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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Opt. 51 (16), 3214-3223 (2012).</li><li>Wang, Q., Ri, S., Tsuda, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Digital+sampling+Moir&#233;+as+a+substitute+for+microscope+scanning+Moir&#233;+for+high-sensitivity+and+full-field+deformation+measurement+at+micron/nano+scales.">Digital sampling Moir&#233; as a substitute for microscope scanning Moir&#233; for high-sensitivity and full-field deformation measurement at micron/nano scales.</a> Appl. Opt. 55 (25), 6858-6865 (2016).</li><li>Dai, F., Wang, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Automatic+fringe+patterns+analysis+using+digital+processing+tehniques:+I+fringe+center+method.">Automatic fringe patterns analysis using digital processing tehniques: I fringe center method.</a> Acta Photonica Sinica. 28, 700-706 (1999).</li><li>Gutmann, B., Weber, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Phase-shifter+calibration+and+error+detection+in+phase-shifting+applications:+a+new+method.">Phase-shifter calibration and error detection in phase-shifting applications: a new method.</a> Appl. Opt. 37 (32), 7624-7631 (1998).</li><li>Wang, Q., Kishimoto, S., Tanaka, Y., Kagawa, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Micro/submicro+grating+fabrication+on+metals+for+deformation+measurement+based+on+ultraviolet+nanoimprint+lithography.">Micro/submicro grating fabrication on metals for deformation measurement based on ultraviolet nanoimprint lithography.</a> Opt. Lasers Eng. 51 (7), 944-948 (2013).</li><li>Min-Jin, T., Hui-Min, X., Yan-Jie, L., Xiao-Jun, L., Dan, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+new+grating+fabrication+technique+on+metal+films+using+UV-nanoimprint+lithography.">A new grating fabrication technique on metal films using UV-nanoimprint lithography.</a> Chin. Phys. Lett. 29 (9), 098101 (2012).</li></ol>

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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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

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

Measurement of Scattering Nonlinearities from a Single Plasmonic Nanoparticle

Plasmonics, which are based on the collective oscillation of electrons due to light excitation, involve strongly enhanced local electric fields and thus have potential applications in nonlinear optics, which requires extraordinary optical intensity. One of the most studied nonlinearities in plasmonics is nonlinear absorption, including saturation and reverse saturation behaviors. Although scattering and absorption in nanoparticles are closely correlated by the Mie theory, there has been no report of nonlinearities in plasmonic scattering until very recently. 
Last year, not only saturation, but also reverse saturation of scattering in an isolated plasmonic particle was demonstrated for the first time. The results showed that saturable scattering exhibits clear wavelength dependence, which seems to be directly linked to the localized surface plasmon resonance (LSPR). Combined with the intensity-dependent measurements, the results suggest the possibility of a common mechanism underlying the nonlinear behaviors of scattering and absorption. These nonlinearities of scattering from a single gold nanosphere (GNS) are widely applicable, including in super-resolution microscopy and optical switches. 
In this paper, it is described in detail how to measure nonlinearity of scattering in a single GNP and how to employ the super-resolution technique to enhance the optical imaging resolution based on saturable scattering. This discovery features the first super-resolution microscopy based on nonlinear scattering, which is a novel non-bleaching contrast method that can achieve a resolution as low as l/8 and will potentially be useful in biomedicine and material studies.

Saturable and reverse saturable scattering were discovered in isolated plasmonic particles and adopted as a novel non-bleaching contrast method in super-resolution microscopy. Here the experimental procedures of detecting and extracting nonlinear scattering are explained in detail, as well as how to enhance resolution with the aid of saturated excitation microscopy.

Plasmonics, which are based on the collective oscillation of electrons due to light excitation, involve strongly enhanced local electric fields and thus ...

