CN111360272B - Oxide interface toughening amorphous-based composite material and preparation method thereof - Google Patents

Oxide interface toughening amorphous-based composite material and preparation method thereof Download PDF

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CN111360272B
CN111360272B CN202010319279.5A CN202010319279A CN111360272B CN 111360272 B CN111360272 B CN 111360272B CN 202010319279 A CN202010319279 A CN 202010319279A CN 111360272 B CN111360272 B CN 111360272B
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amorphous
alloy powder
oxide interface
amorphous alloy
composite material
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CN111360272A (en
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张茂
黄婷
王新云
邓磊
龚攀
金俊松
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Huazhong University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • 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
    • C22C1/11—Making amorphous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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Abstract

The invention belongs to the field of amorphous alloy, and particularly discloses an oxide interface toughening amorphous-based composite material and a preparation method thereof, wherein the preparation method comprises the following steps: s1, carrying out high-energy ball milling treatment on the amorphous alloy powder in an oxygen-containing environment to form an amorphous oxide layer on the surface of the amorphous alloy powder; s2, carrying out hot isostatic pressing sintering forming on the amorphous alloy powder with the amorphous oxide layer formed on the surface, so that a network amorphous oxide interface is formed on the surface of the amorphous alloy powder, and the preparation of the oxide interface toughening amorphous matrix composite material is completed. In the composite material, the amorphous alloy powder is divided into cells with micro-nano scale by the network-shaped amorphous oxide interface, the oxide interface can effectively promote nucleation of a shear transition region, localization of shear deformation is avoided, meanwhile, the shear transition region is difficult to expand through the oxide interface due to the strong bonding effect of metal atoms and oxygen atoms on the oxide interface, and the cooperative improvement of the strength and plasticity of the amorphous-based composite material is realized.

