CN113588699A - SEM-DIC nano speckle preparation method for material micro-area local strain field measurement - Google Patents
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Abstract
The invention relates to a preparation method of SEM-DIC nano speckles for measuring a local strain field of a material micro-area. The speckle material and equipment used in the method comprise nano powder (1), a dispersing agent (3), an ultrasonic cleaning machine (2), a dropper (8) and a substrate material (9). Mixing nano powder with different proportions with a dispersing agent, uniformly dispersing by utilizing ultrasonic, taking a part of the dispersed mixed solution as the mixed solution of speckles, then preparing the nano speckles with high dispersibility, wherein the nano speckles prepared according to the particle size of the nano powder and the concentration of the mixed solution are different and can be used for strain measurement of a field of view of 100 Mum multiplied by 100 Mum to 10 Mum multiplied by 10 Mum under SEM-DIC. The method disclosed by the invention is simple in principle and strong in operability, and the high-precision measurement of the displacement field and the deformation field of the test piece from room temperature to 1200 ℃ under the thermal coupling can be realized by utilizing the cooperation of the in-situ loading platform under the SEM and the high-temperature environment box.
Description
Technical Field
The invention relates to the field of experimental solid mechanics, in particular to a displacement and deformation measuring method for a micro-area full field under a high-resolution SEM under the action of force and thermal coupling, which is applied to high-resolution SEM imaging and DIC measurement in various fields such as aerospace, high-temperature ceramic matrix composite materials, high-temperature alloys and the like to measure the shape, displacement and strain from room temperature to high temperature of 1200 ℃.
Background
Speckle, a key technology in Digital Image Correlation (DIC), is usually applied by spraying white or black paint with a spray gun or a pen to form a contrast spot between black and white on the surface of a sample. When the sample surface is illuminated with white light or monochromatic light (e.g., blue or UV light), a randomly gray-scale image is obtained. The spray gun spraying method is mainly used for preparing macroscale speckles from millimeters to centimeters, and in addition, in material increase speckles, spin coating, a compressed air technology, nanofilm reconstruction, nanoparticle self-assembly, Focused Ion Beam (FIB), photoetching technology and the like are applied to preparing the speckles in a micro-nano scale. In the preparation of the material reducing speckle, scratch, abrasion, chemical corrosion and focused ion beam milling are mainly used for preparing the micro-scale speckle.
Spray gun spraying is the most common method for making large-size speckles. During the speckle size distribution preparation, the nozzle diameter, the distance between the substrate and the nozzle, the gas pressure, and the solution viscosity affect the speckle size distribution. Therefore, preliminary experiments are required to determine speckle preparation parameters. Although speckles produced by spraying and spray gun are cheap and easy to operate, parameters such as raw material powder granularity, liquid viscosity, spraying distance, air pressure and the like need to be determined in advance. Jonnagaddada et al first used the compressed air technique to make micro-scale speckles. Karanjgaokar and the like utilize a compressed air technology to manufacture submicron speckles at 110 ℃, and carry out full-field strain measurement on a gold film in a stretching experiment process. Padilla and his collaborators produced l μm speckle of silicon particles on a surface area of grade 702 zircon with a resolution of 1.2 μm/pixel. Casperso et al studied the problem of fatigue crack propagation and crack closure at 650 ℃ for Hastelloy X with speckles of 1-5 μm silicon particles. Pataky et al studied the non-uniform strain field of Haynes 230 using DIC. Using 0.3 μm Al2O3The powder was subjected to a speckle pattern using a spin coating method at 800 ℃ with a digital image resolution of 0.175 μm/pixel. Despite the use of compressed airTechnically, speckle consistency can be achieved without fear of random large spots, but because speckles adhere to the sample by van der waals forces and electrostatic charges, at higher temperatures (e.g., above 1000 ℃), the stability of the speckles at the substrate surface needs to be considered and more tests performed.
