Device and method for in-situ measurement of mechanical properties and microstructure of metal materials

Abstract

The present invention discloses a device and method for providing atomic-level in-situ isostatic pressure mechanical performance testing for nano-metal samples in a transmission electron microscope. The present invention belongs to the technical field of in-situ testing and characterization of nanomaterial microstructures. The present invention innovatively designs a new isostatic pressure container device: by using micro-manipulation technology, the nano-metal sample is loaded and encapsulated between two carbon nanocones, and an isostatic pressure container can be obtained. More importantly, the design also innovatively realizes the in-situ isostatic pressure mechanical performance testing of metal samples in a transmission electron microscope: by squeezing the side walls of the carbon nanocones with a probe, isostatic pressure is applied to the metal sample in the isostatic environment, thereby realizing the in-situ isostatic pressure mechanical performance testing of the metal sample in a transmission electron microscope, and the static pressure size is controllable.

Description

Technical Field

[0001] The present invention belongs to the technical field of in-situ testing and characterization of nanomaterial microstructures, and in particular relates to a device and method for in-situ measuring the mechanical properties and microstructure of metal materials. Background Art

[0002] Over the past two decades, with economic development, the demand for natural resource extraction and the development of fields such as navigation and aerospace has become more pressing. Critical metal components in equipment such as crustal mining, deep-sea submarines, and high-pressure manufacturing all require operation in high isostatic pressure environments. Exploring the structural evolution of these metals under isostatic pressure and revealing the changes in mechanical properties and structure of metals under isostatic pressure has guiding significance for optimizing the mechanical properties of materials under isostatic pressure and fabricating high-performance materials using isostatic pressing. Recent studies have shown that when the grain size of materials is reduced to nanometers, their mechanical properties differ significantly from those of bulk materials, and this "size effect" has attracted considerable attention. However, current studies of the structural and mechanical properties of materials under isostatic pressure mostly use diamond compression to compress metal samples, followed by indirect characterization of structural changes through changes in XRD, UV, or IR spectra. Direct observation of structural evolution of materials under isostatic pressure using transmission electron microscopy is rare. Although previous studies have used carbon nanotubes as isostatic pressure vessels to achieve in situ studies of metal deformation under high pressure using transmission electron microscopy, this approach has a low success rate and is uncontrollable.

[0003] In response to the above technical difficulties, the present invention takes a different approach and proposes a device and method for in-situ measurement of the mechanical properties and microstructure of metal materials. Summary of the Invention

[0004] In response to the shortcomings of the existing technology, the present invention proposes a device and method for in-situ measurement of the mechanical properties and microstructure of metal materials. Carbon nanocones with high compressive strength (~40GPa) are used as isostatic pressure containers, and the metal sample is loaded into the carbon nanocones through a micro-operating system. The metal sample is then sealed between the two carbon nanocones by applying an electric current, thereby encapsulating the metal nanomaterial in the isostatic pressure container. Afterwards, the prepared sample is mounted on a probe rod, and pressure is applied to the metal sample inside the isostatic pressure container by a mechanical probe. In situ atomic-scale observation of the structural changes of the metal sample under the isostatic pressure environment is achieved in a transmission electron microscope, and the correlation between structure and mechanical properties is established. This new device and experimental method can not only efficiently realize the preparation of nanoscale isostatic pressure containers, but also realize the controllable adjustment of the isostatic pressure of the metal sample in a transmission electron microscope.

[0005] To achieve the above object, the present invention provides the following solutions:

[0006] A device for in-situ measurement of the mechanical properties and microstructure of metal materials, comprising: a W wire substrate, a carbon material, a metal sample, and an in-situ probe rod;

[0007] The specific assembly sequence of the device is: assembling the carbon material and the metal sample on the W wire substrate in sequence, and installing the W wire substrate on the in-situ probe rod.

[0008] Preferably, the carbon material includes but is not limited to: carbon nanocones and carbon nanotubes.

[0009] Preferably, the metal samples include but are not limited to: single crystals, binary alloys, low entropy alloys, medium entropy alloys and high entropy alloys.

[0010] Preferably, the process of obtaining the W wire substrate is: using corroded W wire as the substrate, the specific process is: placing W wire with a diameter of 0.2-0.5 mm in a 5%-10% sodium hydroxide aqueous solution, loading a 2-3V DC power supply, and obtaining a needle-shaped W wire tip.

