthermore, argon is introduced mainly for ensuring that the connecting surface reaches certain cleanliness, creating a reducing atmosphere and preventing the oxidation of two materials, particularly nickel-titanium alloy.
Further, the thinner the thickness is, the easier the sintering together, the more easily plastic deformation occurs, and the better the diffusion effect.
An alumina/Ni-Ti alloy/alumina composite material, Ni-4Ti alloy with relatively high melting point and low vapor pressure, and Al2O3Close coefficient of thermal expansion, favorable boundaryAnd (4) surface connection. The hardness and toughness of the alumina/nickel titanium alloy/alumina composite material are relatively good.
In conclusion, the invention improves Al2O3Toughness of ceramics, realization of Al2O3A reliable method for ceramic and metal joining.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 shows Al in example 12O3/Ni-Ti/Al2O3SEM image of the interface reaction layer;
FIG. 2 shows Al in example 12O3/Ni-Ti/Al2O3EDS picture of interfacial reaction layer.
Detailed Description
The invention provides an alumina/nickel-titanium alloy/alumina composite material prepared by diffusion bonding and a method thereof, wherein Ni-Ti alloy is used for Al2O3Performing gas protection diffusion connection, and preparing aluminum oxide/nickel-titanium alloy/aluminum oxide (Al) through solid-liquid phase reaction2O3/Ni-Ti/Al2O3) A sandwich layered composite material.
The invention relates to a method for preparing an aluminum oxide/nickel-titanium alloy/aluminum oxide composite material by diffusion bonding, which comprises the following steps:
s1, taking nickel-titanium alloy and aluminum oxide as raw materials; ni in the nickel-titanium alloy: the mass percent of Ti is 1.0%: 1.0 percent;
Al2O3ultrasonically cleaning the sheet and the Ni-Ti alloy sheet in acetone for 20 minutes, and placing the Ni-Ti alloy sheet with the thickness of 0.1-1 mm on two Al sheets2O3Preparing a sample with a sandwich structure in the ceramic plate;
the surface of the Ni-Ti alloy sheet is square, the size is 10-20 mm multiplied by 0.1-1 mm, Al2O3The sheet has the size of 10-20 mm multiplied by 1-5 mm and the purity of 96%, and is prepared by a conventional salivation forming method.
S2, placing the sample with the sandwich structure in a graphite mold, and fastening the sample with a fixed-torque wrench, wherein the applied pressure is 1-5 kPa;
s3, annealing the graphite mold in a vacuum carbon tube furnace filled with argon, wherein the heating rate of 0-1200 ℃ is 10 ℃/min, the heating rate of more than 1200 ℃ is 5 ℃/min, the reaction temperature is 1250-1500 ℃, and the heat preservation time is 2-6 h, so that the aluminum oxide/nickel-titanium alloy/aluminum oxide (Al) is prepared2O3/Ni-Ti/Al2O3) A sandwich layered composite material.
The composite material prepared in step S3 was cut along a direction perpendicular to the interface, and the microstructure, degree of reaction and phase composition of the interface were analyzed by SEM and EDS to investigate the effect of temperature and time on the ni-ti alloy/alumina interface reaction layer.
The aluminum/nickel-titanium alloy/aluminum oxide (Al) prepared by diffusion bonding of the invention2O3/Ni-Ti/Al2O3) The sandwich layered composite material comprises an outer layer of aluminum oxide and an intermediate layer of nickel titanium alloy.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Placing Ni-Ti alloy sheets with the thickness of 1mm on two Al sheets2O3Preparing a sample with a sandwich structure in the ceramic plate;
then, the graphite is placed in a graphite mould, fastened by a fixed torque wrench, applied with the pressure of 1kPa, annealed in a vacuum carbon tube furnace filled with argon, the reaction temperature is 1250 ℃, and the temperature is kept for 2 hours.
Referring to fig. 1 and 2, the sample was cut in a direction perpendicular to the interface, and SEM and EDS tests were performed on the interface. The results show that the nickel-titanium alloy and the aluminum oxide are subjected to chemical reaction to generate AlNi2Ti and TiO, the thicknesses of the interface layers are respectively 20 mu m and 18 mu m, the interface layers are thin, and continuous interface layers are not formed.