Nanofilm reconstruction is a method for producing high density speckle. The first time Luo et al systematically investigated the remodeling of gold films (<20nm) by condensable vapors exposed to volatile solvents. The morphology of the metal film is controlled by selecting the initial film thickness, exposure time and substrate temperature. Using this method, the speckles were produced on 50-500 nm polymer and metal materials by Scrivens et al. The study analyzed the effect of exposure time, coating thickness, temperature and chemical vapor type on coating performance. Li et al prepared speckles with a characteristic size of 100-150 nm on an aluminum slide using a nanofilm reconstruction technique. The thermal strain of Al-2024-T3 was measured by SEM-DIC to verify the effectiveness of the speckle pattern. Recently, Di gioaccchino et al developed a new device to make gold speckles by steam assisted remodeling. The size of the nanoscale speckle is 30-150 nm, and a deformation field under the sliding band scale shows the potential of a nanofilm reconstruction technology in a drawing experiment of 304L stainless steel. The nano-film reconstruction has the advantages of controllable particle morphology and regeneration, but is time-consuming and inefficient.
Electron Beam Lithography (EBL) or ultraviolet lithography is mainly used to manufacture integrated circuit chips and micro-scale devices. In DIC, photolithography is used in conjunction with magnified imaging methods (SEM, STEM, AFM) to generate random speckle at micro/nano-scale on the surface of a sample to understand the effect of microstructure (grain boundaries, secondary phases, defects, etc.) on the macroscopic response of the material. Li et al prepared 150-500 nm speckles on aluminum and silicon using ELT. LabView software is used for controlling the motion process of the electron beam, so that the etching time is greatly shortened. Tanaka et al imaged micro/nano-scale random speckles made by photolithography using back-scattered electron imaging (BSEI) under SEM. Scrivens et al prepared 2-20 μm gold, silver or other metal speckles by UV lithography. While ELT is substrate independent, repeatable and programmable, its high cost, and due to its working distance sensitivity, is not suitable for non-planar substrates. Furthermore, it is time consuming and expensive.
Focused Ion Beam (FIB) technology was developed primarily in the late 70 s and early 80 s. Recently, FIB milling and product techniques have been combined with SEM for use in micro-scale DIC deformation measurements. Sebastiani et al prepared periodic holes as speckles by FIB milling techniques. Any shape can be etched by scanning the beam across the substrate, and Li et al prepared speckle on silicon wafers and amorphous silicon carbide surfaces by selecting the best template, appropriate FIB magnification, etch time and ion beam current. Zhu et al studied the influencing parameters of speckle quality, total deposition time, ion beam current density and deposition speckle dwell time. The residual stress distribution of the laser impact on the glass surface is successfully measured, and the effectiveness of speckle is verified. Although the FIB mapping method is repeatable, substrate independent and speckle position controllable, it is expensive and the sample surface is prone to damage.
In addition to the speckle preparation methods described above, extraction of material from the sample surface, including scratching and rubbing, is also used to prepare speckles. The alloy surface was ground using silicon carbide abrasive paper by Grant et al to obtain 10 μm speckles. Dong et Al prepared 1 μm/pixel speckle by scratch method and measured polycrystalline Al2O3A coefficient of thermal expansion of 1400 ℃ is achieved. The scraping or abrading technique is simple and cheap, does not require speckle material, and can produce macro/micro-sized speckles. Measurements can also be made at elevated temperatures depending on the sample material. However, surface damage and residual stress are caused. In addition, once scratching or abrasion failure occurs, the sample is wasted.
In conclusion, most of the micro-scale speckle preparation methods have complex processes and high cost, and the initial parameter search requires a large investment in time and money, so that a low-cost and easy-to-operate micro-nano speckle preparation method is urgently needed to meet the requirement of high-resolution SEM-DIC measurement.
Disclosure of Invention
In order to solve the problems of high cost, high investment and large amount of parameter exploration in the prior art in micro-nano speckle preparation, the invention provides a SEM-DIC nano speckle preparation method for material micro-area local strain field measurement, and the method is low in cost, strong in operability, high-temperature resistant and capable of realizing strain measurement of a 100-10-mum-100-10-mum field under a micro area by combining with a high-resolution SEM.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparing SEM-DIC nano speckle used for measuring the local strain field of a material micro-area comprises nano powder, a dispersing agent, an ultrasonic cleaning machine, a dropper and a substrate material. Wherein the nano powder comprises nano carbon powder and nano Al2O3Powder and the like used as speckle raw materials; the dispersing agent comprises absolute ethyl alcohol, deionized water, PVP and the like and is used for dispersing the nano powder; the ultrasonic cleaning machine is used for generating mechanical vibration and dispersing the mixed liquid of the nano powder and the dispersing agent; the dropper is used for quantitatively taking out the supernatant to form a new speckle solution; the substrate material is used to test whether the resulting speckle is usable. Standing for forming mixed liquor in different states, and removing lower-layer mixed liquor in which large agglomerated particles sink under the action of gravity; the resulting speckles are used to measure the micro-zone strain field of the substrate material under a high resolution SEM.
