A high-toughness aluminum matrix composite material with a physical bonding interface and a preparation method and application thereof

By employing high-energy ball milling and low-temperature sintering hot extrusion processes, a NiTi/Al composite material without interfacial reaction was prepared, solving the problems of interfacial reaction and bonding strength in NiTi/Al composite materials and significantly improving the mechanical properties of the material.

CN119220842BActive Publication Date: 2025-11-25HARBIN INST OF TECH
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Patent Information

Application Number
CN202411338842.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-25
Publication Date
2025-11-25
Estimated Expiration
2044-09-25

AI Technical Summary

Technical Problem

Existing NiTi/Al composites suffer from severe interfacial reactions and diffusion between NiTip and the matrix alloy, leading to the formation of intermetallic compounds, which impairs the interfacial bonding strength. Furthermore, changes in NiTip composition reduce the shape memory effect, while the interfacial bonding area between NiTip and the Al matrix is ​​small and has poor deformability.

Method used

NiTi/Al composite materials without interfacial reactions are prepared by deforming NiTip into elliptical or flat strip shapes using high-energy ball milling, combined with low-temperature discharge plasma sintering and low-temperature hot extrusion. This process avoids interfacial reactions at high temperatures by increasing the contact surface area and interfacial bonding strength between NiTip and the Al matrix.

Benefits of technology

The tensile strength and elongation of the composite material were significantly improved, with yield strength increased by 74.9%, tensile strength increased by 48.8%, and elongation increased by 153.8%, achieving a high strength and toughness effect.

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Abstract

The application discloses a high-toughness aluminum matrix composite material with a physical bonding interface and a preparation method and application thereof, belongs to the field of aluminum matrix composite materials, and aims to solve the technical problem of premature failure of a matrix-reinforcing phase particle interface in a loading process of an existing NiTip reinforced aluminum matrix composite material.The method comprises the following steps: firstly, mixing SiCnp and small-size aluminum matrix powder by high-energy ball milling; then, mixing NiTip and large-size aluminum matrix powder by high-energy ball milling; thirdly, mixing the two kinds of mixed powders and unball-milled aluminum powder by low-speed ball milling to obtain Al-SiCnp-NiTip composite powder; and finally, performing low-temperature discharge plasma sintering and low-temperature hot extrusion on the Al-SiCnp-NiTip composite powder.The method can also be used for the preparation of other metal and alloy composite materials.The obtained composite material has high strength and toughness, and can be applied to the fields of aerospace and automobile engineering.
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Description

Technical Field

[0001] This invention belongs to the field of aluminum-based composite materials, specifically relating to a high-strength and high-toughness aluminum-based composite material with a physical bonding interface, its preparation method, and its application. Background Technology

[0002] NiTi (SMAs) undergoes a martensitic phase transformation when subjected to external stimuli. The shape memory effect or hyperelastic deformation of SMAs can be utilized to dissipate energy and toughen the material during external stress. Previous studies have shown that NiTi alloy-reinforced Al, Mg, and Ag composites exhibit significantly improved mechanical properties. The unique shape memory effect (SME) or hyperelastic deformation of NiTi alloys has been used to apply compressive stress to the matrix, thereby enhancing the ductility and fatigue resistance of the composites.

[0003] However, the current NiTi / Al composite materials have the following problems: (1) NiTi is prone to severe interfacial reaction and interfacial diffusion with the matrix alloy, resulting in the formation of intermetallic compounds, which not only damages the interfacial bonding strength, but also causes changes in NiTi composition and reduces SME ability. (2) In NiTi / Al composite materials, most NiTi are spherical, with a small interfacial bonding area with the Al matrix and poor deformability. Summary of the Invention

[0004] The purpose of this invention is to solve the technical problem of premature failure of the matrix-reinforcing phase particle interface during loading in existing NiTip reinforced aluminum matrix composites, and to provide a high-strength and high-toughness aluminum matrix composite with a physically bonded interface, its preparation method and application.

[0005] The technical solution of the present invention is as follows:

[0006] One objective of this invention is to provide a method for preparing a high-strength and high-toughness aluminum-based composite material with a physically bonded interface, the method comprising the following steps:

[0007] S1: SiCnp is mixed with small-sized aluminum matrix powder by high-energy ball milling to obtain Al-SiCnp mixed powder;

[0008] S2: NiTip is mixed with large-size aluminum matrix powder by high-energy ball milling to obtain Al-NiTip mixed powder;

[0009] S3: Al-SiCnp mixed powder, Al-NiTip mixed powder and unmilled aluminum powder are ball-milled at low speed to obtain Al-SiCnp-NiTip composite powder;

[0010] S4: The Al-SiCnp-NiTip composite powder is first subjected to low-temperature discharge plasma sintering, followed by low-temperature hot extrusion to obtain a high-strength and tough aluminum-based composite material with a physical bonding interface.

