We would like to thank Taarna Studemund and Hagen Wendler for taking photographs of the experimental setup as well as preparing them for figure publication. Furthermore, we would like to thank Anne Hildebrandt for the sample preparation and Sreedhar Unnikrishnakurup, Alexander Battig and Felix Fritzsche for proof-reading.

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P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Introduction+to+NDT+by+active+infrared+thermography.">Introduction to NDT by active infrared thermography.</a> Mater. Eval. 60 (9), 1060-1073 (2002).</li><li>Li, T., Almond, D. P., Rees, D. A. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Crack+imaging+by+scanning+pulsed+laser+spot+thermography.">Crack imaging by scanning pulsed laser spot thermography.</a> Ndt&amp;E Int. 44 (2), 216-225 (2011).</li><li>Lugin, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Detection+of+hidden+defects+by+lateral+thermal+flows.">Detection of hidden defects by lateral thermal flows.</a> Ndt&amp;E Int. 56, 48-55 (2013).</li><li>Li, T., Almond, D. P., Rees, D. A. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Crack+imaging+by+scanning+laser-line+thermography+and+laser-spot+thermography.">Crack imaging by scanning laser-line thermography and laser-spot thermography.</a> Meas. Sci. Technol. 22 (3), (2011).</li><li>Pech-May, N. W., Oleaga, A., Mendioroz, A., Salazar, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fast+Characterization+of+the+Width+of+Vertical+Cracks+Using+Pulsed+Laser+Spot+Infrared+Thermography.">Fast Characterization of the Width of Vertical Cracks Using Pulsed Laser Spot Infrared Thermography.</a> Journal of Nondestructive Evaluation. 35 (2), 22 (2016).</li><li>Thiel, E., Kreutzbruck, M., Ziegler, M., Douglass, M. R., King, P. S., Lee, B. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Proc. SPIE 9761. , (2016).</li><li>Thiel, E., Kreutzbruck, M., Ziegler, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Proc. WCNDT 2016. , 6 (2016).</li><li>Mandelis, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Diffusion-Wave Fields: mathematical methods and Green functions. , (2001).</li><li>Almond, D., Patel, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Photothermal Science and Techniques. 10, (1996).</li><li>Salazar, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Energy+propagation+of+thermal+waves.">Energy propagation of thermal waves.</a> Eur. J. Phys. 27 (6), 1349-1355 (2006).</li><li>Bennett, C. A., Patty, R. 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SPIE 9861. , (2016).</li><li>Ravichandran, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Spatial and temporal modulation of heat source using light modulator for advanced thermography. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> DLP 0.55 XGA Series 450 DMD. , (2015).</li><li>. DLP LightCommander Control Software - User Manual Available from: <a target="_blank" href="https://support.logicpd.com/ProductDownloads/LegacyProducts/DLPLightCommander.aspx?_sw_csrfToken=318b0448">https://support.logicpd.com/ProductDownloads/LegacyProducts/DLPLightCommander.aspx?_sw_csrfToken=318b0448</a> (2011)</li><li>Moench, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High-power+VCSEL+systems+and+applications.">High-power VCSEL systems and applications.</a> Proc. SPIE 9348. , (2015).</li></ol>

The authors have nothing to disclose.

The presented protocol describes how to locate artificial subsurface defects oriented perpendicular to the surface. The main idea of the method is to create interfering thermal wave fields which interact with the subsurface defect. The most important steps are (i) to combine an SLM with a diode laser in order to create two alternating high-power illumination patterns at the sample surface; these patterns are photothermally converted into coherent thermal wave fields, (ii) to let them destructively interfere whilst interacting with a subsurface defect, and (iii) to locate these defects from a surface scan of the dynamic temperature of the sample surface using a thermal imaging IR camera. Since only the relative oscillation of the temperature around a slowly varying mean value and not the absolute temperature value is needed, this approach is extremely sensitive to hidden defects1.
One of the most critical steps within the protocol is to establish sufficient homogeneity of the illumination beam profile when using an SLM-coupled laser source for structured heating (refer to step 1.10). The diode laser offers a high irradiance but has to be fed into the projector containing the SLM with the correct beam diameter and directionality. Due to slight unavoidable geometrical and spectral mismatches with the proprietary optical path within the projector, the generated image on the sample is distorted. Therefore, a numerical correction of the image intensity values controlling the projected image is performed with a referencing beam profile measurement. A second critical step for a successful experiment is to achieve a high spatial resolution of the IR image (refer to steps 3.3.7- 3.3.8). The depletion zone has to be sufficiently spatially resolved, else no depletion and therefore no defect position can be measured.
The nature of the applied thermal waves is a diffusion-like process that leads to a strong attenuation of their amplitude over a few millimeters only. We meet this intrinsic physical limitation by using a high-power diode laser as light source. The bottleneck of the current experimental setup is the thermal stress limit of the SLM21, which means that only a fraction of the available laser power can be applied. Our current solution is to coat the sample surface with a black graphite coating. In the future, we expect setups with higher sensitivity using optimized light engines or even switchable direct laser arrays, such as high-power vertical-cavity surface-emitting laser (VCSEL) arrays22.
The main difference between this method and the existing thermal imaging in non-destructive testing is the fact that we use the destructive interference of fully coherent thermal wave fields; which is possible only after having control over amplitude and phase of a set of individual light sources in a deterministic way. Within the existing thermographic methods, either a planar light source, controlled in the time domain, or a single focused laser spot, controlled in the spatial domain, is used. The major advantage of our approach is high sensitivity to defects lying perpendicular to the sample surface.
Thus far, only two individual light sources have been created. With the laser-coupled SLM we can, in principle, generate and control up to one million individual light sources - one million heat sources - on the sample surface. Clearly this approach opens up the possibilities of arbitrary thermal wave shaping in the long term and transfer techniques from ultrasound or radar to the field of active thermography, within physical limits. Once the irradiance challenge as stated above (i.e. optical power per projected pixel) is satisfactorily solved, even smaller defects located deeper below the surface should become detectable. So far, steel has been tested, but the method is very promising especially for plastics, compound material, and other sensitive materials, due to the low thermal stress applied.

