CN114438427B - Method for inducing grain nanocrystallization by small-scale mechanical deformation at room temperature - Google Patents

Method for inducing grain nanocrystallization by small-scale mechanical deformation at room temperature Download PDF

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CN114438427B
CN114438427B CN202210072147.6A CN202210072147A CN114438427B CN 114438427 B CN114438427 B CN 114438427B CN 202210072147 A CN202210072147 A CN 202210072147A CN 114438427 B CN114438427 B CN 114438427B
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deformation
matrix
small
metal
nanocrystallization
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CN114438427A (en
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郭晓雷
郭强
谭占秋
刘文富
宋俊
石鹏
屈也
唐勇
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Shanghai Jiaotong University
Huanghuai University
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Huanghuai University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D7/00—Modifying the physical properties of iron or steel by deformation
    • C21D7/02—Modifying the physical properties of iron or steel by deformation by cold working
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2200/00—Crystalline structure
    • C22C2200/04—Nanocrystalline

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Abstract

The invention discloses a method for inducing grain nanocrystallization by small-scale mechanical deformation at room temperature. The composite column body is subjected to compression deformation of repeated small-scale cyclic loading at room temperature, nanocrystalline is successfully induced in a metal matrix with a micron size, and the matrix nanocrystallization is possibly induced by simply relying on small-scale mechanical deformation at room temperature. Compared with the factors such as large deformation, high pressure, high temperature and the like commonly used in the traditional grain refinement process, the method for preparing the nanocrystalline has the characteristics of non-uniform deformation, and can realize the grain nanocrystallization by only applying small-scale mechanical deformation to the metal matrix at room temperature and normal pressure, and has the advantages of simplicity and easiness in operation, mild conditions and the like. The invention provides a new idea for nanocrystallization of actual bulk metal.

