This work was supported by JSPS KAKENHI, grant numbers JP16K17988 and JP16K05996, and by the Cross-Ministerial Strategic Innovation Promotion Program, Unit D66, Innovative Measurement and Analysis for Structural Materials (SIP-IMASM), operated by the cabinet office. The authors are also grateful to Drs. Satoshi Kishimoto and Kimiyoshi Naito at NIMS for their CFRP material.

1. Confirmation of the Micro/Nano-scale Grid on the Specimen
<ol>
	<li>Machining of the Specimen
	<ol>
		<li>Cut the specimen to the size required by the specific loading device used under a microscope (e.g., 1 x 5 x 30 mm3), making the surface to be observed 1.5x greater than the region of interest.</li>
		<li>Polish the specimen surface to be observed (e.g., 1 x 30 mm2), successively using coarse and fine sand paper on an automatic polishing machine (e.g., use SiC foil #320 for 3 min and then #800 for 1 min at 150 rpm and 30 N). Clean the specimen using water after each polishing step.</li>
		<li>Polish the same specimen surface, successively using coarse and fine polishing solutions on the automatic polishing machine (e.g., use DP-Spray P 15 &#181;m for 5 min, P 1 &#181;m for 8 min, and P 0.25 &#181;m for 10 min at 150 rpm and 30 N). Clean the specimen using water after each polishing step.</li>
	</ol>
	</li>
	<li>Fabrication of the Micro/Nano-scale Grid If No Periodic Pattern Exists on the Specimen 
	NOTE: This step can be omitted if a natural periodic pattern exists on the micro/nano scale on the specimen surface. Choose the grid fabrication method from the following: ultraviolet (UV) or heating nanoimprint lithography (NIL)26, electron beam lithography (EBL)2, and focused ion beam (FIB) milling6. 
	NOTE: The grid fabrication process is introduced here, with UV NIL as an example.
	<ol>
		<li>Drop 2 mL of UV resist on the specimen surface using a pipette.</li>
		<li>Coat the resist on the specimen surface using a spin coater at 1,500 rpm for 60 s.</li>
		<li>Press a nanoimprint mold to the resist layer at a pressure of 0.2 MPa. Expose the resist to UV with a wavelength of 375 nm for 30 s.</li>
		<li>Separate the nanoimprint mold from the specimen surface.</li>
	</ol>
	</li>
	<li>Observation of the Grid on the Specimen Using a Microscope
	<ol>
		<li>Coat a platinum or gold layer with a thickness of 3-10 nm on the grid surface using an ion coater (e.g., coating for 30 s at 3 Pa with a sputtering current of 30 mA).</li>
		<li>Put the specimen under a laser scanning microscope (LSM)23. 
		NOTE: Other microscopes can also be used, such as a transmission electron microscope (TEM)5, an atomic force microscope (AFM)12, or a scanning electron microscope (SEM)7.</li>
		<li>Adjust the focus and save one grid image using the microscope by clicking &#34;Capture&#34; and &#34;File | Export | Image File&#34; in the image recording software of the microscope.</li>
	</ol>
	</li>
	<li>Calculation of the Grid Pitch (nm or &#181;m) of the Specimen from the Grid Image
	<ol>
		<li>Calculate the average value of more than 10 grid pitches in the central area of the grid image to avoid the potential influence of the scanning or lens distortion. 
		NOTE: The grid on the specimen can be saved for several days at room temperature.</li>
	</ol>
	</li>
</ol>
2. Acquisition of Grid Images in the Loading Test
<ol>
	<li>Preparation of the Loading Test Under the Microscope
	<ol>
		<li>Fix the specimen to a loading device, such as a tensile, compressive, heating, or electrical loading device, under the microscope. 
		NOTE: If the grid pitch is less than 20 nm, a TEM or AFM should be used. If the grid pitch is 20 nm to 10 &#181;m, an SEM can be used. If the grid pitch is greater than 400 nm, an LSM can be used.</li>
		<li>Set the load speed (e.g.,0.01 mm/s) and the load or displacement incremental step (e.g., 0.5 N/step or 0.024 mm/step) according to the specific requirements. Preset both the load and displacement to zero.</li>