The laser projected photothermal thermography (LPPT) method is used to locate subsurface defects that are embedded in the volume of the test specimen and oriented predominantly perpendicular to its surface.
The method uses the destructive interference of two anti-phased thermal wave fields of the same elongation and frequency as shown in Figure 1b. In isotropic defect-free materials, the thermal waves neutralize destructively (i.e. zero temperature oscillation) at the symmetry plane by coherent superposition. In case of a material with a subsurface defect, the method takes advantage of the interaction of the lateral (i.e. in-plane) components between the transient heat flow and this defect. This interaction can be measured in a recreated oscillating temperature elongation at the symmetry line on the sample surface. Now, the defect containing sample is scanned by the superposed thermal wave field and the level of temperature elongation is measured in relation to the sample position. Due to symmetry, the destructive interference condition is satisfied once again when the defect crosses the symmetry plane; this enables us to locate the defect very sensitively. Moreover, since the level of maximal disturbance of the destructive interference correlates with the depth of the defect, it is possible to determine its depth by analyzing the temperature scan1.
The LPPT can be assigned to the active thermography methodology, a well-established non-destructive method, where transient heating is actively generated and the resulting, also transient, temperature distribution is measured via a thermal IR camera. In general, the sensitivity of this methodology is limited to defects which are oriented essentially perpendicular to the transient heat flow. Moreover, since the governing transient heat conduction equation is a parabolic partial differential equation, the heat flow into the volume is strongly damped. As a consequence, the probing depth of the active thermography methodology is limited to a near surface region, usually in the millimeter-range. Two of the most common active thermography techniques are pulsed and lock-in thermography. They are fast due to planar optical surface illumination2, but lead to a transient heat flow perpendicular to the surface. Therefore, the sensitivity of these techniques is limited to defects predominantly oriented parallel (e.g. delaminations or voids) to the heated sample surface. An empirical rule for pulsed thermography states that &#34;the radius of the smallest detectable defect should be at least one to two times larger than its depth under the surface&#34;3. To increase the effective interaction area between a perpendicularly oriented defect (e.g. a crack) and the heat flow, the direction of the heat flow needs to be changed. Local excitation, by using a focused laser with a linear or circular spot for instance, generates a heat flow with an in-plane component that is able to effectively interact with the perpendicular defect4,5,6,7.
In the presented method, we also use the lateral heat flow components to detect subsurface defects, but we use the fact that thermal waves can be superposed, whereas defects, especially vertically oriented ones, disturb this superposition. In this way, the presented method resembles a reference-free, symmetric and very sensitive method, as it is possible to detect artificial subsurface defects at a width/depth ratio of far below one8,9. Until now, it was difficult to create two anti-phased thermal wave fields supplying sufficient energy. We achieved this by coupling a spatial light modulator (SLM) to a high-power diode laser, which enabled us to merge the high optical power of the laser system with the spatial and temporal resolution of the SLM (see Figure 2) into a high-power projector. The thermal wave fields are now created by photothermal conversion of two anti-phased sinusoidally modulated line patterns via the pixel brightness of the projected image (see Figure 2, Figure 1a). This leads to structured heating of the sample surface and results in well-defined destructively interfering thermal wave fields. In order to find a subsurface defect, the disturbance of the destructive inference is measured as a temperature oscillation at the surface using an IR camera.
The term thermal wave, is controversially discussed because thermal waves do not transport energy due to the diffusive character of the heat propagation. Still, there is wave-like behavior when heating periodically, allowing us to use similarities between real waves and diffusion processes10,11,12. Thus, a thermal wave can be understood as highly damped in the propagation direction but periodic over time (Figure 1b). The characteristic thermal diffusion length <img alt="Equation 1" src="/files/ftp_upload/55733/55733eq1.jpg" /> is hereby described by its material properties (thermal conductivity k, heat capacity cp and density &#961;), and the excitation frequency &#402;. Although the thermal wave is decaying strongly, its wave nature can be applied to gain insight into the properties of the sample. The first application of thermal wave interference was used to determine the thickness of layers. In contrast to our method, the interference effect was used in the depth dimension (i.e. perpendicular to the surface)13. Extending the idea of interference to a second dimension by splitting up a laser beam, thermal wave interference was used to size subsurface defects14. Still this method was applied in transmission configuration, which means that it was limited by the penetration depth of the thermal wave. Furthermore, because only one laser source has been used, this method applies constructive interference, meaning that a defect-free reference is needed. Apart from the idea of using thermal wave interference, the first technical approach to spatially and temporally controlled heating was performed by Holtmann et al. using an unmodified liquid crystal display (LCD) projector with the built-in light source, which was severely limited in its optical output power15. Further approaches by Pribe and Ravichandran aimed at increasing the optical output power by also coupling a laser to a SLM16,17.
The protocol presented herein describes how to apply the LPPT method to locate subsurface defects oriented perpendicularly to the surface of steel samples. The method is at an early stage, yet powerful enough to validate the proposed approach; however, it is still limited in terms of the achievable optical output power of the experimental setup. Since the increase of the optical output power remains a challenge, the presented method is applied to coated steel containing artificial electrically discharge machined notches. Nevertheless, the most important and most critical steps of the protocol, generating a homogeneous structured illumination, meeting prerequisites for destructive thermal wave interference, and locating the defect, still hold for more demanding defects as well. Since the governing quantity is the thermal diffusion length &#956;, the LPPT method can be applied to numerous different materials as well.
<img alt="Figure 1" src="/files/ftp_upload/55733/55733fig1.jpg" /> 
Figure 1: Principle of destructive interference effect. (a) Schematic of the illumination pattern used during experiments. The sample is spatially and temporally heated by two periodically illuminated patterns with a phase shift of &#960;. The dashed line represents the symmetry line between both patterns. This line will be used for evaluation as a &#34;depletion line&#34;. (b) Diagram of the spatially and temporally resolved alternating thermal result as calculated from the analytical solution of the thermal heat conduction equation. It shows the responding thermal waves to the illumination of (a) with an irradiance of the two patterns with Popt1 = 1.5 W sin(2&#960; 0.125 Hz t) + 1.5 W and Popt2 = 1.5 W sin(2&#960; 0.125 Hz t + &#960;) + 1.5 W for constructional steel &#961; = 7,850 kg/m3, cp = 461 J/(kg&#183;K), k = 54 W/(m&#183;K). The temperature profile at the dashed line shows no thermal oscillation for homogeneous, isotropic material. <a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55733/55733fig1large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<img alt="Figure 2" src="/files/ftp_upload/55733/55733fig2.jpg" /> 
Figure 2: Schematic of the measurement principle of structured heating used in active thermography. A Gaussian beam homogenized to a top hat profile is applied to a Spatial Light Modulator (SLM). The SLM resolves the beam spatially by its switchable elements and temporally by its switching speed. Each element represents an SLM pixel. In this experiment, the SLM is a digital micro mirror device (DMD). By modulating the pixel brightness A with a time deterministic control software, the sample surface is heated in a structured way. In case of the presented experiment, we modulate two anti-phased lines (phases: &#966; = 0, &#960;), which are the origin of coherently interfering thermal wave fields at the angular frequency &#969;. The wave fields interact with the sample&#39;s inner structure also influencing the temperature field at the surface. This is measured via its thermal radiation by a mid-wave infrared camera. <a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55733/55733fig2large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>

