Name: in depth analyses of leds by a combination of x-ray computed tomography (ct) and light microscopy (lm) correlated with scanning electron microscopy (sem)
Uploaded: 2016-06-16T13:00:00
Description: Watch this Scientific Journal Video about In Depth Analyses of LEDs by a Combination of X-ray Computed Tomography CT and Light Microscopy LM Correlated with Scanning Electron Microscopy SEM at JoVE.co

The authors kindly acknowledge financial support from the &#34;Akademische Gesellschaft Lippstadt&#34; as well as from the &#34;Ministerium f&#252;r Innovation, Wissenschaft und Forschung des Landes Nordrhein-Westfalen&#34;. Photographs in Figures 1, 2 and 5 courtesy to Markus Horstmann, Hamm-Lippstadt University of Applied Sciences.

1. Sample Preparation for X-ray Computed Tomography (CT)
<ol>
	<li>Glue sample (LED cf. materials section) to a 2 mm &#216; hollow carbon fiber bar of appropriate length using hot-melt adhesive.</li>
	<li>Adjust position of specimen by using a hot-air gun if needed. Fix the sample in the CT-sample chamber using the three-jaw chuck.</li>
</ol>
2. CT Measurement Setup
<ol>
	<li>Perform warmup and centering procedures according to the control software of the X-ray tube. 
	NOTE: Use ...