Strain Sensing Based on Multiscale Composite Materials Reinforced with Graphene Nanoplatelets

The electrical response of NH2-functionalized graphene nanoplatelets composite materials under strain was studied. Two different manufacturing methods are proposed to create the electrical network in this work: (a) the incorporation of the nanoplatelets into the epoxy matrix and (b) the coating of the glass fabric with a sizing filled with the same nanoplatelets. Both types of multiscale composite materials, with an in-plane electrical conductivity of ~10-3 S/m, showed an exponential growth of the electrical resistance as the strain increases due to distancing between adjacent functionalized graphene nanoplatelets and contact loss between overlying ones. The sensitivity of the materials analyzed during this research, using the described procedures, has been shown to be higher than commercially available strain gauges. The proposed procedures for self-sensing of the structural composite material would facilitate the structural health monitoring of components in difficult to access emplacements such as offshore wind power farms. Although the sensitivity of the multiscale composite materials was considerably higher than the sensitivity of metallic foils used as strain gauges, the value reached with NH2 functionalized graphene nanoplatelets coated fabrics was nearly an order of magnitude superior. This result elucidated their potential to be used as smart fabrics to monitor human movements such as bending of fingers or knees. By using the proposed method, the smart fabric could immediately detect the bending and recover instantly. This fact permits precise monitoring of the time of bending as well as the degree of bending.

The integration of conductive nanoparticles, such as graphene nanoplatelets, into glass fiber composite materials creates an intrinsic electrical network susceptible to strain. Here, different methods to obtain strain sensors based on the addition of graphene nanoplatelets into the epoxy matrix or as a coating on glass fabrics are proposed.

The electrical response of NH2-functionalized graphene nanoplatelets composite materials under strain was studied. Two different manufacturing methods are ...

Optical Trap Loading of Dielectric Microparticles In Air

We demonstrate a method to trap a selected dielectric microparticle in air using radiation pressure from a single-beam gradient optical trap. Randomly scattered dielectric microparticles adhered to a glass substrate are momentarily detached using ultrasonic vibrations generated by a piezoelectric transducer (PZT). Then, the optical beam focused on a selected particle lifts it up to the optical trap while the vibrationally excited microparticles fall back to the substrate. A particle may be trapped at the nominal focus of the trapping beam or at a position above the focus (referred to here as the levitation position) where gravity provides the restoring force. After the measurement, the trapped particle can be placed at a desired position on the substrate in a controlled manner. 
In this protocol, an experimental procedure for selective optical trap loading in air is outlined. First, the experimental setup is briefly introduced. Second, the design and fabrication of a PZT holder and a sample enclosure are illustrated in detail. The optical trap loading of a selected microparticle is then demonstrated with step-by-step instructions including sample preparation, launching into the trap, and use of electrostatic force to excite particle motion in the trap and measure charge. Finally, we present recorded particle trajectories of Brownian and ballistic motions of a trapped microparticle in air. These trajectories can be used to measure stiffness or to verify optical alignment through time domain and frequency domain analysis. Selective trap loading enables optical tweezers to track a particle and its changes over repeated trap loadings in a reversible manner, thereby enabling studies of particle-surface interaction.

A protocol for launching and stably trapping selected dielectric microparticles in air is presented.

We demonstrate a method to trap a selected dielectric microparticle in air using radiation pressure from a single-beam gradient optical trap. Randomly ...

Standardized Method for Measuring Collection Efficiency from Wipe-sampling of Trace Explosives

One of the limiting steps to detecting traces of explosives at screening venues is effective collection of the sample. Wipe-sampling is the most common procedure for collecting traces of explosives, and standardized measurements of collection efficiency are needed to evaluate and optimize sampling protocols. The approach described here is designed to provide this measurement infrastructure, and controls most of the factors known to be relevant to wipe-sampling. Three critical factors (the applied force, travel distance, and travel speed) are controlled using an automated device. Test surfaces are chosen based on similarity to the screening environment, and the wipes can be made from any material considered for use in wipe-sampling. Particle samples of the explosive 1,3,5-trinitroperhydro-1,3,5-triazine (RDX) are applied in a fixed location on the surface using a dry-transfer technique. The particle samples, recently developed to simulate residues made after handling explosives, are produced by inkjet printing of RDX solutions onto polytetrafluoroethylene (PTFE) substrates. Collection efficiency is measured by extracting collected explosive from the wipe, and then related to critical sampling factors and the selection of wipe material and test surface. These measurements are meant to guide the development of sampling protocols at screening venues, where speed and throughput are primary considerations.