<table border="0" cellpadding="0" cellspacing="0" width="681">
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		<col />
	</colgroup>
	<tbody>
		<tr height="84">
			<td height="84" style="height:84px;width:269px;">500 W diode laser system, 940 nm</td>
			<td style="width:88px;">Laserline</td>
			<td style="width:104px;">LDM 500 - 20</td>
			<td style="width:220px;">Pilot laser class 2 @ 650 nm, diode laser is a class 4 laser system --&#62; special laboratory needed</td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:269px;">Laser control box</td>
			<td style="width:88px;">Laserline</td>
			<td style="width:104px;">Laser control box LDM</td>
			<td style="width:220px;">Add on to the laser system, used to switch electronically, laser threshold, shutter, laser on 0 V ..5 V TTL</td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:269px;">Control box scanner</td>
			<td style="width:88px;">Laserline</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Add on to the laser system, used to adjust the optical output power via analog signal from 0 V..10 V</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Fiber Laser Mount 2&#34;, f = 80 mm</td>
			<td style="width:88px;">Laserline</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Add on to the laser system</td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:269px;">Multifunction Data Aquisition (DAQ) Device + BNC Terminal</td>
			<td style="width:88px;">National Instruments</td>
			<td style="width:104px;">NI-USB 6251</td>
			<td style="width:220px;">The DAQ card is used to trigger the IR camera,&#160; the DLP Light Commander 5500, control Laser and diode PDA 36A</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:269px;">Standard - PC&#160;</td>
			<td style="width:88px;"></td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Control PC - graphic card for two screens, at least 4 x USB, Windows based</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">BNC cabel</td>
			<td style="width:88px;"></td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Standard cable</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">HDMI cable</td>
			<td style="width:88px;"></td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Standard cable</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Micro USB to USB cable</td>
			<td style="width:88px;"></td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Standard cable</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">LabVIEW 2013 SP1 Development System</td>
			<td style="width:88px;">National Instruments</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Development environment for device control</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">LPPT control software</td>
			<td style="width:88px;">BAM</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">part of the LPPT software package by LabVIEW 2013 SP1</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">LPPT intensity&#160; software</td>
			<td style="width:88px;">BAM</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">part of the LPPT software package by LabVIEW 2013 SP1</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">LPPT laser control software</td>
			<td style="width:88px;">BAM</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">part of the LPPT software package by LabVIEW 2013 SP1</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Matlab 2016b</td>
			<td style="width:88px;">MathWorks</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Postprocessing of the measurement data</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">LPPT postprocessing software</td>
			<td style="width:88px;">BAM</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Postprocessing of the measurement data</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">IR camera control PC&#160;</td>
			<td style="width:88px;">InfraTec</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Control PC is supplied by camera distributor</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">IR camera control software</td>
			<td style="width:88px;">InfraTec</td>
			<td style="width:104px;">Irbis 3 Professional</td>
			<td style="width:220px;"></td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:269px;">InfraTec SDK</td>
			<td style="width:88px;">InfraTec</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Dynamic Link Library as interface between the native data aquisition format of Infratec and Matlab</td>
		</tr>
		<tr height="105">
			<td height="105" style="height:105px;width:269px;">IR camera</td>
			<td style="width:88px;">InfraTec</td>
			<td style="width:104px;">Image IR 8300</td>
			<td style="width:220px;">640 x 512, cooled InSb detector, wavelength 2 &#181;m..5.7 &#181;m, noise = 20 mK + accessories (LAN cable, Digital in/out cable, space ring, power supply, case)&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Tripod</td>
			<td style="width:88px;">Manfrotto</td>
			<td style="width:104px;">161MK2B</td>
			<td style="width:220px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">IR camera mount</td>
			<td style="width:88px;">Manfrotto</td>
			<td align="right" style="width:104px;">405</td>
			<td style="width:220px;"></td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:269px;">Projector development kit (PDK) for digital light processing (DLP) technology (DLP Light Commander 5500)</td>
			<td style="width:88px;">Logic PD</td>
			<td style="width:104px;">DLP-LC-DLP5500-10R</td>
			<td style="width:220px;">DLP5500 Digital Micromirror Device from Texas Instruments included , light engine and case need to be disassembed</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:269px;">PDK control software</td>
			<td style="width:88px;">Logic PD</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Included when delivered, DLP Light Commander control software</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Mechanical platform for the PDK</td>
			<td style="width:88px;">BAM</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Self made (140 x 230 x 420) mm</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Power meter control unit</td>
			<td style="width:88px;">Ophir</td>
			<td style="width:104px;">Vega</td>
			<td style="width:220px;">USB Interface</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:269px;">30 W power meter head&#160;</td>
			<td style="width:88px;">Ophir</td>
			<td style="width:104px;">30(150)A-LP1-18</td>
			<td style="width:220px;">Power meter head to determine Transmission of the projector system</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">500 W power meter head</td>
			<td style="width:88px;">Ophir</td>
			<td style="width:104px;">FL500A</td>
			<td style="width:220px;">Power meter for process supervision</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Motion controller</td>
			<td style="width:88px;">Newport</td>
			<td style="width:104px;">ESP301</td>
			<td style="width:220px;">with USB Interface</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Translation stage</td>
			<td style="width:88px;">Newport</td>