		<li>Make the grid surface in the observation plane. Choose an area of interest under a low magnification by moving or rotating the sample stage of the microscope.</li>
		<li>Select an appropriate magnification by making the grid pitch in the image greater than 1.8&#215; one pixel size. 
		NOTE: Usually, it is better to make the grid pitch in the image greater than 2 pixels. The more pixels one grid pitch corresponds, the higher the accuracy of the deformation measurement, but the smaller the field of view of the measurement.</li>
	</ol>
	</li>
	<li>Collection of Grid Images in the Loading Test
	<ol>
		<li>Save a grid image of the area of interest before loading by clicking &#34;Capture&#34; and &#34;File | Export | Image File&#34; in the image recording software of the microscope.</li>
		<li>Begin to load the specimen in situ onto the microscope by exerting the first load step (e.g., 0.5 N or 0.024 mm) using the operating software of the loading device.</li>
		<li>Record a grid image of the area of interest after the first load step (e.g., at 0.5 N or 0.024 mm) by clicking &#34;Capture&#34; and &#34;File | Export | Image File&#34; in the image recording software of the microscope. Ensure that the magnification and working distance of the microscope remain unchanged.</li>
		<li>Continue to load the specimen by exerting each load step using the loading device. Record the grid image after each load step until the specimen is broken or until a certain value is attained (e.g., load 19 times and record 19 grid images at 1 N, 1.5 N, 2.0 N, &#8230;, 10 N, at intervals of 0.5 N; or at 0.048 mm, 0.072 mm, 0.096 mm, &#8230;, 0.48 mm, at intervals of 0.024 mm). Make sure that the magnification and working distance of the microscope remains unchanged. 
		NOTE: The grid images can be saved for an arbitrarily long period of time.</li>
	</ol>
	</li>
</ol>
3. Generation of Sampling Moir&#233; Fringes before and after Deformation
<ol>
	<li>Estimation of Grid Pitches (pixel) in the Grid Images
	<ol>
		<li>Estimate the grid pitch (unit: pixel) in the grid image before loading by measuring the distance between the centers of two adjacent grid dots in an image processing software (e.g., Microsoft Paint).</li>
		<li>Estimate the grid pitch in the grid image at the maximum load.</li>
	</ol>
	</li>
	<li>Determination of Sampling Pitch (pixel)
	<ol>
		<li>Move to step 3.2.2 when the grid pitches before and after deformation are between 1.8 and 2.5 pixels. Skip to step 3.2.3 when the grid pitches before and after deformation are between 2.4 and 3.6 pixels. Skip to step 3.2.4 when the grid pitches before and after deformation are greater than 3.2 pixels.</li>
		<li>Set the sampling pitch to T = 2 pixels. Skip to step 3.3.</li>
		<li>Set the sampling pitch to T = 3 pixels. Skip to step 3.3.</li>
		<li>Set the sampling pitch T to a positive integer within 0.75x and 1.25x the grid pitches before and after deformation, determined from abundant simulation results22. 
		NOTE: If there are 2 positive integers that meet the requirements in steps 3.2.1 and 3.2.4, it is better to choose the greater integer as the sampling pitch. If there are 3 or more positive integers that meet the requirements, it is better to choose the middle integer, as long as it is a little bit greater than the sampling pitch.</li>
	</ol>
	</li>
	<li>Generation of Sampling Moir&#233; Fringes Before Deformation
	<ol>
		<li>Open the grid image before deformation. Assuming that the x direction is horizontally rightward, the y direction is vertically downward, and the coordinate (0, 0) is at the top-left corner, calculate the image width W in the x direction and the image height H in the y direction. 
		NOTE: The y direction can also be defined as vertically upward.</li>
		<li>Move to step 3.3.3 to generate moir&#233; fringes in the y direction. Skip to step 3.3.7 to generate moir&#233; fringes in the x direction.</li>