Optimized sampling protocols and the development of new wipe materials can be facilitated by standardized measurements of collection efficiency from wipe-sampling. Our approach for sampling trace explosives uses an automated device to control speed, force, and distance during wipe-sampling followed by extraction of collected explosives.

One of the limiting steps to detecting traces of explosives at screening venues is effective collection of the sample. Wipe-sampling is the most common ...

Generation of Size-controlled Poly (ethylene Glycol) Diacrylate Droplets via Semi-3-Dimensional Flow Focusing Microfluidic Devices

Uniform and size-controllable poly (ethylene glycol) diacrylate (PEGDA) droplets could be produced via the flow focusing process in a microfluidic device. This paper proposes a semi-three-dimensional (semi-3D) flow-focusing microfluidic chip for droplet formation. The polydimethylsiloxane (PDMS) chip was fabricated using the multi-layer soft lithography method. Hexadecane containing surfactant was used as the continuous phase, and PEGDA with the ultraviolet (UV) photo-initiator was the dispersed phase. Surfactants allowed the local surface tension to drop and formed a more cusped tip which promoted breaking into tiny micro-droplets. As the pressure of dispersed phase was constant, the size of droplets became smaller with increasing continuous phase pressure before dispersed phase flow was broken off. As a result, droplets with size variation from 1 &#181;m to 80 &#181;m in diameter could be selectively achieved by changing the pressure ratio in two inlet channels, and the average coefficient of variation was estimated to be below 7%. Furthermore, droplets could turn into micro-beads by UV exposure for photo-polymerization. Conjugating biomolecules on such micro-beads surface have many potential applications in the fields of biology and chemistry.

Generation of Size-controlled Poly ethylene Glycol Diacrylate Droplets via Semi-3-Dimensional Flow Focusing Microfluidic Devices

Here, we present a protocol to illustrate the fabrication processes and verifying experiments of a semi-three-dimensional (semi-3D) flow-focusing microfluidic chip for droplet formation.

Uniform and size-controllable poly (ethylene glycol) diacrylate (PEGDA) droplets could be produced via the flow focusing process in a microfluidic device. ...

Cutting Procedures, Tensile Testing, and Ageing of Flexible Unidirectional Composite Laminates

Many body armor designs incorporate unidirectional (UD) laminates. UD laminates are constructed of thin (&#60;0.05 mm) layers of high-performance yarns, where the yarns in each layer are oriented parallel to each other and held in place using binder resins and thin polymer films. The armor is constructed by stacking the unidirectional layers in different orientations. To date, only very preliminary work has been performed to characterize the ageing of the binder resins used in unidirectional laminates and the effects on their performance. For example, during the development of the conditioning protocol used in the National Institute of Justice Standard-0101.06, UD laminates showed visual signs of delamination and reductions in V50, which is the velocity at which half of the projectiles are expected to perforate the armor, after ageing. A better understanding of the material property changes in UD laminates is necessary to comprehend the long-term performance of armors constructed from these materials. There are no current standards recommended for mechanically interrogating unidirectional (UD) laminate materials. This study explores methods and best practices for accurately testing the mechanical properties of these materials and proposes a new test methodology for these materials. Best practices for ageing these materials are also described.

The goal of the study was to develop protocols to prepare consistent specimens for accurate mechanical testing of high-strength aramid or ultra-high-molar-mass polyethylene-based flexible unidirectional composite laminate materials and to describe protocols for performing artificial ageing on these materials.

Many body armor designs incorporate unidirectional (UD) laminates. UD laminates are constructed of thin (&#60;0.05 mm) layers of high-performance yarns, ...