			<td style="width:104px;">M-ILS200CC</td>
			<td style="width:220px;">Connected to ESP301</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Photodiode with amplifier</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">PDA 36A-EC</td>
			<td style="width:220px;">1&#34; mount</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Reflective filter ND1</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">ND10A</td>
			<td style="width:220px;">to be mounted to the PDA 36A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Pinhole 1&#34;</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">P1000S</td>
			<td style="width:220px;">to be mounted to the PDA 36A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Optical aluminium breadboard&#160;</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">MB60120/M</td>
			<td style="width:220px;">(1200 mm x 900 mm) base&#160;</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Plano Convex Lens f = 200 mm</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">LA1979-B</td>
			<td style="width:220px;">Coated for IR, first telescope lens</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Plano Convex Lens f = 75 mm</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">LA1145-B</td>
			<td style="width:220px;">Coated for IR, second telescope lens</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">xy-translation stage</td>
			<td style="width:88px;">Newport</td>
			<td style="width:104px;">M401</td>
			<td style="width:220px;">Used for adjusting the telecope</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:269px;">Beamsampler</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">BSF20-B&#160;</td>
			<td style="width:220px;">Splits the optical output, used to reduce the optical input for the projector system</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Mirror</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">BB2-E03</td>
			<td style="width:220px;">Mirror for coupling the beam to the DLP Light Commander</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:269px;">Heavy duty lab jack</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">L490</td>
			<td style="width:220px;">Used for the fiber mount and on top of the linear stage to position the sample (2x)</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:269px;">PDK-objective&#160;</td>
			<td style="width:88px;">Nikon</td>
			<td style="width:104px;">Nikon AF Nikkor 50 mm 1:1:8:D&#160;</td>
			<td style="width:220px;">Objective for DLP Light Commander, 50 mm</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Plano Convex Lens f = 100 mm</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">LA1050 -B</td>
			<td style="width:220px;">Lens is attached to the Nikon Objective</td>
		</tr>
		<tr height="105">
			<td height="105" style="height:105px;width:269px;">Bi-Convex Lens f = 60 mm</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">LB1723 -B</td>
			<td style="width:220px;">Lens to be attached to the Nikon objective in order to determine the optical transmission with the 30 W measurement head</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Square protected gold mirror</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">PFSQ20-03-M01</td>
			<td style="width:220px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">High power IR sensor card</td>
			<td style="width:88px;">Newport</td>
			<td style="width:104px;">F-IRC-HP-M</td>
			<td style="width:220px;">Sensor card to check the optical pathway</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">2&#34; crosshairs</td>
			<td style="width:88px;">BAM</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Selfmade</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">1&#34; crosshairs</td>
			<td style="width:88px;">BAM</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">Selfmade</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Bullseye level</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">LCL01</td>
			<td style="width:220px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Translation Stage</td>
			<td style="width:88px;">Newport</td>
			<td style="width:104px;">M-UMR8.25</td>
			<td style="width:220px;">Used for measuring the beam profile</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Micrometer screw</td>
			<td style="width:88px;">Newport</td>
			<td style="width:104px;">DM17-25</td>
			<td style="width:220px;">Used with translation stage M-UMR8.25</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Mounted Zero Aperture Iris</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">&#160;ID75Z/M</td>
			<td style="width:220px;">used to check the optical pathway</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Bases and Post Holders Essentials Kit, Metric and Universal Components</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">ESK01/M</td>
			<td style="width:220px;">Basis&#160;</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Posts &#38; Accessories Essentials Kit, Metric and Universal Components</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">ESK03/M</td>
			<td style="width:220px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">M6 Cap Screw and Hardware Kit</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">HW-KIT2/M</td>
			<td style="width:220px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Construction Rails</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">XE25L700/M</td>
			<td style="width:220px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">1&#34; Construction Cube</td>
			<td style="width:88px;">Thorlabs</td>
			<td style="width:104px;">RM1G</td>
			<td style="width:220px;">Used to mount construction rails</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:269px;">Electrical discharge machining</td>
			<td style="width:88px;">Sodick</td>
			<td style="width:104px;">AG60L</td>
			<td style="width:220px;">www.sodick.de</td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:269px;">St37 block of steel (100 x 100 x 40) mm</td>
			<td style="width:88px;">BAM</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">selfmade, hidden defect with remaining wall thicknesses of 0.25 mm, 0.5 mm, 0.70 mm 1.25 mm (shown in Fig. 5)</td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:269px;">St37 block of steel (100 x 100 x 40) mm</td>
			<td style="width:88px;">BAM</td>
			<td style="width:104px;"></td>
			<td style="width:220px;">selfmade, hidden defect with remaining wall thicknesses of 1 mm, 1.5 mm, 1.75 mm, 2 mm (shown in Fig. 5)</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:269px;">Graphite spray</td>
			<td style="width:88px;">CRC Industries Europe NV</td>
			<td style="width:104px;">GRAPHIT 33</td>
			<td style="width:220px;">Ref. 20760, 200 ml aerosol (Kontakt-Chemie)</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:269px;">Protective tape</td>
			<td style="width:88px;">Tesa</td>
			<td style="width:104px;">tesakrepp 4348</td>
			<td style="width:220px;">used to protect the hidden defects while coating</td>
		</tr>
	</tbody>
</table>