[0011] The present invention also provides a method for in-situ measuring the mechanical properties and microstructure of a metal material, which is based on the device for in-situ measuring the mechanical properties and microstructure of a metal material and includes the following steps:

[0012] Based on the W wire substrate, the nanometal sample was loaded and encapsulated in the middle of several carbon materials using micromanipulation technology to obtain an isostatic pressing device with W wire as the substrate;

[0013] placing the isostatic pressing device on an in-situ probe rod of a transmission electron microscope;

[0014] A probe is used to apply isostatic pressure of controllable magnitude to the metal sample inside the carbon material, thereby achieving in-situ isostatic pressure performance testing of the metal sample in a transmission electron microscope.

[0015] Preferably, the carbon material includes but is not limited to: carbon nanocones and carbon nanotubes.

[0016] Preferably, the metal samples include but are not limited to: single crystals, binary alloys, low entropy alloys, medium entropy alloys and high entropy alloys.

[0017] Preferably, the method for obtaining a W wire substrate is: using corroded W wire as the substrate, the specific process is: placing a W wire with a diameter of 0.2 to 0.5 mm in a 5% to 10% sodium hydroxide aqueous solution, loading a 2 to 3V DC power supply, and obtaining a needle-shaped W wire tip.

[0018] Preferably, based on a W wire substrate, a method for loading and encapsulating a nanometal sample between a plurality of carbon materials using micromanipulation technology to obtain an isostatic pressing device based on W wire includes:

[0019] Installing the W wire tip and carbon material into a micromanipulation system;

[0020] The carbon material is mounted on the tip of the W wire using a manipulator of a micromanipulation system;

[0021] Load current to weld the carbon material to the tip of the W wire to obtain a carbon material / W wire sample.

[0022] Using a manipulator of a micromanipulation system, the metal sample is transferred to the carbon material / W wire sample to obtain a metal / carbon material / W wire sample;

[0023] A second carbon material is mounted on the metal / carbon material / W wire sample using a micromanipulator, and an electric current is applied to seal the metal sample between the two carbon materials to obtain an isostatic pressing device with W wire as the substrate, wherein the current parameter is: 100~500mA.

[0024] Preferably, the isostatic pressing device with W wire as the substrate is transferred to the in-situ probe rod of the transmission electron microscope, and the side wall of the carbon material is squeezed by the probe to apply controllable isostatic pressure to the metal sample in the isostatic pressing environment, thereby realizing the in-situ isostatic pressure mechanical performance test and atomic-level structural characterization of the metal sample in the transmission electron microscope.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] The present invention provides a novel isostatic pressure container device for nanometal samples, which can be directly transferred to a transmission electron microscope to achieve atomic-level characterization testing with controllable static pressure.

[0027] The present invention can also realize in-situ isostatic pressure mechanical performance testing of metal samples in a transmission electron microscope: the isostatic pressure container is transferred to the in-situ probe rod of the transmission electron microscope, and the side walls of the carbon nanocones are squeezed by the probe to apply isostatic pressure to the metal sample in the isostatic pressure environment, thereby realizing in-situ isostatic pressure mechanical performance testing of the metal sample in a transmission electron microscope.

[0028] The present invention breaks through the limitations of sample preparation during in-situ mechanical characterization testing using a traditional transmission electron microscope, and the isostatic pressing device can be directly installed on an in-situ probe rod in a transmission electron microscope.

[0029] The present invention solves the technical challenge of applying isostatic pressure to metal samples by electron irradiation of carbon atoms in the traditional method, and adopts a probe to apply isostatic pressure of adjustable size. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the technical solution of the present invention, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0031] Figure 1 Schematic diagram of the tip of a 0.2 mm diameter W wire after corrosion in an embodiment of the present invention;

[0032] Figure 2 Schematic diagram of the preparation of carbon nanocones / HEAs / carbon nanocones / W wire samples in an embodiment of the present invention;

[0033] Figure 3 Schematic diagram of in-situ isostatic pressure performance test in an embodiment of the present invention. DETAILED DESCRIPTION

[0034] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0035] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0036] Example 1

[0037] The device for in-situ measurement of the mechanical properties and microstructure of metal materials includes a W-wire substrate, a carbon material, a metal sample, and an in-situ probe rod. The specific assembly sequence for the device is to sequentially assemble the carbon material and the metal sample onto the W-wire substrate, followed by mounting the W-wire substrate onto the probe rod.

[0038] In this embodiment, the carbon material includes but is not limited to carbon nanocones and carbon nanotubes.

[0039] In this embodiment, metal samples include but are not limited to: single crystals, binary alloys, low entropy alloys, medium entropy alloys, and high entropy alloys.