[0011] Further specified, the amount of SiCnp added in S1 is 1.1 to 7.5 wt.% of the small-sized aluminum matrix powder.

[0012] Further specifying, the small-sized aluminum matrix powder in S1 includes aluminum powder and its alloy powder, with a size of 5 to 15 μm.

[0013] Further specified, the high-energy ball milling speed in S1 is 300-400 rpm, and the time is 8-15 h.

[0014] Further specified, the amount of NiTip added in S2 is 11-50 wt.% of the large-size aluminum matrix powder.

[0015] Further specifying, the large-size aluminum matrix powder in S2 includes aluminum powder and its alloy powder, with a size of 50 to 150 μm.

[0016] Further specified, the high-energy ball milling speed in S2 is 300-400 rpm, and the time is 8-15 h.

[0017] Further specified, the mass ratio of Al-SiCnp mixed powder, Al-NiTip mixed powder and unmilled aluminum powder in S3 is 1:1:(0.5~0.8).

[0018] Further specified, the S3 low-speed ball mill speed is 100-200 rpm, and the time is 1-5 hours.

[0019] Further specified, the temperature of the low-temperature discharge plasma sintering in S4 is 500-530℃, the pressure is 40-60MPa, and the time is 5-15min.

[0020] Further specified, the hot extrusion temperature in S4 is 400-430℃, the extrusion ratio is (16-25):1, and the extrusion rate is 0.1-0.5mm / s.

[0021] The second objective of this invention is to provide a high-strength and high-toughness aluminum-based composite material prepared by the above method, wherein the composite material has a tensile strength ≥285GPa and an elongation ≥13.5%.

[0022] The third objective of this invention is to provide an application of a high-strength and high-toughness aluminum-based composite material prepared by the above method in the fields of aerospace and automotive engineering.

[0023] The fourth objective of this invention is to provide an application of the above-mentioned method in the preparation of high-strength and high-toughness metal matrix composites.

[0024] Further specifying, the metal matrix is ​​one of Mg, Fe, Ti, Cu and their respective alloys.

[0025] The advantages of this invention compared to existing technologies are:

[0026] (1) This invention employs a controlled low-temperature SPS + hot extrusion process to prepare NiTi / Al composite materials with no interfacial reaction and good interfacial bonding. Sintering is carried out at a lower temperature to ensure no interfacial reaction, but the density is lower; combined with low-temperature hot extrusion, the composite material is densified and has good interfacial bonding (effective load transfer).

[0027] (2) This invention employs high-energy ball milling to ball mill spherical NiTi / Al powder. Under high milling energy, the NiTi deforms from a spherical shape to an elliptical or flat strip shape, thereby increasing the interfacial bonding between the NiTi and the Al matrix by increasing the surface area of ​​contact between the NiTi and the Al matrix. Then, low-temperature hot extrusion is selected, utilizing its large plastic rheological stress to further promote the deformation of the NiTi. This preparation method largely solves the problem of premature failure of the matrix-reinforcing phase particle interface during loading in traditional NiTi / Al composite materials. Attached Figure Description

[0028] Figure 1 SEM image of the interface-reactive NiTi / Al composite material prepared in Example 1;

[0029] Figure 2 SEM image of the NiTi / Al composite material with interfacial reaction prepared in Comparative Example 1;

[0030] Figure 3 STEM image of the interface-reactive NiTi / Al composite material prepared in Example 1;

[0031] Figure 4 HAADF image of the NiTi / Al composite material without interfacial reaction prepared in Example 1;

[0032] Figure 5 EDS image of the interface-reactive NiTi / Al composite material prepared in Example 1;

[0033] Figure 6 The table shows the room temperature tensile stress-strain curves of the NiTi / Al composite materials prepared in Example 1 and Comparative Example 1. Detailed Implementation

[0034] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0035] Unless otherwise specified, the experimental methods used in the following examples are conventional methods. Unless otherwise specified, the materials, reagents, methods, and instruments used are all conventional materials, reagents, methods, and instruments in the art, and can be obtained commercially by those skilled in the art.

[0036] The terms “comprising,” “including,” “having,” “containing,” or any other variations thereof, as used in the following embodiments, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that includes the listed elements is not necessarily limited to those elements, but may include other elements not expressly listed or elements inherent to such a composition, step, method, article, or apparatus.

[0037] In this invention, "an embodiment" or "embodiment" refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the invention. The phrase "in one embodiment" appearing in different places in this specification does not necessarily refer to the same embodiment, nor is it a single or selective embodiment that excludes other embodiments.

