CN110926974B - Method for testing mechanical property of small sample - Google Patents
Method for testing mechanical property of small sample Download PDFInfo
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- CN110926974B CN110926974B CN201911187125.9A CN201911187125A CN110926974B CN 110926974 B CN110926974 B CN 110926974B CN 201911187125 A CN201911187125 A CN 201911187125A CN 110926974 B CN110926974 B CN 110926974B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/32—Investigating strength properties of solid materials by application of mechanical stress by applying repeated or pulsating forces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0676—Force, weight, load, energy, speed or acceleration
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Abstract
The invention provides a method for testing mechanical properties of a small sample, which comprises the following steps: preparing a micro-nano mechanical sample in a part of area of a macroscopic sample by using a micro-nano processing technology, and ensuring that a clamping end of the micro-nano mechanical sample is connected with the macroscopic sample; and loading the processed macroscopic sample by a mechanical testing instrument, wherein the micro-nano scale mechanical sample is subjected to the action of force in the same direction as the loading direction of the macroscopic sample due to the deformation of the macroscopic sample, and further the mechanical performance test of the micro-nano scale sample is realized. The testing method provided by the invention realizes the mechanical property test of the micro-nano-scale sample by using macroscopic mechanical testing equipment such as a universal testing machine and the like by utilizing the connection between the micro-nano-scale sample and the macroscopic sample and loading the macroscopic sample.
Description
Technical Field
The invention relates to the field of mechanical property testing, and further relates to a method for testing the mechanical property of a small sample.
Background
The small sample mechanical property test comprises the mechanical property tests of nano indentation, stretching, compression, bending and the like of the small-scale sample. The testing technology can not only characterize the mechanical behavior of the material from millimeter scale to micrometer scale and nanometer scale, but also realize the directional research of specific microstructure structure in the material, such as the second equality in a crystal boundary and a matrix, and further reveal the influence mechanism of the microstructure on the macroscopic mechanical behavior of the material. Therefore, the mechanical property test of small samples is widely applied to advanced materials with sample size strictly limited by preparation conditions, such as two-dimensional materials, thin film materials, nano-structure materials and the like.
However, the types of mechanical property tests of current small samples are limited to indentation, compression, tension and bending properties, and it is difficult to realize fatigue tests which have important reference significance for engineering applications. Moreover, the current experimental technology can only realize mechanical testing at normal temperature, and is difficult to test at different temperatures. Meanwhile, the mechanical property test of small samples requires that force and displacement sensors configured by the equipment have microscopic and even nanoscopic resolution and precision, and the micro-nano mechanical test equipment capable of achieving the indexes is high in price. In addition, the test also needs effective connection between the sample and the micro-nano mechanical test equipment, so that the sample and related parts in the equipment need to be subjected to complex micro-nano processing by means of focused ion beams, and the experiment cost is further increased.
Disclosure of Invention
Technical problem to be solved
In view of the above, the present invention provides a method for testing mechanical properties of a small sample, so as to at least partially solve the above technical problems.
(II) technical scheme
In order to achieve the above object, the present invention provides a method for testing mechanical properties of a small sample, which comprises:
preparing a micro-nano mechanical sample in a part of area of a macroscopic sample by using a micro-nano processing technology, and ensuring that a clamping end of the micro-nano mechanical sample is connected with the macroscopic sample;
and loading the processed macroscopic sample by a mechanical testing instrument, wherein the micro-nano scale mechanical sample is subjected to the action of force in the same direction as the loading direction of the macroscopic sample due to the deformation of the macroscopic sample, and further the mechanical performance test of the micro-nano scale sample is realized.
In a further embodiment, the micro-nano processing technique comprises at least one of: focused ion beam technology, optical projection exposure, electron beam exposure, and laser etching.
In a further embodiment, a mechanical testing instrument loads a processed macro sample, and a micro-nano scale mechanical sample is subjected to the same force effect as the macro sample in the loading direction due to the deformation of the macro sample, so that the mechanical performance test of the micro-nano scale sample is realized, and the method comprises the following steps:
loading a macroscopic sample to perform a mechanical experiment, and determining the mechanical property of the macroscopic sample; simulating and determining the corresponding relation between the stress of the macroscopic sample and the stress of the micro-nano scale sample according to the overall shape of the macroscopic sample and the micro-nano size of a partial area; and determining the mechanical property of the micro-nano scale sample according to the mechanical property of the macro sample and the corresponding relation.