Description

Oxide interface toughening amorphous-based composite material and preparation method thereof
Technical Field
The invention belongs to the field of amorphous alloy, and particularly relates to an oxide interface toughened amorphous-based composite material and a preparation method thereof.
Background
The amorphous alloy has excellent performances of high strength, high hardness, high elasticity, corrosion resistance, abrasion resistance and the like, and has wide application prospects in the fields of structural and functional materials. However, there are two problems associated with the large-scale application of amorphous alloys: first, the glass forming ability of amorphous alloys is insufficient and it is difficult to obtain larger size samples by conventional forming methods; second, amorphous alloys have poor plasticity at room temperature, exhibit strong brittleness, are difficult to use as load bearing members, and limit the forming process of amorphous alloys. Therefore, on one hand, a method capable of remarkably enlarging the critical dimension of the amorphous alloy needs to be found; on the other hand, it is also necessary to develop a method capable of strengthening and toughening an amorphous alloy.
The brittleness of amorphous alloys results from the localization of shear strain during deformation and the rapid expansion of individual shear bands. Generally, the introduction of a heterogenous crystalline phase with good plasticity into an amorphous alloy can effectively improve the plasticity of the amorphous alloy, but inevitably reduces the strength of the obtained amorphous-based composite material, which is called a long-term strength-plasticity trade-off problem. Therefore, finding a way to improve the plasticity of the amorphous alloy without reducing the strength is a hot spot of current research work.
In addition, the problem of oxidation of the amorphous alloy is also remarkable, and the common Zr-based and Cu-based amorphous alloys have strong chemical activity and are easy to generate surface oxidation when being heated. The surface activity of the amorphous alloy powder particles with the micro-nano scale is obviously enhanced compared with that of the amorphous alloy powder particles in a block state, and surface oxidation is introduced due to the limitation of the sealing performance and the vacuum performance of instruments and equipment in the sintering process, so that the surface oxidation is very easy to occur even under the room temperature condition. However, the moderate surface oxidation treatment can not only not damage the surface quality of the bulk amorphous alloy, but also effectively improve the surface hardness and corrosion resistance of the amorphous alloy.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides an oxide interface toughened amorphous-based composite material and a preparation method thereof, and aims to introduce an oxide interface layer into an amorphous alloy matrix to form a network-shaped amorphous oxide interface, so that on one hand, the oxide interface can effectively promote nucleation of a shear transition region and avoid localization of shear deformation, and on the other hand, the strong bonding effect of metal atoms and oxygen atoms on the oxide interface makes the shear transition region difficult to expand through the oxide interface, and the synergistic improvement of the material strength and plasticity is realized.
In order to achieve the above object, according to an aspect of the present invention, a method for preparing an oxide interface toughened amorphous-based composite material is provided, which comprises the following steps:
s1, carrying out high-energy ball milling treatment on the amorphous alloy powder in an oxygen-containing environment to form an amorphous oxide layer on the surface of the amorphous alloy powder;
s2, carrying out hot isostatic pressing sintering forming on the amorphous alloy powder with the amorphous oxide layer formed on the surface, so that a network amorphous oxide interface is formed on the surface of the amorphous alloy powder, and the preparation of the oxide interface toughening amorphous matrix composite material is completed.
Preferably, the amorphous alloy powder is prepared by the following method:
the pure metal raw materials are mixed in proportion, the amorphous master alloy is prepared by a copper mold water quenching method, and then the amorphous master alloy is prepared into amorphous alloy powder.
Further preferably, the amorphous master alloy is prepared into amorphous alloy powder by using a gas atomization method, a mechanical ball milling method, a plasma ball milling method or a plasma rotating electrode method.
Further preferably, in S1, when the high energy ball milling treatment is performed, air drying is ensured, and the oxygen content in the amorphous alloy powder with the amorphous oxide layer formed on the surface is not more than 10%.
More preferably, in the step S2, when the hot isostatic pressing sintering molding is performed, the temperature is controlled within a supercooled liquid phase region temperature of the amorphous alloy powder, the pressure is controlled to be 100MPa to 300MPa, the vacuum degree is controlled to be not more than 10Pa, and the duration is 10min to 30 min.
According to another aspect of the invention, the oxide interface toughened amorphous-based composite material prepared by the method is provided.
Further preferably, the amorphous alloy powder comprises amorphous alloy powder and a network-shaped amorphous oxide interface on the surface of the amorphous alloy powder, wherein the network-shaped amorphous oxide interface divides the amorphous alloy powder into cells with a micro-nano scale.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. according to the invention, an oxidation interface layer is introduced into an amorphous alloy matrix to form a network-shaped amorphous oxide interface, on one hand, the oxide interface can effectively promote nucleation of a shear transition region, so that localization of shear deformation is avoided, and on the other hand, the strong bonding effect of metal atoms and oxygen atoms on the oxide interface enables the shear transition region to be difficult to expand through the oxide interface, so that the shear deformation is strictly limited in a single cell formed by the oxide interface, and a mature shear band cannot be formed; in this way, not only does it not need to sacrifice the strength of the material, but a synergistic increase in its strength and plasticity can be achieved.
2. When the amorphous alloy powder is subjected to hot isostatic pressing sintering forming, the powder is subjected to surface pre-oxidation treatment to introduce an oxide interface toughening phase, so that the limitation of the forming capacity of amorphous alloy glass can be effectively overcome, and a large-size bulk amorphous sample is prepared.
3. The invention reduces the requirement on the vacuum degree of equipment in the preparation process of the amorphous alloy powder and is beneficial to reducing the production cost; meanwhile, the whole preparation process is simple, the requirement on equipment is low, special equipment is not needed, the method is easy to popularize, and the amorphous-based bulk material has good commercial application value.
4. The invention can prepare parts with any shape by hot isostatic pressing, and can further improve the material quality by specifically setting the process parameters such as temperature, pressure, time and the like during hot isostatic pressing.
Drawings
FIG. 1 is a schematic structural diagram of an oxide interface toughened amorphous-based composite according to an embodiment of the present invention;
FIG. 2 is a flow chart of the preparation of the oxide interface toughened amorphous matrix composite according to the embodiment of the present invention;
FIG. 3 is an atomic structure diagram of an oxide interface toughened Cu-Zr amorphous-based composite material according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The preparation method of the oxide interface toughened amorphous-based composite material provided by the embodiment of the invention, as shown in fig. 2, comprises the following steps:
s1, mixing pure metal raw materials in proportion, preparing amorphous master alloy by a copper mold water quenching method, and preparing amorphous master alloy into amorphous alloy powder; specifically, the pure metal material may be any pure metal material capable of forming amorphous alloy, such as pure metals of Cu, Zr, Ti, Ni, etc.;
s2, carrying out high-energy ball milling treatment on the amorphous alloy powder in an oxygen-containing environment to form an amorphous oxide layer on the surface of the amorphous alloy powder;
s3, carrying out hot isostatic pressing sintering forming on the amorphous alloy powder with the amorphous oxide layer formed on the surface, so that a network amorphous oxide interface is formed on the surface of the amorphous alloy powder, and the preparation of the oxide interface toughening amorphous matrix composite material is completed.
Further, in S1, the amorphous master alloy is prepared into the amorphous alloy powder with the nano-scale particle size by using an air atomization method, a mechanical ball milling method, a plasma ball milling method or a plasma rotating electrode method.
Further, in S2, when the high-energy ball milling is performed, air drying is ensured, and the oxidation degree of the amorphous alloy powder is controlled by adjusting the ball milling time, so that the oxygen content in the obtained amorphous alloy powder having the amorphous oxide layer on the surface thereof is not more than 10% (atomic ratio).
Further, in the step S3, when the hot isostatic pressing sintering forming is performed, the temperature is controlled within a supercooled liquid phase region temperature of the amorphous alloy powder (generally 400 ℃ to 500 ℃), the pressure is controlled to be 100MPa to 300MPa, the vacuum degree is not greater than 10Pa, and the duration is 10min to 30 min.
The oxide interface toughened amorphous-based composite material is prepared, as shown in fig. 1, an oxide interface layer is introduced into an amorphous alloy matrix to form a network-shaped amorphous oxide interface, and the amorphous oxide interface divides the amorphous alloy matrix into cells with a micro-nano scale.
The following are specific examples:
aiming at the application bottleneck of the Cu-Zr-based amorphous alloy and the manufacturing requirement of a novel structural material, in order to obtain a block Cu-Zr amorphous-based composite material which has stronger strength and plasticity and an oxide interface toughening layer, the preparation process comprises the following steps:
(1) mixing two pure metal raw materials of Cu and Zr according to the atomic ratio of 64:36, and preparing the amorphous master alloy Cu by a copper mold water quenching method64Zr36(ii) a And then carrying out gas spray treatment on the master alloy to obtain micro-nano amorphous alloy powder, and uniformly mixing the powdery Cu and Zr amorphous alloy powder by adopting ball milling.
(2) The high-energy ball milling surface oxygen permeation treatment is carried out under the environment of room temperature, drying and standard atmospheric pressure, so that an amorphous oxide layer is formed on the surface of the amorphous alloy powder. Adjusting the ball milling time to ensure that the oxygen content of the obtained amorphous alloy powder is about 8 percent, namely the amorphous alloy powder is transformed into Cu through decomposition59Zr33O8。
(3) Preparing the pre-oxidized amorphous alloy mixed powder into a Cu-Zr amorphous-based composite material with an oxide interface by a hot isostatic pressing technology at the temperature of 600K, keeping the static pressure at 100MPa for 20min, and obtaining a bulk material which can be used as a bearing structure material and the atomic structure of which is shown in figure 3. The prepared composite material Cu of oxide interface toughening amorphous base59Zr33O8It is an alloy system with Cu and Zr as main alloy components and oxygen-containing interface layer, and has homogeneous internal components and no macro elementsThe difference of component concentration, the tensile strength can reach 3.0GPa, and the elongation is higher than 0.5, which means that the proposed oxide interface toughened amorphous-based composite material can obtain better plasticity without sacrificing the strength, and can even further improve the strength, thereby solving the long-term strength-plasticity balance dilemma.
Compared with the traditional mode of introducing a softer crystalline second phase, the method greatly increases the strength and plasticity of the material on one hand due to the existence of oxygen; on the other hand, the problem that the surface oxidation is easy to occur when the Zr-based and Cu-based amorphous alloys which puzzle a long time are heated due to strong chemical activity is solved, the requirements on production conditions are effectively reduced, and the production cost is reduced.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (4)