subsurface defect localization by structured heating using laser projected photothermal thermography

The presented method is used to locate subsurface defects oriented perpendicularly to the surface. To achieve this, we create destructively interfering thermal wave fields that are disturbed by the defect. This effect is measured and used to locate the defect. We form the destructively interfering wave fields by using a modified projector. The original light engine of the projector is replaced with a fiber-coupled high-power diode laser. Its beam is shaped and aligned to the projector&#39;s spatial light modulator and optimized for optimal optical throughput and homogeneous projection by first characterizing the beam profile, and, second, correcting it mechanically and numerically. A high-performance infrared (IR) camera is set up according to the tight geometrical situation (including corrections of the geometrical image distortions) and the requirement to detect weak temperature oscillations at the sample surface. Data acquisition can be performed once a synchronization between the individual thermal wave field sources, the scanning stage, and the IR camera is established by using a dedicated experimental setup which needs to be tuned to the specific material being investigated. During data post-processing, the relevant information on the presence of a defect below the surface of the sample is extracted. It is retrieved from the oscillating part of the acquired thermal radiation coming from the so-called depletion line of the sample surface. The exact location of the defect is deduced from the analysis of the spatial-temporal shape of these oscillations in a final step. The method is reference-free and very sensitive to changes within the thermal wave field. So far, the method has been tested with steel samples but is applicable to different materials as well, in particular to temperature sensitive materials.

Following the protocol, side 1 of the steel sample with a subsurface defect at a depth of 0.25 mm was chosen to generate representative results. The defect was initially positioned approximately at the center of the illuminated area. The sample was then moved from -5 mm to 5 mm via the linear stage at a speed of 0.05 mm/s. Using these parameters, Figure 11a shows the scan data after extracting them from the depletion line. At this stage, the success of the experiment can be estimated, as the raw data is available from the IR camera control software as a preview (optional: Use the line tool to preview the data, cf. Figure 8, step i.4). Following further signal post-processing, Figure 11b shows the defect position at the minimum of the Hilbert curve (blue) at 0.3 mm.
To validate the experiment, the curve should have the following properties: it should be symmetrical, have a pronounced minimum at the symmetry plane and two equal maxima to its left and right. The maxima arise because the heat flow from one of the line sources dominates over the other due to the accumulation of heat at the defect. This is especially the case when the defect is positioned close to the symmetry plane. The defect forms a barrier for the heat flow so we can observe the heat flow of the dominating source and its reflection from the defect. If the defect is positioned symmetrically in the middle, the heat flow splits up equally, which results in a minimum1.
The effect of the scan speed is shown in Figure 11c. Here, the scan speed was doubled to 0.1 mm/s to evaluate the same defect. Beforehand, the sample was shifted slightly on the stage in order to gain a different relative position. The defect position was determined to be -2 mm. The level of elongation was similar to the data shown in Figure 11a, demonstrating good reproducibility of the experiment, but with fewer oscillations. Since the maximal elongation correlates with the depth of the defect, information about position and depth can be maintained as well1.
Figure 11d shows a suboptimal dataset. The defect was 1 mm below the surface, which is almost at the detection limit of this diffusion length and the available optical power. Although the location of the defect can still be determined, the measurement uncertainty is larger because the location of the zero oscillation is already affected by noise. From this behavior, we can infer that the most obvious signs for a failure of the defect detection experiment are if the depletion line vanishes completely or if there is a strong asymmetrical behavior. This can be due to the following reasons: (i) the spatial resolution of the IR camera is not sufficient and the depletion line cannot be resolved properly, (ii) the noise of the camera is too high in comparison to the temperature rise, (iii) the illumination pattern is inhomogeneous and has not been corrected properly, (iv) the chosen stage velocity is too high, as compared to the modulation frequency of the illumination pattern, and (v) the thermal diffusion length (via the modulation frequency) is not adapted to the defect depth.
<img alt="Figure 11" src="/files/ftp_upload/55733/55733fig11.jpg" /> 
Figure 11: Representative dataset from experiments to locate subsurface defects. (a) Representative experimental data from the St37 sample, side 1 with a defect at a depth of 0.25 mm. The black line shows temperature information over time (top axis). By translating the stage at a velocity v = 0.05 mm/s, the position is retrieved (bottom axis). The red curve shows a polynomial fit (7th degree) used to gain the alternating temperature component. The dashed red line represents the position of the subsurface defect.(b) The black curve shows the alternating temperature graph obtained by subtracting the polynomial fit from the temperature data of panel (a). The blue curve was obtained by applying Hilbert transformation to the black curve and averaging. (c) Representative experimental data of the same side over a range of -7 mm to 3 mm at a stage velocity of 0.1 mm/s. The frequency is halved but the elongation is similar to panel (a). (d) Suboptimal experimental data acquired when the subsurface defect was at a depth of 1 mm. <a href="https://cloudflare-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55733/55733fig11large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>

Watch this Scientific Journal Video about Subsurface Defect Localization by Structured Heating Using Laser Projected Photothermal Thermography at JoVE.com

Subsurface Defect Localization by Structured Heating Using Laser Projected Photothermal Thermography

This method aims at locating vertical subsurface defects. Here, we couple a laser with a spatial light modulator and trigger its video input to heat a sample surface deterministically with two anti-phased modulated lines while acquiring highly resolved thermal images. The defect position is retrieved from evaluating thermal wave interference minima.

The presented method is used to locate subsurface defects oriented perpendicularly to the surface. To achieve this, we create destructively interfering ...

subsurface-defect-localization-structured-heating-using-laser

Nanyang Technological University

Research

JoVE Journal

Engineering

11.0K Views.  Bundesanstalt für Materialforschung und -prüfung (BAM). This method aims at locating vertical subsurface defects. Here, we couple a laser with a spatial light modulator and trigger its video input to heat a sample surface deterministically with two anti-phased modulated lines while acquiring highly resolved thermal images. The defect position is retrieved from evaluating thermal wave interference minima.