In a further embodiment, the mechanical property test of the micro-nano scale sample further comprises: when the macroscopic sample is loaded, the environmental temperature of the macroscopic sample is changed to carry out the experiment at the set temperature.
In a further embodiment, the mechanical property test of the micro-nano scale sample further comprises: when the mechanical experiment is carried out on the macroscopic sample, the atmosphere of the macroscopic sample is changed to carry out the experiment under the set atmosphere.
In a further embodiment, the shape of the macroscopic sample is a geometric shape that is symmetrical about a set axis.
In further embodiments, the mechanical property test comprises at least one of: tensile, compressive, flexural, fracture toughness, fatigue and torsional properties.
In a further embodiment, the partial area micro-nano scale sample is at the edge of the upper surface, the central part of the upper surface, the edge of the side surface or the center of the macro sample.
(III) advantageous effects
According to the method for testing the mechanical property of the small sample, the micro-nano-scale sample is effectively connected with the macro sample, the micro-nano-scale sample is loaded by means of load transfer through loading the macro sample, and the mechanical property of the micro-nano-scale sample is tested by using macro mechanical testing equipment such as a universal testing machine, so that the micro-nano-scale sample is prevented from being mechanically tested by using the micro-nano mechanical testing equipment;
the method for testing the mechanical property of the small sample can circularly load the micro-nano-scale sample, can also install the environment box capable of realizing temperature and atmosphere regulation and control at the periphery of a mechanical testing instrument, further realizes the fatigue test of the micro-nano-scale sample and various mechanical property tests at different temperatures and under different atmospheres, is not limited by material types, and has universality.
Drawings
FIG. 1 is a three-dimensional schematic of a macroscopic sample of an embodiment of the present invention.
Fig. 2A and fig. 2B are a three-dimensional schematic diagram and a top-view schematic diagram of the micro-nano scale sample partially shown in fig. 1, respectively.
Fig. 3 is a schematic diagram of stress simulation of the micro-nano scale sample in fig. 2A.
FIG. 4 is a flowchart of a method for testing mechanical properties of a small sample according to an embodiment of the present invention.
Detailed Description
In the present invention, the technical terms referred to have the following meanings:
macroscopic sample: samples with sample sizes on the millimeter scale and above.
Small samples: particularly samples having three dimensional dimensions of less than a millimeter, typically from micrometers to nanometers. Such as two-dimensional materials, thin-film materials, and/or nanostructured materials.
And (3) testing the mechanical property of the small sample: mechanical property tests for small samples are collectively referred to as small sample mechanical property tests, and include tensile, compression, bending, fracture toughness, fatigue, torsion and the like.
Fracture toughness: characterizing the ability of the material to resist crack propagation; the higher the fracture toughness value, the stronger the material's resistance to crack propagation.
Micro-nano mechanical testing equipment: force sensors and displacement sensors have devices with microscopic, nanoscopic resolution and accuracy.
A mechanical testing instrument: the device for realizing mechanical tests of tension, compression, bending, torsion and the like on a macro scale comprises a universal testing machine, a tension table and the like.
Micro-nano processing technology: the technology for processing and preparing the micro-nano scale component or device comprises a focused ion beam technology, optical projection exposure, electron beam exposure, laser etching and the like.
DIC (digital image correlation) technology: the method is a non-contact deformation measurement technology, and can accurately represent the deformation of a sample in a mechanical experiment.
GPa: unit of stress magnitude, 1GPa to 1 x 109Pa
Micro-nano scale: the sample size is smaller than the millimeter size scale, typically from tens of micrometers to nanometers.
The embodiment of the invention aims to provide a universal method for testing the mechanical property of a small sample, which can test the mechanical behavior of the sample such as stretching, compression, bending and the like, solve the problem that the fatigue test cannot be carried out on a micro-nano scale and the mechanical property test cannot be carried out at different temperatures at present, avoid the serious dependence of the test on micro-nano mechanical test equipment, and realize the purpose of representing the mechanical behavior of the micro-nano scale sample by using a universal testing machine.