[0038] The endpoints and any values ​​of the ranges disclosed in this invention are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0039] Example 1: The preparation method of the high-strength and high-toughness aluminum-based composite material with a physical bonding interface in this example is carried out according to the following steps:

[0040] S1: 0.28g of SiCnp (average diameter ~43nm) and 23.72g of spherical aluminum powder (purity 99.9%, average diameter ~7.8μm) were added to a planetary ball mill and mixed at 300rpm for 10h with a ball-to-material ratio of 15:1 to obtain Al-SiCnp mixed powder.

[0041] S2: 12.48g of NiTip (Ni:Ti atomic ratio = 50.82:49.18, average diameter ~18.10μm) and 47.52g of spherical aluminum powder (purity 99.9%, average diameter ~72.48μm) were added to a planetary ball mill and mixed at 300rpm for 10h with a ball-to-material ratio of 15:1 to obtain Al-NiTip mixed powder;

[0042] S3: Add 24g of Al-SiCnp mixed powder, 24g of Al-SiCnp mixed powder and 12g of unmilled aluminum powder (purity 99.9%, average diameter ~72.48μm) to a planetary ball mill and mix them at 200rpm for 5h with a ball-to-material ratio of 15:1 to obtain Al-SiCnp-NiTip composite powder;

[0043] S4: The Al-SiCnp-NiTip composite powder was encapsulated in a graphite mold. The mold was then placed in a discharge plasma sintering furnace and evacuated to prevent powder oxidation contamination from contact with air. Discharge plasma sintering was performed at a temperature of 530℃, a uniaxial pressure of 50MPa, and a holding time of 10min. After sintering and furnace cooling, the mold was placed in a ring furnace. The mold contained, from top to bottom, an extrusion cup, a pure aluminum block, the sintered composite material, and a graphite gasket. Low-temperature hot extrusion was performed at a temperature of 430℃, a holding time of 1.5h, an extrusion ratio of 25:1, and an extrusion rate of 0.5mm / s, resulting in a high-strength and tough aluminum-based composite material with a physical bonding interface.

[0044] Comparative Example 1: The preparation method of the aluminum-based composite material with interfacial reaction in this embodiment is carried out according to the following steps:

[0045] S1: 0.28g of SiCnp (average diameter ~43nm) and 23.72g of spherical aluminum powder (purity 99.9%, average diameter ~7.8μm) were added to a planetary ball mill and mixed at 300rpm for 10h with a ball-to-material ratio of 15:1 to obtain Al-SiCnp mixed powder.

[0046] S2: 12.48g of NiTip (Ni:Ti atomic ratio = 50.82:49.18, average diameter ~18.10μm) and 47.52g of spherical aluminum powder (purity 99.9%, average diameter ~72.48μm) were added to a planetary ball mill and mixed at 300rpm for 10h with a ball-to-material ratio of 15:1 to obtain Al-NiTip mixed powder;

[0047] S3: Add 24g of Al-SiCnp mixed powder, 24g of Al-SiCnp mixed powder and 12g of unmilled aluminum powder (purity 99.9%, average diameter ~72.48μm) to a planetary ball mill and mix them at 200rpm for 5h with a ball-to-material ratio of 15:1 to obtain Al-SiCnp-NiTip composite powder;

[0048] S4: The Al-SiCnp-NiTip composite powder was encapsulated in a graphite mold. The mold was then placed in a discharge plasma sintering furnace and evacuated to prevent powder oxidation contamination from contact with air. Discharge plasma sintering was performed at a temperature of 530℃, a uniaxial pressure of 50MPa, and a holding time of 10min. After sintering and furnace cooling, the mold was placed in a ring furnace. The mold contained, from top to bottom, an extrusion cup, a pure aluminum block, the sintered composite material, and a graphite gasket. Hot extrusion was performed at a temperature of 480℃, a holding time of 1.5h, an extrusion ratio of 25:1, and an extrusion rate of 0.5mm / s, resulting in an aluminum-based composite material with interfacial reactions.

[0049] Figure 1 SEM images of the interface-free composite material prepared in Example 1, from... Figure 1 As can be seen, after hot extrusion deformation, the Al-SiCnps region is significantly elongated along the extrusion direction, the reinforcing phase is uniformly dispersed, and Al-NiTip and Al regions are interspersed between the Al-SiCnp regions. The NiTip in the Al-NiTip region is uniformly distributed and the NiTip is deformed significantly, all developing into elongated strips. However, under large deformation, no obvious defects or interfacial reactions were found at the interface with the Al matrix, indicating good interfacial bonding.

[0050] Figure 2 SEM images of the composite material with interfacial reaction prepared in Comparative Example 1 were obtained from... Figure 2 As can be seen, when hot extrusion is performed at higher temperatures, the NiTip in the Al-NiTip region is uniformly distributed and the NiTip deformation is large, but the NiTip undergoes severe interfacial reaction, and obvious defects can be observed at the interface.