Description

Method for inducing grain nanocrystallization by small-scale mechanical deformation at room temperature
Technical Field
The invention belongs to the field of material interface treatment, and relates to a method for inducing grain nanocrystallization by small-scale mechanical deformation at room temperature.
Background
The grain size of a metal has a significant impact on its strength and shape. After the metal grains are refined, grain boundaries in unit volume are increased, movement barriers of dislocation are increased, and the strength is increased as resistance to shaping deformation of the metal material is increased. Meanwhile, the number of crystal grains participating in deformation is increased due to the increase of crystal boundaries, and the deformation is even, so that the larger deformation capacity is obtained, and the shaping is enhanced. The method of improving the mechanical properties of materials, typically by way of grain refinement, is known as fine grain strengthening. The strength and grain size of the metal material satisfy the Hall-Petch formula: sigma (sigma) s ＝σ i +K y d -1/2 Wherein sigma s Is the yield strength, sigma i And Ky is a constant related to the material and d is the grain size, the above formula shows that the strength of the material increases with decreasing grain size, generally in the range of 0.3-400 μm, and anti-Hall-Petch occurs when the grain size is less than 300 nm. The relationship between toughness and grain size satisfies: βtc= lnB-lnC-lnd -1/2 Where β, B, C are constants, tc is the brittle transition temperature, d is the grain size, the above formula shows that the toughness of the material increases as the grain size decreases. In general, for structural regulation of metal, strength enhancement is often accompanied by plastic reduction, and there is an inversion relation of strong plastic mismatch, while grain refinement can meet dual strength and toughness enhancement within a certain grain size range.
The above researches show that the grain refinement can significantly improve the strength and the shaping of the material, but the grain refinement has certain difficulty. There are two general ways of grain refinement to produce nanocrystals: 1) The Bottom-up concept designs and synthesizes fine grain structures from the angles of atoms and molecules, such as rapid solidification, vapor deposition and the like; 2) The Top-Down concept refines bulk metals into fine grains, such as equal channel extrusion, multi-axis compression/forging, cumulative stacking, continuous shear deformation, high pressure torsion, etc. It is known that the existing implementation scheme for grain refinement in the technology adopting the Top-Down concept has the characteristics of high energy consumption such as large deformation, high temperature, high pressure and the like. The method for circularly loading the sample in small scale at room temperature to obtain the nanocrystalline provides a new research idea for the current grain refinement process.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the purposes of the invention is to provide a method for inducing the nano-crystallization of crystal grains by small-scale mechanical deformation at room temperature.
One of the purposes of the invention is realized by adopting the following technical scheme:
a method for inducing grain nanocrystallization by small-scale mechanical deformation at room temperature, comprising the following steps:
(1) Preparing a composite column body of a metal matrix and a carrier, wherein the metal matrix in the composite column body is arranged at the upper part and the lower part of the carrier, and an independent interface with an inclination angle is formed between the metal matrix and the carrier;
(2) And (3) carrying out uniaxial compression deformation on the composite column body obtained in the step (1), wherein the loading mode is repeated cyclic loading, and the composite column body shape variable is 2% -7%.
Further, the loading times are more than or equal to 30.
Further, the diameter of the composite column in the step (1) is 1-3 μm.
Further, the inclination angle in the step (1) is 30-60 degrees.
Further, in the step (1), the ratio of the elastic modulus of the carrier to the elastic modulus of the metal matrix is more than or equal to 5. A material having a modulus of elasticity much greater than that of the target metal is selected as the carrier, which needs to have good wettability with the metal to form good interface contact. After the metal matrix and the high-modulus carrier are compounded, under the same deformation, the phase change is mainly concentrated on the metal matrix, and the deformation of the carrier is tiny and negligible and can be regarded as a rigid body.
Further, in the step (1), the composite column is prepared by a focused ion beam method after a metal matrix and a carrier form a composite.
Further, the method for forming the compound by the metal aggregate and the carrier is a stirring casting method. The stirring casting method is easy to introduce large-size grains between the metal aggregate and the carrier, and provides effective correspondence for the nanocrystallization of the grains after deformation.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for inducing grain nanocrystallization by small-scale mechanical deformation at room temperature. The composite column body is subjected to compression deformation of repeated small-scale cyclic loading at room temperature, nanocrystalline is successfully induced in a metal matrix with a micron size, and the matrix nanocrystallization is possibly induced by simply relying on small-scale mechanical deformation at room temperature. Compared with the factors of large deformation, high pressure, high temperature and the like necessary in the traditional grain refinement process, the method for obtaining the nanocrystalline has the characteristics of non-uniform deformation, and can realize the grain nanocrystallization by only applying small-scale mechanical deformation to the metal matrix at room temperature and normal pressure, and has the advantages of simple and easy control of operation, mild conditions and the like. The method provides an example for realizing the nanocrystallization of the crystal grains by simply relying on small-scale mechanical deformation at room temperature, and provides a new idea for the nanocrystallization of actual bulk metal.
Drawings
FIG. 1 is a schematic diagram showing a process of compounding a metallic Al matrix and a carrier SiC ceramic by a stirring manufacturing method according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of a small-scale mechanical deformation induced grain nanocrystallization at room temperature obtained in the embodiment of the invention, wherein FIG. 2a is a process of preparing SiC/Al MMCs by immersing a 4H-SiC single crystal wafer in molten Al liquid; FIG. 2b shows that SiC/Al MMCs are fixed on a 45 DEG wedge stage, and a single SiC/Al composite microcolumn with a 45 DEG inclination angle is prepared by adopting an FIB; FIG. 2c is a nanoindentation uniaxial compression experiment of a SiC/Al composite microcolumn; FIG. 2d is a multiple uniaxial compression of a SiC/Al composite microcolumn, wherein 1-3 represent the first uniaxial compression (1 st UC), nth cumulative uniaxial compression (n th -UC) after grain refinement of Al matrix, X-th cumulative uniaxial compression (X) th -UC) post-Al matrix MS structure morphology; FIG. 2e is a schematic representation of the microstructure characterization of a transmission electron microscope;