The design basic principle of the embodiment of the invention is that a micro-nano scale sample is prepared on a macro sample by utilizing a micro-nano processing technology, and then the macro sample is loaded through a universal testing machine so as to realize the test of the tensile, bending, compression and fracture toughness properties of the micro-nano scale sample; particularly, when a cyclic load is applied to a macroscopic sample, the fatigue mechanical property test of the micro-nano scale sample can be realized; meanwhile, an environment box or a high-temperature furnace can be installed on the universal testing machine, and then mechanical tests at different temperatures and under different atmospheres are realized. On the other hand, the testing method provided by the embodiment of the invention needs to combine numerical simulation or theoretical model to characterize the stress state of the micro-nano scale sample, and needs to combine DIC technology or other effective methods to characterize the strain field of the micro-nano scale sample.
Referring to fig. 4, an embodiment of the present invention provides a method for testing mechanical properties of a small sample, where the method includes:
s100: preparing a micro-nano mechanical sample in a part of area of a macroscopic sample by using a micro-nano processing technology, and ensuring that the micro-nano mechanical sample is connected with the macroscopic sample (for example, a clamping end of the micro-nano mechanical sample is connected with the macroscopic sample);
s200: and loading the processed macroscopic sample through a mechanical testing instrument so as to realize the mechanical property test of the micro-nano scale sample.
The micro-nano processing technology comprises at least one of the following steps: focused ion beam technology, optical projection exposure, electron beam exposure, and laser etching.
In step S200, the machined macro sample is loaded by a mechanical testing instrument, and the micro-nano scale mechanical sample is subjected to the same force as the macro sample loading direction due to the deformation of the macro sample, so as to realize the mechanical property test of the micro-nano scale sample, which specifically includes:
loading a macroscopic sample to perform a mechanical experiment, and determining the mechanical property of the macroscopic sample;
simulating and determining the corresponding relation between the stress of the macroscopic sample and the stress of the micro-nano scale sample according to the overall shape of the macroscopic sample and the micro-nano size of a partial area;
and determining the mechanical property of the micro-nano scale sample according to the mechanical property of the macro sample and the corresponding relation.
In some embodiments, in step S200, for the mechanical property test of the micro-nano scale sample, the method further includes: when the mechanical experiment is carried out on the macroscopic sample, the temperature of the macroscopic sample is changed to carry out the experiment at the set temperature.
In some embodiments, in step S200, for the mechanical property test of the micro-nano scale sample, the method further includes: when the mechanical experiment is carried out on the macroscopic sample, the atmosphere of the macroscopic sample is changed to carry out the experiment under the set atmosphere.
In some embodiments, the shape of the macroscopic sample is a geometric shape that is symmetric about a set axis.
In some embodiments, the mechanical property test comprises at least one of: tensile, compressive, flexural, fracture toughness, fatigue and torsional properties.
In some embodiments, the partial area micro-nano scale sample is at the edge of the upper surface, the central part of the upper surface, the edge of the side surface or the center of the macro sample.
The invention will be further described with reference to specific examples, but it is to be understood that the following specific steps are illustrative of the invention and are not to be construed as limiting the invention.
The method for testing the mechanical property of the small sample of the specific embodiment can comprise the following steps:
the method comprises the following steps: preparing a macro sample by using machining methods such as electrospark wire-electrode cutting and the like, polishing the surface of the macro sample, and preparing a micro-nano scale sample by using a micro-nano machining technology, wherein the size of the micro-nano scale sample is shown in figure 1. The geometric shape of the macroscopic sample is not limited to the dog bone shape shown in fig. 1, but can be other geometric shapes convenient for mechanical testing; meanwhile, the position of the micro-nano scale sample on the macro sample is not limited to the edge of the upper surface shown in fig. 1, and can also be positioned at the center of the upper surface, the edge of the side surface and the center. In addition, the macro-scale sample and the micro-nano-scale sample are not limited to be the same material, for example, the micro-nano-scale sample can be a film, a coating and other materials, and the macro-scale sample is a substrate for bearing the film or the coating.
Step two: the macroscopic sample is clamped on a mechanical tester, and mechanical properties such as stretching, compression, bending, fatigue and the like can be tested according to the loading type. The stress level in the macro sample can be obtained according to a formula (stress is force/area), and the stress level of the micro-nano scale sample needs to be given through numerical simulation or a theoretical model. At the same time, the strain in the macroscopic sample can be given using DIC techniques or otherwise. In addition, an environment box can be additionally arranged on the universal testing machine to carry out high and low temperature experiments. The mechanical testing device in the invention is not limited to a universal testing machine, and can also be a mechanical device which can be integrated in an optical mirror device or an electron microscope device, such as a stretching table.