		<li>Process the grid image to a grating image using a low-pass filter (LPF). For example, use an FT algorithm to suppress the grating, with a principal direction of x, where the principal direction is defined as the direction perpendicular to the grating lines. Set the filter size to be close to the grid pitch.</li>
		<li>Thin out the grid image by only extracting the gray values in several horizontal lines, with the spacing of the sampling pitch T (T &#8805;2) from y = k pixels (k = 0) (Figure 1) (i.e., only keep the gray values in sampling lines of y = k pixels, y = k+T pixels, &#8230; , y = k + iT pixels, where i is a positive integer). Make the coordinate of the last sampling line, k + iT, less than the image height H.</li>
		<li>Generate a sampling moir&#233; pattern in the y direction by performing full-field intensity interpolation (linear or B-spline) of the image with horizontal sampling lines.</li>
		<li>Generate other T-1 sampling moir&#233; patterns in the y direction by repeating steps 3.3.4 and 3.3.5 T-1 times by changing k at the incremental step of 1 pixel (i.e., shifting the starting point of thinning out to y = k pixels; k = 1, &#8230;, T-1).</li>
		<li>Use the same procedures in steps 3.3.3-3.3.6 to generate T-step spatial phase-shifting sampling moir&#233; patterns in the x direction by changing x to y in step 3.3.3, changing the image height H to the image width W, and changing y to x in steps 3.3.4-3.3.6. 
		NOTE: The sampling pitch in the x direction can be different from that in the y direction.</li>
	</ol>
	</li>
	<li>Generation of Sampling Moir&#233; Fringes After Deformation
	<ol>
		<li>Open all grid images at different loads. Suppose the number of grid images is N.</li>
		<li>Generate N groups of T-step spatial phase-shifting moir&#233; fringes in the y direction by repeating steps 3.3.3-3.3.6 N times.</li>
		<li>Generate N groups of T-step spatial phase-shifting moir&#233; fringes in the x direction by repeating step 3.3.7 N times.</li>
	</ol>
	</li>
</ol>
4. Deformation Measurement of the Specimen in the Loading Test
<ol>
	<li>Determination of the Intensities of Moir&#233; Fringes Before and After Deformation
	<ol>
		<li>Extract the intensities of the T-step moir&#233; fringes before deformation in the y direction in steps 3.3.5 and 3.3.6; determine those moir&#233; intensities in the x direction in step 3.3.7. Describe the T-step (T &#8805;2) moir&#233; intensities before deformation in the j (j = x, y) direction using the following equation23: 
		<img alt="Equation 1" src="/files/ftp_upload/55739/image001.jpg" /> (1) 
		where pj is the grid pitch before deformation in the j (j = x, y) direction, A is the modulated amplitude, and D includes the background and the higher-frequency intensities.</li>
		<li>Extract the intensities of the T-step moir&#233; fringes after deformation in the y direction in step 3.4.2 and determine those moir&#233; intensities in the x direction in step 3.4.3. Describe the T-step (T &#8805; 2) moir&#233; intensities after deformation in the j (j = x, y) direction using the same equation as above (Equation 1) by changing Im,j(k), pj, A, and D to I&#39;m,j(k), p&#39;j, A&#39;, and D&#39;, respectively, where the superscript single quote means after deformation. 
		NOTE: If the sampling pitch is T &#8805; 3 pixels, ignore this step and skip to step 4.3.</li>
	</ol>
	</li>
	<li>&#160;
	<ol>
		<li>Reconstruct multiplication moir&#233; fringes from the multiplicative interference between the two-step sampling moir&#233; intensities (Figure 1a) before deformation using the following equation23 
		<img alt="Equation 2" src="/files/ftp_upload/55739/image002.jpg" /> (2) 
		where Imulti,j stands for the intensity of the reconstructed multiplication moir&#233; fringes in the j ( j = x, y) direction before deformation.</li>