Further, the nano powder is nano carbon powder and nano Al2O3Powder, nano-graphene and other different powders, and powder conducting under SEM, such as nano-carbon powder and the like.
Further, the different dispersants correspond to different nano-powders, for example, the dispersant of nano-graphene is deionized water, and nano-Al is2O3The dispersant of the powder is polyethylene glycol, and the dispersant of the nano carbon powder is absolute ethyl alcohol.
Further, the supernatant liquid needs to be left standing for different times.
Further, the strain calculation method is a Digital Image Correlation (DIC) based method.
A preparation method of SEM-DIC nano speckles for measuring a local strain field of a material micro-area comprises the following steps:
1) mixing nano powder with a certain mass and a dispersing agent, and putting the mixture into a beaker; further mixing the carbon powder and the absolute ethyl alcohol in a ratio of 0.02-0.05g of nano carbon powder and 60-75mL of absolute ethyl alcohol;
2) dispersing the mixed solution in an ultrasonic cleaning machine for 30-60 min;
3) standing the dispersed mixed solution for 24h, 144h, 720h and other different times;
4) taking the maximum 0.2ml of the supernatant after standing by using a 0.2ml dropper, and dripping the supernatant into a beaker to form new mixed liquid; the new mixed solution is supernatant of any one of the mixed solutions which are kept standing for different time, or mixture of supernatant of any several of the mixed solutions, for example, supernatant of 24h, 144h5 and 720h is taken to form new mixed solution.
5) Putting the substrate material into the new mixed solution, performing ultrasonic dispersion for 30-60 min by an ultrasonic cleaning machine, taking out the substrate material, and performing dispersant evaporation;
6) obtaining uniformly dispersed nano speckles, and measuring a micro-area strain field of the substrate material under SEM by combining DIC;
7) the invention adopts nano powder and can carry out local measurement in the range of 100 Mum multiplied by 100 Mum to 10 Mum multiplied by 10 Mum in combination with high resolution SEM; the nano carbon powder has better conductivity under SEM, and can be particularly used for measuring ceramic matrix composite materials; and the supernatant liquor after standing is used as the dispersion mixed liquor again, so that no overlarge particles are ensured, and the random distribution of the speckle particles without large particles is met. The nano carbon powder is adopted, and the ultrasonic dispersion mode is adopted, so that the advantage of low cost is obvious;
the invention relates to an application of a preparation method of SEM-DIC nano speckles for measuring a local strain field of a material micro-area, which is used for carrying out non-contact and high-precision measurement on full-field deformation of aerospace materials such as ceramic composite materials and high-temperature alloys caused by force and heat load in room temperature and high-temperature environments.
The invention has the beneficial effects that:
1. the adoption of the nano carbon powder can ensure the electric conduction under SEM and simultaneously the white spots and the substrate material form gray contrast; the nano carbon powder is adopted, so that the SEM + EBSD material can be simultaneously analyzed, and the base material is not influenced. By using Al2O3Can meet the requirement of in-situ heat below 1200 DEG CAnd (4) performing high-resolution SEM-DIC measurement in a force coupling state.
2. The method adopts the anhydrous ethanol capable of volatilizing naturally as a dispersing agent, and does not add extra heating or other treatment to the speckle distribution;
3. the invention adopts a method of dispersing nano particles to prepare nano speckles. The method of selecting the upper suspension which is kept standing after the mechanical vibration physical dispersion and then carrying out the ultrasonic dispersion for the second time ensures the better dispersibility of the nano particles.
Because the nano particles are easy to agglomerate to form large particles, agglomerated particles which are not dispersed can exist during ultrasonic dispersion, the large agglomerated particles are large, the agglomerated particles can sink under the action of gravity after standing, the dispersed single particles are suspended on the surface layer of the mixed liquid, then a dropper is used for selecting the supernatant, the supernatant and a sample are simultaneously placed into a beaker, after secondary dispersion is carried out by utilizing ultrasonic, the test piece is taken out, and the particles attached to the surface of the sample are speckles.