And aiming at the calculation of the stress level in the micro-nano scale sample related in the step two, the invention provides an example through finite element simulation and refers to the example.
For the above loading conditions, uniaxial stretching, with tungsten as the material, Young's modulus 410GPa, Poisson's ratio 0.28, macroscopic strain 0.2%; the geometric dimensions of the micro-nano scale sample are shown in figures 2A and 2B. Simulation results show that the average stress level of the macro sample is 825MPa, and the stress level of the parallel section of the micro-nano scale sample is 2080MPa, which is shown in figure 3.
Through the embodiment, the purpose of carrying out fatigue performance test on the micro-nano scale sample by preparing the micro-nano scale mechanical sample on the macro sample by utilizing the micro-nano processing technology and carrying out cyclic loading on the macro sample is provided. The test method provided does not depend on micro-nano mechanical test equipment, and the test can be realized through a universal tester. Meanwhile, an environment box or a high-temperature furnace can be installed on the universal testing machine, and then mechanical tests at different temperatures and under different atmospheres are realized. The technical scheme provided by the embodiment of the invention has universality, is not limited by the type of the material, and can realize the tests of tensile, compression, bending, fracture toughness and bending mechanical properties.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for testing mechanical properties of a small sample comprises the following steps:
preparing a micro-nano scale sample in a part of area of a macroscopic sample by using a micro-nano processing technology, and ensuring the connection of the micro-nano scale sample and the macroscopic sample;
the method comprises the following steps of loading a processed macroscopic sample through a mechanical testing instrument for testing the mechanical property of the macroscopic sample, obtaining the stress state of the micro-nano scale sample by combining numerical simulation or a theoretical model under the action of the force in the same direction as the loading direction of the macroscopic sample due to the deformation of the micro-nano scale sample, and further realizing the mechanical property test of the micro-nano scale sample, wherein the mechanical testing instrument comprises:
loading a macroscopic sample to perform a mechanical experiment, and determining the mechanical property of the macroscopic sample;
simulating and determining the corresponding relation between the stress of the macroscopic sample and the stress of the micro-nano scale sample according to the overall shape of the macroscopic sample and the micro-nano size of a partial area;
and determining the mechanical property of the micro-nano scale sample according to the mechanical property of the macro sample and the corresponding relation.
2. The method according to claim 1, wherein the micro-nano machining technology comprises at least one of:
focused ion beam technology, optical projection exposure, electron beam exposure, and laser etching.
3. The method according to claim 1, wherein the mechanical property test of the micro-nano scale sample further comprises:
when the macroscopic sample is loaded, the environmental temperature of the macroscopic sample is changed to carry out the experiment at the set temperature.
4. The method according to claim 1, wherein the mechanical property test of the micro-nano scale sample further comprises:
when the mechanical experiment is carried out on the macroscopic sample, the atmosphere of the macroscopic sample is changed to carry out the experiment under the set atmosphere.
5. The method of claim 1, wherein the shape of the macroscopic sample is a geometric shape that is symmetric about a set axis.
6. The method of claim 1, wherein the mechanical property test comprises at least one of:
tensile, compressive, flexural, fracture toughness, fatigue and torsional properties.
7. The method according to claim 1, wherein the partial area micro-nano scale sample is at the edge of the upper surface, the central part of the upper surface, the edge of the side surface or the center of the macro sample.
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| CN202057549U (en) * | 2011-04-29 | 2011-11-30 | 吉林大学 | Mechanics performance testing platform for cross-scale micro nano-scale in-situ combined loads |
| CN202195986U (en) * | 2011-09-05 | 2012-04-18 | 吉林大学 | Scale-span micro nanometer in situ tension mechanic performance testing device |
| US9535086B2 (en) * | 2014-06-24 | 2017-01-03 | Femtotools Ag | Interface of a microfabricated scanning force sensor for combined force and position sensing |
| CN104764660A (en) * | 2015-03-29 | 2015-07-08 | 北京工业大学 | Thermal-driving uniaxial drawing/compressive deformation device for scanning/transmission electron microscope |
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| CN107703012B (en) * | 2017-10-20 | 2024-02-02 | 吉林大学 | Variable-temperature indexable micro-nano indentation testing device |
| CN110044753B (en) * | 2019-05-21 | 2022-04-01 | 吉林大学 | High-temperature micro-nano indentation testing device and method with inert gas protection function |
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