[0040] In this embodiment, the process of obtaining a W wire substrate is: using corroded W wire as the substrate, the specific process is: placing a W wire with a diameter of 0.2 to 0.5 mm in a 5% to 10% sodium hydroxide aqueous solution, loading a 2 to 3V DC power supply, and obtaining a needle-shaped W wire tip.

[0041] In this embodiment, the in-situ characterization and mechanical property testing of the metal sample in a transmission electron microscope are achieved by transferring the W wire tip to the in-situ probe rod.

[0042] Example 2

[0043] The present invention also provides a method for in-situ measuring the mechanical properties and microstructure of a metal material, comprising the following steps:

[0044] Based on the W wire substrate, the nanometal sample was loaded and encapsulated in the middle of several carbon materials using micromanipulation technology to obtain an isostatic pressing device with W wire as the substrate;

[0045] The isostatic pressing device is placed on the in-situ probe rod of the transmission electron microscope;

[0046] By applying controllable isostatic pressure to the metal sample inside the carbon material through a probe, in-situ isostatic pressure performance testing of the metal sample in a transmission electron microscope can be achieved.

[0047] In this embodiment, the carbon material includes but is not limited to carbon nanocones and carbon nanotubes.

[0048] In this embodiment, metal samples include but are not limited to: single crystals, binary alloys, low entropy alloys, medium entropy alloys, and high entropy alloys.

[0049] In this embodiment, the method for obtaining a W wire substrate is: using corroded W wire as the substrate, the specific process is: placing a W wire with a diameter of 0.2 to 0.5 mm in a 5% to 10% sodium hydroxide aqueous solution, loading a 2 to 3V DC power supply, and obtaining a needle-shaped W wire tip.

[0050] In this embodiment, based on a W wire substrate, a micromanipulation technique is used to load and encapsulate a nanometal sample between several carbon materials to obtain an isostatic pressing device with a W wire substrate:

[0051] Install the W wire tip and carbon material into the micromanipulation system;

[0052] The carbon material is mounted on the tip of the W wire using a micromanipulator;

[0053] Load current to weld the carbon material to the tip of the W wire to obtain a carbon material / W wire sample.

[0054] Using a manipulator of a micromanipulation system, the metal sample is transferred to the carbon material / W wire sample to obtain a metal / carbon material / W wire sample;

[0055] A second carbon material is mounted on the metal / carbon material / W wire sample using a micromanipulator, and an electric current is applied to seal the metal sample between the two carbon materials, thereby obtaining an isostatic pressing device with W wire as the substrate, i.e., an isostatic pressing container device that can be transferred to a transmission electron microscope, wherein the current parameter is 100 to 500 mA.

[0056] In this embodiment, the isostatic pressure container with W wire as the base is transferred to the in-situ probe rod of the transmission electron microscope. The probe squeezes the side wall of the carbon material and applies controllable isostatic pressure to the metal sample in the isostatic pressure environment, thereby realizing in-situ isostatic pressure mechanical performance testing and atomic-level structural characterization of the metal sample in the transmission electron microscope.

[0057] Example 3

[0058] In this embodiment, a W wire with a diameter of 0.2 mm is selected and then electrochemically corroded in a 10% sodium hydroxide aqueous solution. The corrosion parameter is a 2V DC power supply. After the corrosion is completed, a needle-like W wire tip can be obtained. The specific morphology is shown in the attached figure. Figure 1 As shown. The corroded W wire substrate and carbon nanocone are installed in the micromanipulation system, and the carbon nanocone is installed on the tip of the W wire using the manipulator of the micromanipulation system. The carbon nanocone is welded to the tip of the W wire using a current of 200mA to obtain a carbon nanocone / W wire sample; then the solid high entropy alloy (HEAs) sample is transferred to the carbon nanocone / W wire tip using a micromanipulation arm to obtain a HEAs / carbon nanocone / W wire sample; the second carbon nanocone is installed on the tip of the HEAs / carbon nanocone / W wire sample using the manipulator of the micromanipulation system again, and the HEAs sample is sealed between the two carbon nanocones using a current of 200mA to obtain a carbon nanocone / HEAs / carbon nanocone / W wire sample: an isostatic pressure container that can be transferred to a transmission electron microscope. The preparation schematic diagram is shown in the attached figure. Figure 2 The isostatic pressure container with W wire as the base is transferred to the in-situ probe rod of the transmission electron microscope. The probe squeezes the side wall of the carbon nanocone and applies a controllable isostatic pressure to the metal sample in the isostatic pressure environment, thereby realizing the in-situ isostatic pressure performance test of the metal sample in the transmission electron microscope. The specific test method is shown in the attached figure. Figure 3 shown.