The supernatant is used as the dispersion liquid again, so that smaller nano particles can be ensured to be reserved, and the uniformity of the particles is improved;
4. the interference of large-particle powder is eliminated by adopting a long-time standing mode;
5. the digital image correlation method is used for accurately tracking displacement and measuring strain, and can obtain a more accurate strain calculation result while maintaining high efficiency.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic of the process of the present invention;
FIG. 2 is an optical image of speckles formed by using nano carbon powder and an anhydrous alcohol dispersant;
wherein a is a field range of 65 μm × 66 μm; b is an optical image with a field range of 13 μm × 13.2 μm.
FIG. 3 is an SEM image of speckles;
FIG. 4 shows Al2O3An optical image of speckle.
In the figure: 1. nano powder; 2. an ultrasonic cleaning machine; 3. a dispersant; 4. standing for 24 h; 5. standing for 144 h; 6. standing for 720 h; 7. mixing the solution; 8. a dropper; 9. supernatant liquor; 10. a base material; 11. evaporating the dispersing agent; 12. nano speckle; 13. nanometer speckle.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example one
As shown in fig. 1, a SEM-DIC nano speckle preparation method for material micro-area local strain field measurement, dispersing a mixed solution of 0.02g of nano carbon powder 1 and 60ml of absolute ethyl alcohol 3 in an ultrasonic cleaning machine 2 for 30min, then taking supernatant liquid 9 which is left standing for 24h 4, 144h5, 720h 6 by using a dropper 8 to form a new mixed solution 0.2ml 7, then putting a substrate material 10 into the new mixed solution 7, performing ultrasonic dispersion for 30min by the ultrasonic cleaning machine 2, then taking out the substrate material, and performing dispersant evaporation 11 to obtain uniformly dispersed nano speckles 12 and 13; the nano powder 1 is used as a raw material for speckles 12 and 13; the ultrasonic cleaning machine 2 is used for mechanically dispersing the nano speckle powder 1; the dispersing agent 3 is used for forming suspension and dispersing nano powder; the 4, 5 and 6 are used for forming mixed liquor of which the upper layer is kept still for different time, and removing lower mixed liquor of which the agglomerated particles are greatly sunk under the action of gravity; the dropper 8 is used for taking out supernatant liquor which is kept stand for different time periods 4, 5 and 6; the supernatant liquid 9 is used for forming a new mixed liquid 7; the speckles 12 and 13 are used to measure the micro-zone strain field of the substrate material 10 under SEM.
Example two
As shown in FIG. 2, an SEM-DIC nanometer speckle used for measuring local strain field of material micro-area (a, b are different field ranges of 65 μm 66 μm and 13 μm 13.2 μm), a mixed solution of 0.05g of nanometer carbon powder and 75mL of absolute ethyl alcohol 3 is dispersed in an ultrasonic cleaning machine 2 for 60min, then 0.1 μ L of supernatant liquid which is kept still for 480h is taken by a 0.2mL dropper 8 and directly dripped on the surface of a sample 10, and when the dispersing agent 3 is naturally volatilized, speckles 12 and 13 are formed for measuring the micro-area strain field of a base material 10 under SEM.
EXAMPLE III
As shown in fig. 3, in a SEM-DIC nano speckle preparation method for local strain field measurement in a material micro-area (51.7 μm × 52.6 μm), a mixed solution of 0.02g of nano carbon powder 1 and 60mL of absolute ethyl alcohol 3 in a certain mass is dispersed in an ultrasonic cleaning machine 2 for 30min, then 0.2mL of supernatant which is stood for 480h is taken by a dropper 8 to form a new mixed solution 7, then a substrate material 10 is put into the new mixed solution 7, and is ultrasonically dispersed for 60min by the ultrasonic cleaning machine 2, then the substrate material is taken out, and a dispersing agent is evaporated 11 to obtain uniformly dispersed nano speckles 12 and 13; the nano powder 1 is used as a raw material for speckles 12 and 13; the ultrasonic cleaning machine 2 is used for mechanically dispersing the nano speckle powder 1; the dispersing agent 3 is used for forming suspension and dispersing nano powder; the dropper 8 is used for taking out supernatant liquor which is kept stand for different time periods 4, 5 and 6; the supernatant liquid 9 is used for forming a new mixed liquid 7; the speckles 12 and 13 are used to measure the micro-zone strain field of the substrate material 10 under SEM.