Video: Subsurface Defect Localization by Structured Heating Using Laser Projected Photothermal Thermography

Investigation of Early Plasma Evolution Induced by Ultrashort Laser Pulses

Early plasma is generated owing to high intensity laser irradiation of target and the subsequent target material ionization. Its dynamics plays a significant role in laser-material interaction, especially in the air environment1-11.
Early plasma evolution has been captured through pump-probe shadowgraphy1-3 and interferometry1,4-7. However, the studied time frames and applied laser parameter ranges are limited. For example, direct examinations of plasma front locations and electron number densities within a delay time of 100 picosecond (ps) with respect to the laser pulse peak are still very few, especially for the ultrashort pulse of a duration around 100 femtosecond (fs) and a low power density around 1014 W/cm2. Early plasma generated under these conditions has only been captured recently with high temporal and spatial resolutions12. The detailed setup strategy and procedures of this high precision measurement will be illustrated in this paper. The rationale of the measurement is optical pump-probe shadowgraphy: one ultrashort laser pulse is split to a pump pulse and a probe pulse, while the delay time between them can be adjusted by changing their beam path lengths. The pump pulse ablates the target and generates the early plasma, and the probe pulse propagates through the plasma region and detects the non-uniformity of electron number density. In addition, animations are generated using the calculated results from the simulation model of Ref. 12 to illustrate the plasma formation and evolution with a very high resolution (0.04 ~ 1 ps).
Both the experimental method and the simulation method can be applied to a broad range of time frames and laser parameters. These methods can be used to examine the early plasma generated not only from metals, but also from semiconductors and insulators.

An experimental method to examine the early plasma evolution induced by ultrashort laser pulses is described. Using this method, high quality images of early plasma are obtained with high temporal and spatial resolutions. A novel integrated atomistic model is used to simulate and explain the mechanisms of early plasma.

Early plasma is generated owing to high intensity laser irradiation of target and the subsequent target material ionization. Its dynamics plays a ...

Fabrication of Nano-engineered Transparent Conducting Oxides by Pulsed Laser Deposition

Nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas allows the deposition of metal oxides with tunable morphology, structure, density and stoichiometry by a proper control of the plasma plume expansion dynamics. Such versatility can be exploited to produce nanostructured films from compact and dense to nanoporous characterized by a hierarchical assembly of nano-sized clusters. In particular we describe the detailed methodology to fabricate two types of Al-doped ZnO (AZO) films as transparent electrodes in photovoltaic devices: 1) at low O2 pressure, compact films with electrical conductivity and optical transparency close to the state of the art transparent conducting oxides (TCO) can be deposited at room temperature, to be compatible with thermally sensitive materials such as polymers used in organic photovoltaics (OPVs); 2) highly light scattering hierarchical structures resembling a forest of nano-trees are produced at higher pressures. Such structures show high Haze factor (&gt;80%) and may be exploited to enhance the light trapping capability. The method here described for AZO films can be applied to other metal oxides relevant for technological applications such as TiO2, Al2O3, WO3 and Ag4O4.

We describe the experimental method to deposit nanostructured oxide thin films by nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas. By using this method Al-doped ZnO (AZO) films, from compact to hierarchically structured as nano-tree forests, can be deposited.

Nanosecond Pulsed  Laser Deposition (PLD) in the presence of a background gas allows the deposition  of metal oxides with tunable morphology, structure, ...

Selective Area Modification of Silicon Surface Wettability by Pulsed UV Laser Irradiation in Liquid Environment

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of biosensing devices. We report on a protocol of using KrF and ArF lasers irradiating Si (001) samples immersed in a liquid environment with low number of pulses and operating at moderately low pulse fluences to induce Si wettability modification. Wafers immersed for up to 4 hr in a 0.01% H2O2/H2O solution did not show measurable change in their initial contact angle (CA) ~75&#176;. However, the 500-pulse KrF and ArF lasers irradiation of such wafers in a microchamber filled with 0.01% H2O2/H2O solution at 250 and 65 mJ/cm2, respectively, has decreased the CA to near 15&#176;, indicating the formation of a superhydrophilic surface. The formation of OH-terminated Si (001), with no measurable change of the wafer&#8217;s surface morphology, has been confirmed by X-ray photoelectron spectroscopy and atomic force microscopy measurements. The selective area irradiated samples were then immersed in a biotin-conjugated fluorescein-stained nanospheres solution for 2 hr, resulting in a successful immobilization of the nanospheres in the non-irradiated area. This illustrates the potential of&#160;the method for selective area biofunctionalization and fabrication of advanced Si-based biosensing architectures. We also describe a similar protocol of irradiation of wafers immersed in methanol (CH3OH) using ArF laser operating at pulse fluence of 65 mJ/cm2 and in situ formation of a strongly hydrophobic surface of Si (001) with the CA of 103&#176;. The XPS results indicate ArF laser induced formation of Si&#8211;(OCH3)x compounds responsible for the observed hydrophobicity. However, no such compounds were found by XPS on the Si surface irradiated by KrF laser in methanol, demonstrating the inability of the KrF laser to photodissociate methanol and create -OCH3 radicals.

We report on a process of in situ alteration of HF treated Si (001) surface into a hydrophilic or hydrophobic state by irradiating samples in microfluidic chambers filled with&#160;H2O2/H2O solution (0.01%-0.5%) or methanol solutions using pulsed UV laser of a relative low pulse fluence.

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of ...