<ol>
	<li>Mueller-Mach, R., Mueller, G. O., Krames, M. R., Trottier, T. <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+phosphor-converted+light-emitting+diodes+based+on+III-Nitrides.">High-power phosphor-converted light-emitting diodes based on III-Nitrides.</a> IEEE J. Sel. Top. Quantum Electron. 8 (2), 339-345 (2002).</li><li>Branas, C., Azcondo, F. J., Alonso, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solid-State+Lighting:+A+System+Review.">Solid-State Lighting: A System Review.</a> IEEE Ind. Electron. Mag. 7 (4), 6-14 (2013).</li><li>Chang, M. -. H., Das, D., Varde, P. V., Pecht, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Light+emitting+diodes+reliability+review.">Light emitting diodes reliability review.</a> Microelectron. Reliab. 52 (5), 762-782 (2012).</li><li>Ayodha, T., Han, H. S., Kim, J., Kim, S. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+chip+die+bonding+on+thermal+resistance+of+high+power+LEDs.">Effect of chip die bonding on thermal resistance of high power LEDs.</a> Intersoc. Conf. Therm. Thermomechanical Phenom. Electron. Syst. ITHERM. , 957-961 (2012).</li><li>Cason, M., Estrada, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Application+of+X-ray+MicroCT+for+non-destructive+failure+analysis+and+package+construction+characterization.">Application of X-ray MicroCT for non-destructive failure analysis and package construction characterization.</a> Proc. Int. Symp. Phys. Fail. Anal. Integr. Circuits, IPFA. , (2011).</li><li>Chen, R., Zhang, Q., Peng, T., Jiao, F., Liu, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Failure+analysis+techniques+for+high+power+light+emitting+diodes.">Failure analysis techniques for high power light emitting diodes.</a> 2011 12th Int. Conf. Electron. Packag. Technol. High Density Packag. , 1-4 (2011).</li><li>Chen, Z., Zhang, Q., 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=Study+on+the+reliability+of+application-specific+led+package+by+thermal+shock+testing,+failure+analysis,+and+fluid-solid+coupling+thermo-mechanical+simulation.">Study on the reliability of application-specific led package by thermal shock testing, failure analysis, and fluid-solid coupling thermo-mechanical simulation.</a> IEEE Trans. Components, Packag. Manuf. Technol. 2 (7), 1135-1142 (2012).</li><li>Luniak, M., Holtge, H., Brodmann, R., Wolter, K. -. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Optical+Characterization+of+Electronic+Packages+with+Confocal+Microscopy.">Optical Characterization of Electronic Packages with Confocal Microscopy.</a> 2006 1st Electron. Syst. Technol. Conf. 2 (16), 1813-1815 (2006).</li><li>Marks, M. R., Hassan, Z., Cheong, K. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+Methods+for+Ultrathin+Wafer+and+Die+Quality:+A+Review.">Characterization Methods for Ultrathin Wafer and Die Quality: A Review.</a> IEEE Trans. Components, Packag. Manuf. Technol. 4 (12), 2042-2057 (2014).</li><li>Rosc, J., Hammer, 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=Reliability+assessment+of+contact+wires+in+LED-devices+using+in+situ+X-ray+computed+tomography+and+thermo-mechanical+simulations.">Reliability assessment of contact wires in LED-devices using in situ X-ray computed tomography and thermo-mechanical simulations.</a> Proc. 5th Electron. Syst. Technol. Conf. , 1-6 (2014).</li><li>Zhaohui, C., Qin, Z., Kai, W., Xiaobing, L., Sheng, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reliability+test+and+failure+analysis+of+high+power+LED+packages.">Reliability test and failure analysis of high power LED packages.</a> J. Semicond. 32 (1), 014007 (2011).</li><li>Hamon, B., Bataillou, B., Hamon, B., Mendizabal, L., Gasse, A., Feuillet, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=N-contacts+degradation+analysis+of+white+flip+chip+LEDs+during+reliability+tests.">N-contacts degradation analysis of white flip chip LEDs during reliability tests.</a> 2014 IEEE Int. Reliab. Phys. Symp. , FA.1.1-FA.1.6 (2014).</li><li>Tsai, M. -. Y., Tang, C. -. Y., Yen, C. -. Y., Chang, L. -. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bump+and+Underfill+Effects+on+Thermal+Behaviors+of+Flip-Chip+LED+Packages:+Measurement+and+Modeling.">Bump and Underfill Effects on Thermal Behaviors of Flip-Chip LED Packages: Measurement and Modeling.</a> IEEE Trans. Device Mater. Reliab. 14 (1), 161-168 (2014).</li><li>Wang, F. -. K., Lu, Y. -. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Useful+lifetime+analysis+for+high-power+white+LEDs.">Useful lifetime analysis for high-power white LEDs.</a> Microelectron. Reliab. 54 (6-7), 1307-1315 (2014).</li><li>Liu, Y., Zhao, J., Yuan, C. C. -. A., Zhang, G. Q., Sun, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chip-on-Flexible+Packaging+for+High-Power+Flip-Chip+Light-Emitting+Diode+by+AuSn+and+SAC+Soldering.">Chip-on-Flexible Packaging for High-Power Flip-Chip Light-Emitting Diode by AuSn and SAC Soldering.</a> IEEE Trans. Components, Packag. Manuf. Technol. 4 (11), 1754-1759 (2014).</li><li>Thomas, C., Edelmann, M., Lysenkov, D., Hafner, C., Bernthaler, T., Schneider, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Correlative+Light+and+Electron+Microscopy+(CLEM)+for+Characterization+of+Lithium+Ion+Battery+Materials.">Correlative Light and Electron Microscopy (CLEM) for Characterization of Lithium Ion Battery Materials.</a> Microsc. Microanal. 16, 784-785 (2010).</li><li>Thomas, C., Ogbazghi, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Correlative+Microscopy+of+Optical+Materials.">Correlative Microscopy of Optical Materials.</a> Imaging &amp; Microscopy. 3, 32-34 (2014).</li></ol>

The advantages of this multimodal approach consist in the location-dependent correlation of the acquired data. The multimodal approach described here should be contrasted in subsequent analyses with each technique separately. For example, luminescence properties visible in LM can be linked to compositions as detected using SEM/EDS. The volume information obtained by CT can be extended with in depth analyses of cross-sections prepared in a targeted fashion. CT data also enable fast location of possible areas of interest i...