Intermediate Strain Rate Material Characterization with Digital Image Correlation

The mechanical response of a material under dynamic load is typically different than its behavior under static conditions; therefore, the common quasistatic equipment and procedures used for material characterization are not applicable for materials under dynamic loads. The dynamic response of a material depends on its deformation rate and is broadly categorized into high (i.e., greater than 200/s), intermediate (i.e., 10&#8722;200/s) and low strain rate regimes (i.e., below 10/s). Each of these regimes calls for specific facilities and testing protocols to ensure the reliability of the acquired data. Due to the limited access to high-speed servo-hydraulic facilities and validated testing protocols, there is a noticeable gap in the results at the intermediate strain rate. The current manuscript presents a validated protocol for the characterization of different materials at these intermediate strain rates. Strain gauge instrumentation and digital image correlation protocols are also included as complimentary modules to extract the utmost level of detailed data from every single test. Examples of raw data, obtained from a variety of materials and test setups (e.g., tensile and shear) is presented and the analysis procedure used to process the output data is described. Finally, the challenges of dynamic characterization using the current protocol, along with the limitations of the facility and methods of overcoming potential problems are discussed.

Here we present a methodology for the dynamic characterization of tensile specimens at intermediate strain rates using a high-speed servo-hydraulic load frame. Procedures for strain gauge instrumentation and analysis, as well as for digital image correlation strain measurements on the specimens, are also defined.

The mechanical response of a material under dynamic load is typically different than its behavior under static conditions; therefore, the common ...

Method Development for Contactless Resonant Cavity Dielectric Spectroscopic Studies of Cellulosic Paper

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of data that can be obtained from an individual sample and renders it difficult to produce statistically relevant data for unique and rare materials. Resonant cavity dielectric spectroscopy is a non-destructive, contactless technique which can simultaneously interrogate both sides of a sheeted material and provide measurements which are suitable for statistical interpretations. This offers analysts the ability to quickly discriminate between sheeted materials based on composition and storage history. In this methodology article, we demonstrate how contactless resonant cavity dielectric spectroscopy may be used to differentiate between paper analytes of varying fiber species compositions, to determine the relative age of the paper, and to detect and quantify the amount of post-consumer waste (PCW) recycled fiber content in manufactured office paper.

A protocol for the non-destructive analysis of the fiber content and relative age of paper.

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of ...

Measuring Sub-23 Nanometer Real Driving Particle Number Emissions Using the Portable DownToTen Sampling System

The current particle size threshold of the European Particle Number (PN) emission standards is 23 nm. This threshold could change because future combustion engine vehicle technology may emit large amounts of sub-23 nm particles. The Horizon 2020 funded project DownToTen (DTT) developed a sampling and measurement method to characterize particle emissions in this currently unregulated size range. A PN measurement system was developed based on an extensive review of the literature and laboratory experiments testing a variety of PN measurement and sampling approaches. The measurement system developed is characterized by high particle penetration and versatility, which enables the assessment of primary particles, delayed primary particles, and secondary aerosols, starting from a few nanometers in diameter. This paper provides instruction on how to install and operate this Portable Emission Measurement System (PEMS) for Real Drive Emissions (RDE) measurements and assess particle number emissions below the current legislative limit of 23 nm.

Presented here is the DownToTen (DTT) portable emission measurement system to assess real driving automotive emissions of sub-23 nm particles.

The current particle size threshold of the European Particle Number (PN) emission standards is 23 nm. This threshold could change because future ...

Calibration Procedures for Orthogonal Superposition Rheology

Orthogonal superposition (OSP) rheology is an advanced rheological technique that involves superimposing a small-amplitude oscillatory shear deformation orthogonal to a primary shear flow. This technique allows the measurement of structural dynamics of complex fluids under non-linear flow conditions, which is important for the understanding and prediction of the performance of a wide range of complex fluids. The OSP rheological technique has a long history of development since the 1960s, mainly through the custom-built devices that highlighted the power of this technique. The OSP technique is now commercially available to the rheology community. Given the complicated design of the OSP geometry and the non-ideal flow field, users should understand the magnitude and sources of measurement error. This study presents calibration procedures using Newtonian fluids that includes recommendations for best practices to reduce measurement errors. Specifically, detailed information on the end-effect factor determination method, sample filling procedure, and identification of the appropriate measurement range (e.g., shear rate, frequency, etc.) are provided.

We present a detailed calibration protocol for a commercial orthogonal superposition rheology technique using Newtonian fluids including end-effect correction factor determination methods and recommendations for best practices to reduce experimental error.

Orthogonal superposition (OSP) rheology is an advanced rheological technique that involves superimposing a small-amplitude oscillatory shear deformation ...