Multifunctional Hybrid Fe2O3-Au Nanoparticles for Efficient Plasmonic Heating

One of the most widely used methods for manufacturing colloidal gold nanospherical particles involves the reduction of chloroauric acid (HAuCl4) to neutral gold Au(0) by reducing agents, such as sodium citrate or sodium borohydride. The extension of this method to decorate iron oxide or similar nanoparticles with gold nanoparticles to create multifunctional hybrid Fe2O3-Au nanoparticles is straightforward. This approach yields fairly good control over Au nanoparticle dimensions and loading onto Fe2O3. Additionally, the Au metal size, shape, and loading can easily be tuned by changing experimental parameters (e.g., reactant concentrations, reducing agents, surfactants, etc.). An advantage of this procedure is that the reaction can be done in air or water, and, in principle, is amenable to scaling up. The use of such optically tunable Fe2O3-Au nanoparticles for hyperthermia studies is an attractive option as it capitalizes on plasmonic heating of gold nanoparticles tuned to absorb light strongly in the VIS-NIR region. In addition to its plasmonic effects, nanoscale Au provides a unique surface for interesting chemistries and catalysis. The Fe2O3 material provides additional functionality due to its magnetic property. For example, an external magnetic field could be used to collect and recycle the hybrid Fe2O3-Au nanoparticles after a catalytic experiment, or alternatively, the magnetic Fe2O3 can be used for hyperthermia studies through magnetic heat induction. The photothermal experiment described in this report measures bulk temperature change and nanoparticle solution mass loss as functions of time using infrared thermocouples and a balance, respectively. The ease of sample preparation and the use of readily available equipment are distinct advantages of this technique. A caveat is that these photothermal measurements assess the bulk solution temperature and not the surface of the nanoparticle where the heat is transduced and the temperature is likely to be higher.

Multifunctional Hybrid Fe2O3-Au Nanoparticles for Efficient Plasmonic Heating

We describe the synthesis and properties of multifunctional Fe2O3-Au nanoparticles produced by a wet chemical approach and investigate their photothermal properties using laser irradiation. The composite Fe2O3-Au nanoparticles retain the properties of both materials, creating a multifunctional structure with excellent magnetic and plasmonic properties.

One of the most widely used methods for manufacturing colloidal gold nanospherical particles involves the reduction of chloroauric acid (HAuCl4) to ...

Compact Lens-less Digital Holographic Microscope for MEMS Inspection and Characterization

A micro-electro-mechanical-system (MEMS) is a widely used component in many industries, including energy, biotechnology, medical, communications, and automotive. However, effective inspection and characterization metrology systems are needed to ensure the functional reliability of MEMS. This study presents a system based on digital holography as a tool for MEMS metrology. Digital holography has gained increasing attention in the past 20 years. With the fast development and decreasing cost of sensor arrays, resolution of such systems has increased broadening potential applications. Thus, it has attracted attention from both research and industry sides as a potential reliable tool for industrial metrology. Indeed, by recording the interference pattern between an object beam (which contains sample height information) and a reference beam on a CCD camera, one can retrieve the quantitative phase information of an object. However, most of digital holographic systems are bulky and thus not easy to implement on industry production lines. The novelty of the system presented is that it is lens-less and thus very compact. In this study, it is shown that the Compact Digital Holographic Microscope (CDHM) can be used to evaluate several characteristics typically consider as criteria in MEMS inspections. The surface profiles of MEMS in both static and dynamic conditions are presented. Comparison with AFM is investigated to validate the accuracy of the CDHM.

We present a compact reflection digital holographic system (CDHM) for inspection and characterization of MEMS devices. A lens-less design using a diverging input wave providing natural geometrical magnification is demonstrated. Both static and dynamic studies are presented.

A micro-electro-mechanical-system (MEMS) is a widely used component in many industries, including energy, biotechnology, medical, communications, and ...

Electroactive Polymer Nanoparticles Exhibiting Photothermal Properties

A method for the synthesis of electroactive polymers is demonstrated, starting with the synthesis of extended conjugation monomers using a three-step process that finishes with Negishi coupling. Negishi coupling is a cross-coupling process in which a chemical precursor is first lithiated, followed by transmetallation with ZnCl2. The resultant organozinc compound can be coupled to a dibrominated aromatic precursor to give the conjugated monomer. Polymer films can be prepared via electropolymerization of the monomer and characterized using cyclic voltammetry and ultraviolet-visible-near infrared (UV-Vis-NIR) spectroscopy. Nanoparticles (NPs) are prepared via emulsion polymerization of the monomer using a two-surfactant system to yield an aqueous dispersion of the polymer NPs. The NPs are characterized using dynamic light scattering, electron microscopy, and UV-Vis-NIR-spectroscopy. Cytocompatibility of NPs is investigated using the cell viability assay. Finally, the NP suspensions are irradiated with a NIR laser to determine their effectiveness as potential materials for photothermal therapy (PTT).

A protocol is presented for the synthesis and preparation of nanoparticles consisting of electroactive polymers.

A method for the synthesis of electroactive polymers is demonstrated, starting with the synthesis of extended conjugation monomers using a three-step ...

Automation of Mode Locking in a Nonlinear Polarization Rotation Fiber Laser through Output Polarization Measurements

When a laser is mode-locked, it emits a train of ultra-short pulses at a repetition rate determined by the laser cavity length. This article outlines a new and inexpensive procedure to force mode locking in a pre-adjusted nonlinear polarization rotation fiber laser. This procedure is based on the detection of a sudden change in the output polarization state when mode locking occurs. This change is used to command the alignment of the intra-cavity polarization controller in order to find mode-locking conditions. More specifically, the value of the first Stokes parameter varies when the angle of the polarization controller is swept and, moreover, it undergoes an abrupt variation when the laser enters the mode-locked state. Monitoring this abrupt variation provides a practical easy-to-detect signal that can be used to command the alignment of the polarization controller and drive the laser towards mode locking. This monitoring is achieved by feeding a small portion of the signal to a polarization analyzer measuring the first Stokes parameter. A sudden change in the read out of this parameter from the analyzer will occur when the laser enters the mode-locked state. At this moment, the required angle of the polarization controller is kept fixed. The alignment is completed. This procedure provides an alternate way to existing automating procedures that use equipment such as an optical spectrum analyzer, an RF spectrum analyzer, a photodiode connected to an electronic pulse-counter or a nonlinear detecting scheme based on two-photon absorption or second harmonic generation. It is suitable for lasers mode locked by nonlinear polarization rotation. It is relatively easy to implement, it requires inexpensive means, especially at a wavelength of 1550 nm, and it lowers the production and operation costs incurred in comparison to the above-mentioned techniques.