1. The preparation method of the oxide interface toughened amorphous-based composite material is characterized by comprising the following steps of:
s1, carrying out high-energy ball milling treatment on the amorphous alloy powder in an oxygen-containing environment to form an amorphous oxide layer on the surface of the amorphous alloy powder; when high-energy ball milling treatment is carried out, air drying is ensured, and the oxygen content in the amorphous alloy powder with the amorphous oxide layer formed on the surface is not more than 10 percent;
the amorphous alloy powder is prepared by the following method: mixing pure metal raw materials in proportion, preparing amorphous master alloy by a copper mold water quenching method, and preparing amorphous master alloy into amorphous alloy powder;
s2, carrying out hot isostatic pressing sintering forming on the amorphous alloy powder with the amorphous oxide layer formed on the surface, and controlling the temperature within the supercooled liquid phase interval temperature of the amorphous alloy powder when carrying out hot isostatic pressing sintering forming, wherein the supercooled liquid phase interval temperature is 400-500 ℃, the pressure is controlled to be 100-300 MPa, the vacuum degree is not more than 10Pa, and the duration is 10-30 min, so that a network amorphous oxide interface is formed on the surface of the amorphous alloy powder, and the preparation of the oxide interface toughening amorphous matrix composite material is completed.
2. The method for preparing the oxide interface toughened amorphous-based composite material according to claim 1, wherein the amorphous master alloy is prepared into the amorphous alloy powder by using an air atomization method, a mechanical ball milling method, a plasma ball milling method or a plasma rotating electrode method.
3. An oxide interface toughened amorphous-based composite material, characterized by being prepared by the method of claim 1 or 2.
4. The oxide interface toughened amorphous-based composite material of claim 3, comprising amorphous alloy powder and a network-like amorphous oxide interface on the surface thereof, wherein the network-like amorphous oxide interface divides the amorphous alloy powder into cells of micro-nano scale.
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