Example 2
Placing Ni-Ti alloy sheets with the thickness of 1mm on two Al sheets2O3Preparing a sample with a sandwich structure in the ceramic plate;
then, the graphite is placed in a graphite mold, fastened by a fixed torque wrench, applied with pressure of 2kPa, annealed in a vacuum carbon tube furnace filled with argon, the reaction temperature is 1400 ℃, and the temperature is kept for 4 hours.
The sample was cut perpendicular to the interface direction and SEM and EDS tests were performed on the interface. The results show that the nickel-titanium alloy and the aluminum oxide are subjected to chemical reaction to generate AlNi2Ti and TiO, the thickness of the interface layer is 22 μm and 4 μm.
Example 3
Placing Ni-Ti alloy sheets with the thickness of 1mm on two Al sheets2O3Preparing a sample with a sandwich structure in the ceramic plate;
then, the graphite mold is placed in a graphite mold, the graphite mold is fastened by a fixed torque wrench, the pressure is applied to 4kPa, the annealing reaction is carried out in a vacuum carbon tube furnace filled with argon, and the temperature is kept for 6 hours.
The sample was cut perpendicular to the interface direction and SEM and EDS tests were performed on the interface. The results show that the nickel-titanium alloy and the aluminum oxide are subjected to chemical reaction to generate AlNi2Ti and TiO, the thickness of the interface layer is 18 μm and 14 μm.
Example 4
Placing Ni-Ti alloy sheets with the thickness of 1mm on two Al sheets2O3Preparing a sample with a sandwich structure in the ceramic plate;
then, the graphite mold is placed in a graphite mold, the graphite mold is fastened by a fixed torque wrench, the pressure is applied to 5kPa, the annealing reaction is carried out in a vacuum carbon tube furnace filled with argon, and the temperature is kept for 6 hours.
The sample was cut perpendicular to the interface direction and SEM and EDS tests were performed on the interface. The results show that the nickel-titanium alloy and the aluminum oxide are subjected to chemical reaction to generate AlNi2Ti and TiO, the thickness of the interface layer is 20 μm and 11 μm.
Al2O3The matrix and the Ni-Ti alloy are fully reacted, and the nickel-titanium alloy and the ceramic are reacted, so that the wettability between the ceramic and the metal is improved, and the alumina ceramic and the metal nickel-titanium alloy are in good contact.
In conclusion, the aluminum oxide/nickel-titanium alloy/aluminum oxide composite material prepared by diffusion bonding and the method thereof realize the bonding of metals with larger differences of the properties of the metals and ceramics, enable the metallurgical bonding to be formed at the interface at the early stage, and have excellent mechanical properties and wide application range.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (4)

1. A method for preparing an alumina/nickel-titanium alloy/alumina composite material by diffusion bonding is characterized by comprising the following steps:
s1, taking a nickel-titanium alloy sheet and an aluminum oxide sheet as raw materials, placing the nickel-titanium alloy sheet between two aluminum oxide sheets to prepare a sample with a sandwich structure, wherein the surface of the nickel-titanium alloy sheet is square, the size of the nickel-titanium alloy sheet is 10-20 mm multiplied by 0.1-1 mm, and the size of the aluminum oxide sheet is 10-20 mm multiplied by 1-5 mm;
s2, placing the sandwich structure sample obtained in the step S1 in a graphite mold and fastening;
s3, placing the graphite mold into a vacuum carbon tube furnace, and annealing to obtain the aluminum oxide/nickel-titanium alloy/aluminum oxide sandwich layered composite material, wherein the temperature rise rate of the annealing treatment is 5-10 ℃/min, the reaction temperature is 1250-1500 ℃, the heat preservation time is 2-6 h, and in the aluminum oxide/nickel-titanium alloy/aluminum oxide sandwich layered composite material, nickel is containedThe titanium alloy and the alumina are chemically reacted to generate AlNi2Ti and TiO, AlNi2The thickness of the interface layer of Ti is 18-22 μm, and the thickness of the interface layer of TiO is 4-18 μm.
2. The method according to claim 1, wherein in step S2, the fastening is performed by applying a pressure of 1 to 5 kPa.
3. The method according to claim 1, wherein in step S3, argon gas is introduced into the vacuum carbon tube furnace.
4. An alumina/nitinol/alumina composite prepared according to the method of claim 1.
CN202010768576.8A 2020-08-03 2020-08-03 Aluminum oxide/nickel-titanium alloy/aluminum oxide composite material prepared by diffusion bonding and method thereof Active CN112109393B (en)

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