FIG. 3 shows a composite column with a diameter of 1 μm prepared by a focused ion beam obtained in the embodiment of the invention, a metal Al matrix under an upper SiC ceramic carrier, and an independent interface with a 45-degree inclination angle;
FIG. 4 is a microstructure characterization of a composite cylinder of an embodiment of the present invention before and after application of small-scale mechanical deformation induction, wherein FIG. 4a is a representation of the Al matrix in a single crystal state in the range of several microns at the near interface of SiC contacts prior to deformation; FIG. 4b shows the Al matrix after multiple small-scale cyclic loading; fig. 4c is a TEM dark field image of the microstructure after induced by the application of small-scale mechanical deformation, and fig. 4d is an electron diffraction pattern of the SAED selected region of the circled selected region of fig. 4 c.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and detailed description, wherein it is to be understood that, on the premise of no conflict, the following embodiments or technical features may be arbitrarily combined to form new embodiments.
Examples
A method for inducing grain nanocrystallization by small-scale mechanical deformation at room temperature, comprising the following steps:
(1) The schematic diagram of the process for preparing the composite column of the metal Al matrix and the SiC ceramic carrier is shown in FIG. 1, firstly, the SiC substrate is lifted in melted pure Al, so that the Al is solidified on two sides of the SiC substrate, and an Al-SiC-Al model material similar to a sandwich structure is prepared, thus the Al matrix and the SiC ceramic carrier composite (SiC/Al MMCs); the SiC/Al MMCs are fixed on a 45-degree wedge-shaped table, a composite of metal Al and a SiC ceramic carrier is prepared into a composite column with the diameter of 1 mu m by utilizing a focused ion beam, a metal Al matrix is arranged on the upper side, the SiC ceramic carrier is arranged on the lower side and the single interface is at a 45-degree inclination angle, a specific SEM (scanning electron microscope) chart is shown in figure 3, and the preparation method is described in the prior publication of the inventor: guo X, et al Interfacial strength and deformation mechanism of SiC-Al composite micro-pilers [ J ]. Scripta Materialia,2016.
(2) And (3) adopting a flat head pressure head of the nanoindenter to uniaxially compress and deform the composite column obtained in the step (1), and introducing an inclination angle of 45 degrees to an interface in the composite column to enable the Al matrix part to generate gradient deformation during uniaxial compression. The compression deformation is strain controlled, the deformation amount is small-scale 2% elastic deformation, the loading mode is that after repeated cyclic loading is carried out for 22 times, the deformation is gradually transited to 20% plastic deformation, the total loading times are 36 times, the non-uniform deformation of the matrix is continuously accumulated due to the cyclic loading of the small scale, and finally the nano-crystallization of the inner crystal grains of the metal Al is realized.
FIG. 2 is a schematic diagram of a process of inducing nanocrystalline grain by small-scale mechanical deformation at room temperature according to the present invention, wherein FIG. 2a is a process of preparing SiC/Al MMCs by immersing a 4H-SiC single crystal wafer in molten Al liquid; FIG. 2b shows that SiC/Al MMCs are fixed on a 45 DEG wedge stage, and a single SiC/Al composite microcolumn with a 45 DEG inclination angle is prepared by adopting an FIB; FIG. 2c is a nanoindentation uniaxial compression experiment of a SiC/Al composite microcolumn; FIG. 2d shows multiple uniaxial compression of a SiC/Al composite microcolumn, wherein 1-3 represent the morphology of an Al matrix MS after the first uniaxial compression (1 st-UC), after the nth cumulative uniaxial compression (nth-UC), and after the xth-UC), respectively; FIG. 2e is a schematic representation of the characterization of microstructures using transmission electron microscopy.
After the deformation is finished, TEM sample preparation is carried out on the composite column body, microstructure comparison is carried out on the composite column body and the sample before the deformation, and the nano-crystallization condition of the crystal grains in the Al matrix is observed. FIG. 4 is a microstructure characterization of a composite cylinder of an embodiment of the present invention before and after application of small-scale mechanical deformation induction, wherein FIG. 4a shows that the Al matrix is in a single-crystal state in the range of several microns at the near-interface of SiC contacts before deformation; FIG. 4b shows that after multiple small-scale cyclic loading, the Al matrix is plastically deformed and TEM bright field image shows grain refinement; fig. 4c shows the same grain refinement for the TEM dark field image, and fig. 4d shows the SAED diffraction ring near the interface of fig. 4c (selected part of circle), indicating that the grain nanocrystallization at the Al matrix interface has been achieved, with a grain size of-30 nm.
In summary, the invention firstly combines the metal material with the high modulus material, the high modulus material plays a role of a carrier, and meanwhile, the high modulus material has good wettability with the metal matrix, and can form good interface combination. After the combination, a well-combined interface is formed, and the interface shows the action of dislocation constraint in the later deformation. Then under the additional load, the interface formed by the composite cylinder of the invention and the stress axis form a certain inclination angle relation, so that the stress acts on the interface to generate non-uniform deformation. In addition, in order to apply compressive stress to the metal base, the composite column with a diameter of several micrometers, a metal base under a carrier and a single interface at a certain inclination angle with a compression axis is prepared by virtue of the micro-nano etching function of the focused ion beam. The preparation of the composite microcolumn is used for standardizing the sample dimension and facilitating later mechanical analysis. The key point of the invention is that in the uniaxial compression process, multiple compression deformation controlled by strain is adopted, the deformation amount is 2-7% of the small scale, and the loading mode is multiple cyclic loading. This small scale cyclic loading causes non-uniform deformation of the matrix to accumulate, eventually leading to nanocrystallization within the metal matrix. The method provided by the invention can be conveniently expanded to other actual metal materials, and provides a thinking for realizing the induction of the nanocrystallization of the metal materials by small-scale mechanical deformation at room temperature.
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, but any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention are intended to be within the scope of the present invention as claimed.