This article demonstrates the potential and advantages of a combination of X-ray computed tomography (CT) with correlative light and electron microscopy (CLEM) for the exemplary in depth characterization of light emitting diodes (LED). With this technique it is possible to plan the micro preparation of the LED in such a fashion that while a cross section can be imaged microscopically the electrical functionality is preserved in the remainder of the specimen. The procedure has several unique features: firstly, the planned micro preparation by aid of the rendered volume of the entire sample obtained by CT; secondly, the observation of the LED by light microscopy (LM) with the complete variety of imaging techniques available (bright and dark field, polarization contrast, etc.); thirdly, observation of the LED in operation by LM; fourthly, observation of identical regions with the full variety of electron microscopy imaging techniques comprising secondary electron (SE) and back scatter electron (BSE) imaging, as well as energy dispersive X-ray fluorescence spectroscopy (EDX).
LEDs for illumination applications are designed to emit white light, although in certain applications color variability may be favorable. This broad emission cannot be achieved by emission from one compound semiconductor, since LEDs emit radiation in a narrow spectral band (circa 30 nm full width half maximum (FWHM)). Therefore white LED light is commonly generated by the combination a blue LED with phosphors which convert the short-wavelength radiation into broad emission over a large spectral range1. Color variable LED solutions usually make use of at least three primaries, which generally results in higher market prices.2
The use of either CT, LM or SEM is of course well established (e.g., in failure analysis for LEDs3-15), however the comprehensive and purposeful combination of all three techniques described here may offer new insights and will enable faster tracks towards meaningful characterization results.
From 3D microstructural analysis of the packaged device in CT the regions of interest (ROIs) can be identified and selected. With this non-destructive method, electrical connections can also be identified and considered for further preparation. The precise preparation of a 2D cross section allows investigations of the device in operation despite the destructive nature of this method. The cross section can now be characterized by CLEM16,17 which enables a very efficient and flexible characterization of identical ROIs with LM as well as SEM. By this approach, the advantages of both microscopy techniques can be combined. For example, a fast identification of ROIs in the LM is followed by high-resolution imaging in the SEM. But furthermore, the correlation of information from the LM (e.g., color, optical properties, particle distribution) with the visualization and analysis techniques of the SEM (e.g., particle size, surface morphology, element distribution) allows a deeper understanding of functional behavior and microstructure within a white LED.

<table border="0" cellpadding="0" cellspacing="0" width="758">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">X-Ray Computer Tomograph</td>
			<td style="width:119px;">General Electric</td>
			<td style="width:139px;">not applicable</td>
			<td style="width:239px;">type: nanotom s research edition</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:263px;">acquisition software</td>
			<td style="width:119px;">General Electric</td>
			<td style="width:139px;">not applicable</td>
			<td>phoenix Datos| x2 acquisition and corresponding manual</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:263px;">reconstruction software</td>
			<td style="width:119px;">General Electric</td>
			<td style="width:139px;">not applicable</td>
			<td>phoenix Datos| x2 acquisition and corresponding manual</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">rendering software</td>
			<td style="width:119px;">Volume Graphics</td>
			<td style="width:139px;">not applicable</td>
			<td>VGStudio Max 2.2 and corresponding manual</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">grinder (manual)</td>
			<td style="width:119px;">Struers</td>
			<td align="right" style="width:139px;">5296327</td>
			<td>Labopol 21</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">sample holder</td>
			<td style="width:119px;">Struers</td>
			<td align="right" style="width:139px;">4886102</td>
			<td>UniForce</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">grinder (automated)</td>
			<td style="width:119px;">Struers</td>
			<td align="right" style="width:139px;">6026127</td>
			<td>Tegramin 25</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:263px;">epoxy resin/hardener</td>
			<td style="width:119px;">Struers</td>
			<td style="width:139px;">40200030/40200031</td>
			<td>Epoxy fix resin / Epoxy fix hardener</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">Ethanol</td>
			<td style="width:119px;">Struers</td>
			<td align="right" style="width:139px;">950301</td>
			<td>Kleenol</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">Light Microscope</td>
			<td style="width:119px;">Zeiss</td>
			<td style="width:139px;">not applicable</td>
			<td>Axio Imager M2m&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">Electron Microscope</td>
			<td style="width:119px;">Zeiss</td>
			<td style="width:139px;">not applicable</td>
			<td>Sigma&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">CLEM software</td>
			<td style="width:119px;">Zeiss</td>
			<td style="width:139px;">not applicable</td>
			<td>Axio Vision SE64 Rel.4.9 and corresponding manual</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">CLEM sample holder</td>
			<td style="width:119px;">Zeiss</td>
			<td style="width:139px;">432335-9101-000</td>
			<td>Specimen holder CorrMic MAT Universal B</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">SEM Adapter for CLEM sample holder</td>
			<td style="width:119px;">Zeiss</td>
			<td style="width:139px;">432335-9151-000</td>
			<td>SEM Adapter for Specimen holder CorrMic MAT Universal B</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">sputter coater</td>
			<td style="width:119px;">Quorum</td>
			<td style="width:139px;">not applicable</td>
			<td>Q150TES</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">EDS detector</td>
			<td style="width:119px;">R&#246;ntec</td>
			<td style="width:139px;">not applicable</td>
			<td>X-Flash 1106</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">solder</td>
			<td style="width:119px;">Stannol</td>
			<td align="right" style="width:139px;">535251</td>
			<td>type: HS10</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:263px;">LED</td>
			<td style="width:119px;">Lumileds</td>
			<td style="width:139px;">not applicable</td>
			<td>LUXEON Rebel warm white, research sample</td>
		</tr>
	</tbody>
</table>