[0059] This embodiment can realize in-situ isostatic pressure performance testing of HEAs in a transmission electron microscope, filling a gap in this research field and playing a vital role in the future development of crustal resource mining, submarines and other equipment.

[0060] The embodiments described above are merely descriptions of preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Without departing from the spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by persons skilled in the art should fall within the scope of protection defined by the claims of the present invention.

Claims

1. A device for in-situ measurement of the mechanical properties and microstructure of metal materials, characterized in that: include: W wire substrate, carbon material, metal sample and in situ probe rod; The specific assembly sequence of the device is: assembling the carbon material and the metal sample on the W wire substrate in sequence, and installing the W wire substrate on the in-situ probe rod; A second carbon material was mounted on the metal / carbon material / W wire sample using a micromanipulator, and an electric current was applied to seal the metal sample between the two carbon materials.

2. The device for in-situ measurement of mechanical properties and microstructure of metal materials according to claim 1, characterized in that: The carbon material includes at least one of carbon nanocones or carbon nanotubes.

3. The device for in-situ measurement of mechanical properties and microstructure of metal materials according to claim 1, characterized in that: The metal sample includes at least one of a single crystal, a binary alloy, a low entropy alloy, a medium entropy alloy or a high entropy alloy.

4. The device for in-situ measurement of mechanical properties and microstructure of metal materials according to claim 1, characterized in that: The process of obtaining the W wire substrate is as follows: using corroded W wire as the substrate, the specific process is: placing W wire with a diameter of 0.2~0.5 mm in a 5%~10% sodium hydroxide aqueous solution, loading a 2~3 V DC power supply, and obtaining a needle-shaped W wire tip.

5. The method for in-situ measurement of the mechanical properties and microstructure of a metal material is implemented based on the device for in-situ measurement of the mechanical properties and microstructure of a metal material according to claim 1, characterized in that: The following steps are involved: Based on the W wire substrate, the nanometal sample was loaded and encapsulated in the middle of several carbon materials using micromanipulation technology to obtain an isostatic pressing device with W wire as the substrate; placing the isostatic pressing device on an in-situ probe rod of a transmission electron microscope; A probe is used to apply isostatic pressure of controllable magnitude to the metal sample inside the carbon material, thereby achieving in-situ isostatic pressure performance testing of the metal sample in a transmission electron microscope.

6. The method for in-situ measurement of mechanical properties and microstructure of metal materials according to claim 5, characterized in that: The carbon material includes at least one of carbon nanocones or carbon nanotubes.

7. The method for in-situ measurement of mechanical properties and microstructure of metal materials according to claim 5, characterized in that: The metal sample includes at least one of a single crystal, a binary alloy, a low entropy alloy, a medium entropy alloy or a high entropy alloy.

8. The method for in-situ measurement of mechanical properties and microstructure of metal materials according to claim 5, characterized in that: The method for obtaining a W wire substrate is: using corroded W wire as the substrate. The specific process is: placing a W wire with a diameter of 0.2~0.5 mm in a 5%~10% sodium hydroxide aqueous solution, loading a 2~3 V DC power supply, and obtaining a needle-shaped W wire tip.

9. The method for in-situ measurement of mechanical properties and microstructure of metal materials according to claim 8, characterized in that: Based on a W wire substrate, a method for loading and encapsulating a nanometal sample between a plurality of carbon materials using micromanipulation technology to obtain an isostatic pressing device based on the W wire includes: Installing the W wire tip and carbon material into a micromanipulation system; The carbon material is mounted on the tip of the W wire using a manipulator of a micromanipulation system; Load current to weld the carbon material to the tip of the W wire to obtain a carbon material / W wire sample. Using a manipulator of a micromanipulation system, the metal sample is transferred to the carbon material / W wire sample to obtain a metal / carbon material / W wire sample; A second carbon material is mounted on the metal / carbon material / W wire sample using a micromanipulator, and an electric current is applied to seal the metal sample between the two carbon materials to obtain an isostatic pressing device with the W wire as the substrate, wherein the current parameter is: 100~500 mA.

10. The method for in-situ measurement of mechanical properties and microstructure of metal materials according to claim 5, characterized in that: The isostatic pressing device based on W wire is transferred to the in-situ probe rod of the transmission electron microscope. The side wall of the carbon material is squeezed by the probe, and a controllable isostatic pressure is applied to the metal sample in the isostatic pressing environment, thereby realizing the in-situ isostatic pressure mechanical performance test and atomic-level structural characterization of the metal sample in the transmission electron microscope.

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