Claims (1)

1. The method for inducing the grain nanocrystallization by small-scale mechanical deformation at room temperature is characterized by comprising the following steps of:
(1) Preparing a composite column body of a metal matrix and a carrier, wherein the metal matrix in the composite column body is arranged at the upper part and the lower part of the carrier, and an independent interface with an inclination angle is formed between the metal matrix and the carrier;
the preparation process of the composite column body is as follows: pulling the SiC substrate in melted pure Al, so that the Al is solidified on two sides of the SiC substrate, and obtaining an Al matrix and SiC ceramic carrier compound; fixing the composite of the Al matrix and the SiC ceramic carrier on a 45-degree wedge-shaped table, and preparing the composite of the metal Al and the SiC ceramic carrier into a composite column with the diameter of 1 mu m by utilizing a focused ion beam, wherein the metal Al matrix is arranged on the upper side, the SiC ceramic carrier is arranged on the lower side and the single interface is at an inclination angle of 45 degrees;
(2) Adopting a flat head pressure head of a nanoindenter to carry out uniaxial compression deformation on the composite column obtained in the step (1), wherein the compression deformation is strain control, the deformation amount is small-scale 2% elastic deformation, the loading mode is repeated cyclic loading, after 22 times of loading, the transition is carried out to 20% plastic deformation, and the total loading times are 36 times; the small-scale cyclic loading enables the non-uniform deformation of the matrix to be continuously accumulated, and finally the nano-crystallization of the inner crystal grains of the metal Al is realized.
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CN102560045B (en) * 2010-12-22 2014-10-01 中国科学院金属研究所 Block nano structure low-carbon steel and manufacturing method thereof
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