in depth analyses of leds by a combination of x-ray computed tomography (ct) and light microscopy (lm) correlated with scanning electron microscopy (sem)

In failure analysis, device characterization and reverse engineering of light emitting diodes (LEDs), and similar electronic components of micro-characterization, plays an important role. Commonly, different techniques like X-ray computed tomography (CT), light microscopy (LM) and scanning electron microscopy (SEM) are used separately. Similarly, the results have to be treated for each technique independently. Here a comprehensive study is shown which demonstrates the potentials leveraged by linking CT, LM and SEM. In depth characterization is performed on a white emitting LED, which can be operated throughout all characterization steps. Major advantages are: planned preparation of defined cross sections, correlation of optical properties to structural and compositional information, as well as reliable identification of different functional regions. This results from the breadth of information available from identical regions of interest (ROIs): polarization contrast, bright and dark-field LM images, as well as optical images of the LED cross section in operation. This is supplemented by SEM imaging techniques and micro-analysis using energy dispersive X-ray spectroscopy.

The characterized LED is shown in Figure 1. It is a white emitting LED with a Chip size of 1 x 1 mm2 and a partially ceramic luminescent color converter. Gluing the LED in a slightly slanted position onto a carbon fiber bar avoids CT artifacts caused by sample symmetry (Figure 2). Results of the CT measurement allow for planning the position of the cross section of the sample, and ensure electrical operability after partial abrasion (Fi...

Watch this Scientific Journal Video about In Depth Analyses of LEDs by a Combination of X-ray Computed Tomography CT and Light Microscopy LM Correlated with Scanning Electron Microscopy SEM at JoVE.co

In Depth Analyses of LEDs by a Combination of X-ray Computed Tomography CT and Light Microscopy LM Correlated with Scanning Electron Microscopy SEM

A workflow for comprehensive micro-characterization of active optical devices is outlined. It contains structural as well as functional investigations by means of CT, LM and SEM. The method is demonstrated for a white LED which can be still be operated during characterization.

In Depth Analyses of LEDs by a Combination of X-ray Computed Tomography (CT) and Light Microscopy (LM) Correlated with Scanning Electron Microscopy (SEM)

In failure analysis, device characterization and reverse engineering of light emitting diodes (LEDs), and similar electronic components of ...