[0051] Figure 3 STEM image of the interface-free composite material prepared in Example 1, from Figure 3 It can be observed that NiTi is composed of fine nanoparticles, and the grains in the Al matrix are elongated after extrusion. The interface is well bonded and there are no obvious defects; there are no obvious reaction products at the interface.

[0052] Figure 4 The HAADF plot of the interface-free composite material prepared in Example 1 is shown below. Figure 4As can be seen, the NiTip interface is flat, but there is a transition layer with a thickness of ~10nm.

[0053] Figure 5 The image shows the EDS plot of the interface-reactive composite material prepared in Example 1. Linear mapping using energy dispersive spectroscopy (EDS) further confirmed that the NiTi / Al interface consists of a 5-15 nm thick amorphous oxide interface layer, which is beneficial for the bonding of NiTi to the aluminum matrix. Furthermore, there is no significant inter-element diffusion between NiTi and the Al matrix, and the interface is very clear, indicating the successful preparation of an interface-reactive NiTi / Al composite material.

[0054] Room temperature tensile tests were conducted on the NiTi / Al composites prepared in Example 1 and Comparative Example 1, and the results showed that... Figure 6 ),from Figure 6 As can be seen, the interfacial reaction has a significant impact on the mechanical properties of NiTi / Al composites. Compared with NiTi / Al composites with interfacial reactions, the yield strength, tensile strength, and elongation of NiTi / Al composites without interfacial reactions are all significantly improved. The yield strength increased from 143.2 MPa to 250.5 MPa, an increase of 74.9%; the tensile strength increased from 192.0 MPa to 285.7 MPa, an increase of 48.8%; and the elongation increased from 5.2% to 13.5%, an increase of 153.8%. It is noteworthy that the presence of the interfacial reaction has a direct impact on the strengthening effect of the composite. This indicates that the preparation of NiTi / Al composites without interfacial reactions has great potential in achieving the goal of strengthening and toughening aluminum-based composites.

[0055] The above description is merely a preferred embodiment of the present invention. These specific embodiments are different implementations based on the overall concept of the present invention, and the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A method for preparing a high-strength and high-toughness aluminum-based composite material with a physical bonding interface, characterized in that, The method described: S1: SiCnp is mixed with small-sized aluminum matrix powder by high-energy ball milling to obtain Al-SiCnp mixed powder; the SiCnp addition amount is 1.1~7.5 wt.% of the matrix powder, and the size of the small-sized aluminum matrix powder is 5~15μm; S2: NiTip is mixed with large-size aluminum matrix powder by high-energy ball milling to obtain Al-NiTip mixed powder; the amount of NiTip added is 11~50wt.% of the matrix powder, and the size of the large-size aluminum matrix powder is 50~150μm; S3: Al-SiCnp mixed powder, Al-NiTip mixed powder and unmilled aluminum powder are ball-milled at low speed to obtain Al-SiCnp-NiTip composite powder; the mass ratio of Al-SiCnp mixed powder, Al-NiTip mixed powder and unmilled aluminum powder is 1:1:(0.5~0.8). S4: The Al-SiCnp-NiTip composite powder is first subjected to low-temperature discharge plasma sintering, followed by low-temperature hot extrusion to obtain a high-strength and tough aluminum-based composite material with a physical bonding interface; the sintering temperature is 500~530℃, and the hot extrusion temperature is 400~430℃.

2. The method according to claim 1, characterized in that, The aluminum matrix powder in S1 includes aluminum powder and its alloy powder. The ball milling speed is 300~400 rpm and the time is 8~15 h.

3. The method according to claim 1, characterized in that, The aluminum-based matrix powder in S2 includes aluminum powder and its alloy powder. The ball milling speed is 300~400 rpm and the time is 8~15 h.

4. The method according to claim 1, characterized in that, In S3, the ball mill speed is 100~200 rpm, and the time is 1~5 hours.

5. The method according to claim 1, characterized in that, The sintering pressure in S4 is 40~60MPa, and the time is 5~15min.

6. The method according to claim 1, characterized in that, The extrusion ratio in S4 is (16~25):1, and the extrusion rate is 0.1~0.5mm / s.

7. The high-strength and high-toughness aluminum-based composite material obtained by the method according to any one of claims 1-6, characterized in that, The composite material has a tensile strength ≥285GPa and an elongation ≥13.5%.

8. The application of the high-strength and high-toughness aluminum-based composite material according to claim 7 in the fields of aerospace and automotive engineering.

9. The application of the method according to any one of claims 1-6 in the preparation of high-strength and high-toughness metal matrix composites.

10. The application according to claim 9, characterized in that, The metallic matrix is ​​one of Mg, Fe, Ti, Cu, and their respective alloys.

Citation Information

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