A protocol to detect and automate mode locking in a pre-adjusted nonlinear polarization rotation fiber laser is presented. The detection of a sudden change in the output polarization state when mode locking occurs is used to command the alignment of an intra-cavity polarization controller in order to find mode-locking conditions.

When a laser is mode-locked, it emits a train of ultra-short pulses at a repetition rate determined by the laser cavity length. This article outlines a ...

Measuring Spray Droplet Size from Agricultural Nozzles Using Laser Diffraction

When making an application of any crop protection material such as an herbicide or pesticide, the applicator uses a variety of skills and information to make an application so that the material reaches the target site (i.e., plant). Information critical in this process is the droplet size that a particular spray nozzle, spray pressure, and spray solution combination generates, as droplet size greatly influences product efficacy and how the spray moves through the environment. Researchers and product manufacturers commonly use laser diffraction equipment to measure the spray droplet size in laboratory wind tunnels. The work presented here describes methods used in making spray droplet size measurements with laser diffraction equipment for both ground and aerial application scenarios that can be used to ensure inter- and intra-laboratory precision while minimizing sampling bias associated with laser diffraction systems. Maintaining critical measurement distances and concurrent airflow throughout the testing process is key to this precision. Real time data quality analysis is also critical to preventing excess variation in the data or extraneous inclusion of erroneous data. Some limitations of this method include atypical spray nozzles, spray solutions or application conditions that result in spray streams that do not fully atomize within the measurement distances discussed. Successful adaption of this method can provide a highly efficient method for evaluation of the performance of agrochemical spray application nozzles under a variety of operational settings. Also discussed are potential experimental design considerations that can be included to enhance functionality of the data collected.

We present protocols to be used in the measurement of spray droplet size from agricultural nozzles used in both aerial and ground based agrochemical applications. These methods presented were developed to provide consistent and repeatable droplet size data both inter- and intra-laboratory, when using laser diffraction systems.

When making an application of any crop protection material such as an herbicide or pesticide, the applicator uses a variety of skills and information to ...

Quantitative Analysis of Vacuum Induction Melting by Laser-induced Breakdown Spectroscopy

Vacuum induction melting is a popular method for refining high purity metal and alloys. Traditionally, standard process control in metallurgy involves several steps, include drawing samples, cooling, cutting, transport to the laboratory, and analysis. The whole analysis process requires more than 30 minutes, which hinders on-line process control. Laser-induced breakdown spectroscopy is an excellent on-line analysis method that can satisfy the requirements of vacuum induction melting because it is fast and noncontact and does not require sample preparation. The experimental facility uses a lamp-pumped Q-switched laser to ablate melted liquid steel with an output energy of 80 mJ, a frequency of 5 Hz, a FWHM pulse width of 20 ns, and a working wavelength of 1,064 nm. A multi-channel linear charge coupled device (CCD) spectrometer is used to measure the emission spectrum in real time, with a spectral range from 190 to 600 nm and a resolution of 0.06 nm at a wavelength of 200 nm. The protocol includes several steps: standard alloy sample preparation and an ingredient test, smelting of standard samples and determination of the laser breakdown spectrum, and construction of the elements concentration quantitative analysis curve of each element. To realize the concentration analysis of unknown samples, the spectrum of a sample also needs to be measured and disposed with the same process. The composition of all main elements in the melted alloy can be quantitatively analyzed with an internal standard method. The calibration curve shows that the limit of detection of most metal elements ranges from 20-250 ppm. The concentration of elements, such as Ti, Mo, Nb, V, and Cu, can be lower than 100 ppm, and the concentrations of Cr, Al, Co, Fe, Mn, C, and Si range from 100-200 ppm. The R2 of some calibration curves can exceed 0.94.

During vacuum induction melting, laser-induced breakdown spectroscopy is used to perform real-time quantitative analysis of the main-ingredient elements of a molten alloy.

Vacuum induction melting is a popular method for refining high purity metal and alloys. Traditionally, standard process control in metallurgy involves ...

Pore-scale Imaging and Characterization of Hydrocarbon Reservoir Rock Wettability at Subsurface Conditions Using X-ray Microtomography

In situ wettability measurements in hydrocarbon reservoir rocks have only been possible recently. The purpose of this work is to present a protocol to characterize the complex wetting conditions of hydrocarbon reservoir rock using pore-scale three-dimensional X-ray imaging at subsurface conditions. In this work, heterogeneous carbonate reservoir rocks, extracted from a very large producing oil field, have been used to demonstrate the protocol. The rocks are saturated with brine and oil and aged over three weeks at subsurface conditions to replicate the wettability conditions that typically exist in hydrocarbon reservoirs (known as mixed-wettability). After the brine injection, high-resolution three-dimensional images (2 &#181;m/voxel) are acquired and then processed and segmented. To calculate the distribution of the contact angle, which defines the wettability, the following steps are performed. First, fluid-fluid and fluid-rock surfaces are meshed. The surfaces are smoothed to remove voxel artefacts, and in situ contact angles are measured at the three-phase contact line throughout the whole image. The main advantage of this method is its ability to characterize in situ wettability accounting for pore-scale rock properties, such as rock surface roughness, rock chemical composition, and pore size. The in situ wettability is determined rapidly at hundreds of thousands of points. 
The method is limited by the segmentation accuracy and X-ray image resolution. This protocol could be used to characterize the wettability of other complex rocks saturated with different fluids and at different conditions for a variety of applications. For example, it could help in determining the optimal wettability that could yield an extra oil recovery (i.e., designing brine salinity accordingly to obtain higher oil recovery) and to find the most efficient wetting conditions to trap more CO2 in subsurface formations.

This protocol is presented to characterize the complex wetting conditions of an opaque porous medium (hydrocarbon reservoir rock) using three-dimensional images obtained by X-ray microtomography at subsurface conditions.

In situ wettability measurements in hydrocarbon reservoir rocks have only been possible recently. The purpose of this work is to present a protocol to ...