		<li>Process the reconstructed multiplication moir&#233; fringes before deformation using the fringe centering technique24. Assign consecutive integers and half integers fj = [1, 1.5, 2, 2.5, &#8230;] to the fringe orders at the center lines of the reconstructed multiplication moir&#233;. 
		NOTE: If the multiplication moir&#233; fringes are too dense, the fringe orders of the two-step sampling moir&#233; can be determined first (i.e., fj(0) = [1, 0, 2, 0, 3, 0, &#8230;] and fj(1) = [0, 1.5, 0, 2.5, 0, 3.5, &#8230;]). The fringe order of the multiplication moir&#233; fringes will be fj = fj(0) + fj(1) = [1, 1.5, 2, 2.5, 3, 3.5, &#8230;]. The rigid-body displacement will not affect the strain result.</li>
		<li>Measure the relative strain of the specimen before deformation relative to the sampling pitch using the following equations23 
		<img alt="Equation 3" src="/files/ftp_upload/55739/image003.jpg" /> (3) 
		<img alt="Equation 4" src="/files/ftp_upload/55739/image004.jpg" /> (4) 
		where uj_rela and &#949;j_rela represent the relative displacement and the relative strain of the specimen before deformation in the j (j = x, y) direction, respectively, and &#947;xy_rela expresses the relative shear strain before deformation.</li>
		<li>Repeat steps 4.2.1-4.2.3 to determine the relative strains of the specimen after deformation in the x and y directions for N times, changing Imulti,j, Im,j(0), Im,j(1), pj, A, D, uj_rela (j = x, y), &#949;j_rela, and &#947;xy_rela in equations (2)-(4) to I&#39;multi,j, I&#39;m,j(0), I&#39;m,j(1), p&#39;j, A&#39;, D&#39;, u&#39;j_rela (j = x, y), &#949;&#39;j_rela, and &#947;&#39;xy_rela, respectively, where the superscript single quote means after deformation.</li>
		<li>Determine the actual normal strain &#949;j in the j (j = x, y) direction, which is the relative change of the grid pitch and the shear strain, &#947;xy, which is the absolute variation of the grid angle of the specimen caused by the load from the relative strains before and after deformation20. 
		<img alt="Equation 5" src="/files/ftp_upload/55739/image005.jpg" /> (5) 
		<img alt="Equation 6" src="/files/ftp_upload/55739/image006.jpg" /> (6)</li>
	</ol>
	</li>
	<li>Deformation Measurement When the Sampling Pitch is T &#8805; 3 pixels
	<ol>
		<li>Calculate the phase of the sampling moir&#233; fringes in the j (j = x, y) direction before deformation when k = 0 (Figure 1b) using the spatial phase-shifting technique21 
		<img alt="Equation 7" src="/files/ftp_upload/55739/image007.jpg" /> (7)</li>
		<li>Obtain the phase of the sampling moir&#233; fringes in the j (j = x, y) direction after deformation when k =0 by replacing &#966;m,j and Im,j(k) in equation (7) with &#966;&#39;m,j and I&#39;m,j(k), respectively, where the superscript single quote means after deformation. Repeat N times for N loads. 
		NOTE: If there is too much random noise in the phase distributions in steps 4.3.1 and 4.3.2, a sin/cos filter25 can be used to smooth the phases.</li>
		<li>Determine the phase difference of the sampling moir&#233; fringes in the j (j = x, y) direction before and after deformation (i.e.,&#916;&#966;m,j=&#966;&#39;m,j-&#966;m,j).</li>
		<li>Measure the distributions of displacement uj, normal strain &#949;j in the j (j = x, y) direction, and the shear strain &#947;xy of the specimen caused by the load. Use the following equations6,21 
		<img alt="Equation 8" src="/files/ftp_upload/55739/image008.jpg" /> (8) 
		<img alt="Equation 9" src="/files/ftp_upload/55739/image009.jpg" /> (9) 
		<img alt="Equation 10" src="/files/ftp_upload/55739/image010.jpg" /> (10) 
		NOTE: If there is too much noise in the strain distributions, an average smoothing filter can be used, with a filter size smaller than 2 grid pitches.</li>
	</ol>
	</li>
	<li>Result Storage
	<ol>
		<li>Save the data of the moir&#233; fringes, phases (when the sampling pitch is T &#8805;3 pixels), displacements, and strains in the forms of images, such as .tif or .bmp files, and text, such as .txt or .csv files.</li>
	</ol>
	</li>
</ol>