Example four
As shown in FIG. 4, a method for preparing DIC nano speckle for measuring local strain field of micro region (481 μm × 489 μm) of material comprises mixing Al 0.2g with certain mass2O3Pouring the powder and 0.006g of polyethylene glycol into 100ml of deionized water, dispersing the mixed solution in an ultrasonic cleaning machine 2 for 30min, taking 0.1 mu l of supernatant which is kept stand for 24h by using a 0.2ml dropper 8, directly dripping the supernatant on the surface of a sample 10, and forming speckles 12 and 13 for measuring the micro-area strain field of the substrate material 10 under SEM after the dispersing agent 3 is naturally volatilized.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. A SEM-DIC nanometer speckle preparation method for measuring a local strain field of a material micro-area is characterized by comprising the following steps: the speckle material and equipment used in the preparation method of the nanometer speckle comprise nanometer powder, a dispersing agent, an ultrasonic cleaning machine, a dropper and a substrate material; the preparation method comprises the following steps:
1) mixing the nano powder with a dispersing agent and putting the mixture into a beaker to form a mixed solution;
2) dispersing the mixed solution in an ultrasonic cleaning machine for 30-60 min;
3) placing the dispersed mixed solution in different containers to stand for different times respectively, wherein the time is at least 24 hours;
4) taking 0.1 mu L-0.2ml of supernatant after standing, wherein the supernatant is any one of mixed solutions which are stood for different time;
5) directly dripping the supernatant on the surface of the substrate material, or putting the substrate material into the supernatant, ultrasonically dispersing for 30-60 min by an ultrasonic cleaning machine, and then taking out the substrate material;
6) evaporating the dispersing agent;
7) and acquiring uniformly dispersed nano speckles, and combining DIC (digital image computer) to measure the micro-area strain field of the substrate material under SEM (scanning electron microscope).
2. The SEM-DIC nanospeckle preparation method for local strain field measurement of material micro-regions according to claim 1, wherein the method comprises the following steps: the nanometer powder is powder suitable for high temperature environment measurement or powder conductive under SEM, such as nanometer carbon powder and nanometer Al2O3Powder, nano graphene powder.
3. The SEM-DIC nanospeckle preparation method for local strain field measurement of material micro-regions according to claim 1, wherein the method comprises the following steps: the dispersing agent is absolute ethyl alcohol or deionized water.
4. The SEM-DIC nanospeckle preparation method for local strain field measurement of material micro-regions according to claim 1, wherein the method comprises the following steps: the ultrasonic dispersion is to utilize an ultrasonic cleaning machine to carry out vibration dispersion on the dispersing agent and the nano powder.
5. The SEM-DIC nanospeckle preparation method for local strain field measurement of material micro-regions according to claim 1, wherein the method comprises the following steps: the substrate material is the material to be measured.
6. The SEM-DIC nanospeckle preparation method for local strain field measurement of material micro-regions according to claim 1, wherein the method comprises the following steps: the new mixed solution is formed by dripping supernatant liquid taken out by a dropper into a new beaker.
7. The SEM-DIC nanospeckle preparation method for local strain field measurement of material micro-regions according to claim 1, wherein the method comprises the following steps: the nano speckles are prepared by a drop coating method.
8. Use of the SEM-DIC nanospecks preparation method for local strain field measurement of material micro-regions according to any of claims 1-7 for non-contact, high precision measurement of full-field deformation of aerospace materials such as ceramic composites, superalloys caused by force, thermal load at room temperature, high temperature environment.
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| CN115872742A (en) * | 2022-12-14 | 2023-03-31 | 北京航空航天大学 | Preparation method of DIC speckle at room temperature of-3000 DEG C |
| CN116144263A (en) * | 2023-04-17 | 2023-05-23 | 兰州大学 | Preparation process of low-temperature large-deformation speckle, speckle and optical path observation system |
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| CN115872742B (en) * | 2022-12-14 | 2023-08-11 | 北京航空航天大学 | Preparation method of DIC speckle at room temperature-3000 DEG C |
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