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The authors have nothing to disclose.

In the described technique, one challenging step is the micro/nano-scale grid or grating (abbreviated as grid) fabrication26 if no periodic pattern exists on the specimen. The grid pitch should be uniform before deformation because it is an important parameter for the deformation measurement. If the material is a metal, a metal alloy, or a ceramic, UV or heating nanoimprint lithography (NIL)27, electron beam lithography (EBL)2, focused ion beam (FIB)...

Micro/nano-scale deformation measurements are vitally essential for evaluating the mechanical properties, instability behaviors, residual stresses, and crack occurrences of advanced materials. Since optical techniques are non-contact, full-field, and non-destructive, various optical methods have been developed for deformation measurement during the last few decades. In recent years, the micro/nano-scale deformation measurement techniques mainly include the moir&#233; methods1,2,3,4, geometric phase analysis (GPA)5,6, Fourier transformation (FT), digital image correlation (DIC), and electronic speckle pattern interferometry (ESPI). Among these techniques, GPA and FT are not well suited for complex deformation measurements because multiple frequencies exist. The DIC method is simple but powerless against noise because the deformation carrier is random speckle. Finally, ESPI is strongly sensitive to vibration.
Among micro/nano-scale moir&#233; methods, the most commonly used methods at present are the microscope scanning moir&#233; methods, such as electron scanning moir&#233;7,8,9, laser scanning moir&#233;10,11, and atomic force microscope (AFM) moir&#233;12, and some microscope-based moir&#233; methods, such as the digital/overlapping moir&#233;13,14,15 method and the multiplication/fractional moir&#233; method16,17. The scanning moir&#233; method has many advantages, such as a wide field of view, high resolution, and insensitivity to random noise. However, the traditional scanning moir&#233; method is inconvenient for 2D strain measurements because it is necessary to rotate the sample stage or the scanning direction by 90&#176; and to scan twice to generate moir&#233; fringes in two directions18. Rotation and the dual scanning processes introduce rotation error and take a long time, seriously influencing the measurement accuracy of the 2D strain, especially for the shear strain. Although the temporal phase-shifting technique19,20 can improve the deformation measurement accuracy, it requires time and a special phase-shift device unsuitable for dynamic tests.
The sampling moir&#233; method21,22 has a high accuracy in displacement measurements and is now mainly used for deflection measurements on bridges when automobiles pass. To extend the sampling moir&#233; method to micro/nano-scale 2D strain measurements, a reconstructed multiplication moir&#233; method has been newly developed23 from 2-pixel sampling moir&#233; fringes, in which the measurements are twice as sensitive and the wide field of view of the scanning moir&#233; method is kept. Moreover, the spatial phase-shifting sampling moir&#233; method is also developed from multi-pixel sampling moir&#233; fringes, allowing for high-accuracy strain measurements. This protocol will introduce the detailed strain measurement procedure and is expected to help researchers and engineers learn how to measure deformation, improving the manufacturing processes of materials and products.

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			<td style="width:201px;">EUN-4200</td>
			<td style="width:167px;">Can be replaced with a electron beam lithography device or a focused ion beam milling device</td>
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micro/nano-scale strain distribution measurement from sampling moir&#233; fringes

This work describes the measurement procedure and principles of a sampling moir&#233; technique for full-field micro/nano-scale deformation measurements. The developed technique can be performed in two ways: using the reconstructed multiplication moir&#233; method or the spatial phase-shifting sampling moir&#233; method. When the specimen grid pitch is around 2 pixels, 2-pixel sampling moir&#233; fringes are generated to reconstruct a multiplication moir&#233; pattern for a deformation measurement. Both the displacement and strain sensitivities are twice as high as in the traditional scanning moir&#233; method in the same wide field of view. When the specimen grid pitch is around or greater than 3 pixels, multi-pixel sampling moir&#233; fringes are generated, and a spatial phase-shifting technique is combined for a full-field deformation measurement. The strain measurement accuracy is significantly improved, and automatic batch measurement is easily achievable. Both methods can measure the two-dimensional (2D) strain distributions from a single-shot grid image without rotating the specimen or scanning lines, as in traditional moir&#233; techniques. As examples, the 2D displacement and strain distributions, including the shear strains of two carbon fiber-reinforced plastic specimens, were measured in three-point bending tests. The proposed technique is expected to play an important role in the non-destructive quantitative evaluations of mechanical properties, crack occurrences, and residual stresses of a variety of materials.

The 2D displacement and strain distributions of two carbon fiber-reinforced plastic (CFRP) specimens (#1 and #2) were measured according to the moir&#233; formation principle23 and the measurement process (Figure 1). The CFRP specimens were made up of 10-11 &#181;m-diameter K13D carbon fibers and epoxy resins. The deformation of CFRP #1 was determined using the reconstructed multiplication moir&#233; method from two-step sampling moir&...

Watch this Scientific Journal Video about Micro/Nano-scale Strain Distribution Measurement from Sampling MoirÃ© Fringes at JoVE.com

Micro/Nano-scale Strain Distribution Measurement from Sampling Moir&amp;#233; Fringes

A sampling moir&#233; technique featuring 2-pixel and multi-pixel sampling methods for high-accuracy strain distribution measurements at the micro/nano-scale is presented here.

Micro/Nano-scale Strain Distribution Measurement from Sampling Moir&#233; Fringes

This work describes the measurement procedure and principles of a sampling moir&#233; technique for full-field micro/nano-scale deformation measurements. ...

The overall goal of this experiment is to accurately measure the strain distributions of materials at the micro or nano scale using the two-pixel or multi-pixel sampling moir

micronano-scale-strain-distribution-measurement-from-sampling-moir

Research

JoVE Journal

Engineering

12.2K Views.  National Institute of Advanced Industrial Science and Technology (AIST). The overall goal of this experiment is to accurately measure the strain distributions of materials at the micro or nano scale using the two-pixel or multi-pixel sampling moir