The overall goal of this multimodal micro-characterization procedure is to provide a method for the location-dependent correlation of the data acquired by X-ray Computed Tomography, Light Microscopy and Scanning Electron Microscopy. This method can help answer key questions in the micro-characterization field such as failure analysis or reverse engineering of microelectronic devices. The main advantage of this technique is that optical properties of a sample may be linked to the microstructure and even to submicrometer structural details.The implications of this technique extends toward prevention of device failure because optical defects or in homogeneities can definitively and traceably be linked to structural or electrical defects of the devices. So this method can provide insight into microelectronic devices. It can also be applied to other structural analysis such as characterization of composite materials.Begin this procedure with simple preparation and CT measurement setup as described in text protocol. Select the region of interest or ROI by identifying the area not obscured by the measured object during one full rotation. In the measurement window with the live image press and hold the left mouse button and draw a red frame window.Right-click on this window's frame to open a context menu. Then select Set as Observation Window. The frame's color will change to yellow and the observation window will be fixed in the measurement window.Activate the software module Auto-scan Optimizer, through which nine images are taken before the actual scan of the sample. These are images are taken in 40-degree steps while rotating the sample. Simultaneously, activate the module Detector Shift routine.The simultaneous activation of these two modules before starting the actual CT scan ensures correction for movements of the sample and for ring artifacts. Next, scan the sample by starting the Data Acquisition routine in the acquisition software. Transfer the reconstruction data to the CT Data Analysis software and align the sample in X-Y, X-Z and Y-Z planes using the simple registration function in the software.Apply median filtering using a filter size of 3. For micro preparation embed LED in epoxy resin using transparent supports. Drill two small holes on opposite sides of the support and feed the silver wire through it.At this point it's crucial the carefully position of the sample. If the deviation from the ideal position is defined by the CT scan as too big, electrical failures may result and the protocol will have to be started from the beginning. Position the LED by means of tightening or loosening the silver wire to align the front edge of the LED and the support.Fill the ring with epoxy inside a silicon beaker pre-treated to ensure that it will not stick to the epoxy. Then, allow the epoxy to harden. Mechanically remove any excessive resin by grinding with coarse-abrasive paper.Using a stereo microscope, visually ensure that the support and LED are aligned, then fix the LED embedded in the epoxy resin in a planer fashion to a simple holder for precision grinding. Use a grinder with abrasion measurement and remove the sample surface up to 100 microns from the targeted plane's position. After polishing, observe the smooth and scratch-free surface using a stereo microscope.Clean the specimen with de-ionized water and cotton pads, then remove the water by rinsing with ethanol, and drying using a hair dryer. Melt the specimen in an appropriate sample holder for Correlative Light and Electron Microscopy, or CLEM for short. Ensure that the sample holder fixes the sample for use in LM, sputter coater and SEM.Adjust the calibration marks to the same height as sample's surface. Ensure that the polished surface is parallel to the focal plane of the LM.Next, fix the sample holder on to the motorized X-Y stage of the LM.Connect the LED to the power supply. The power supply should operate in constant current mode.Using the microscope software, calibrate the sample holder position on the X-Y stage by saving the position of calibration marks as reference points. Move the X-Y stage of the LM such that the ROI of the sample is in the field of view of the LM.Switch on the power supply and tune the LED emission. Switch off LM illumination and adjust the exposure time of the LM camera.Obtain the LM image of the light distribution within the sample. If applicable, image luminescence together with other contrasts by activating LM Illumination and LED simultaneously. Save all LM images together with the corresponding stage position as described in the user manual.Prepare for SEM analysis by sputter coating the sample and performing setup as described in the text protocol. Move the stage to show the ROI on the sample and perform SEM analysis in the same location as done for LM.Select Backscattered Electron Detector for material contrast. For this sample, choose an Electron Energy of 20 keV.Set the aperture to 30 microns and position the sample at a working distance of 8.7 mm. Select Secondary Electron Detector for microstructure surface imaging. Then change to EDS Detector for element mapping.For this sample, select an aperture of 60 microns to increase the beam current, and position the sample at a working distance of 9 mm. Representative results for the Micro-characterization of an electrically operable LED are shown here. Here is the specimen prepared for a CT scan, with chip surface of 1 squared mm.Reconstructive CT volume information enables planning of cutting planes for micro-preparation. By carefully positioning the cross section of the sample, electrical operability after partial operation is ensured. Information of the luminescence behavior is gained by optical microscopy of the electrically-driven LED.Blue emission of the semiconductor is well distinguished from red and yellow emission of the phosphors using this device. Overlay of the light microscopy images with SE Microgras through Correlated Microscopy enhances information depth. In this example, the microstructure of the two phosphors is revealed.Further information may be gained by energy Dispersive X-ray Fluorescence Spectroscopy overlays. Once mastered the fluid device characterization including all models shown can be done in 48 hours if it's performed properly. While attempting this procedure it's important to remember to check repeatedly for device operability during cross section preparation.Following this procedure, other methods like Fluorescence Microscopy can be performed in order to answer additional questions like excitation and emission behavior of the phosphors. This technique enables researchers in the field of micro-characterization to explore electro-optical devices in full function.

in-depth-analyses-leds-combination-x-ray-computed-tomography-ct-light

Research

JoVE Journal

Engineering

Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial resolution, and is even capable of providing atomically resolved elemental maps. In this technique, a highly focused electron beam is incident upon a thin sample and the energy of emitted X-rays is measured in order to determine the atomic species of material within the beam path. This elementally sensitive spectroscopy technique can be extended to three dimensional tomographic imaging by acquiring multiple spectrum images with the sample tilted along an axis perpendicular to the electron beam direction.
Elemental distributions within single nanoparticles are often important for determining their optical, catalytic and magnetic properties. Techniques such as X-ray tomography and slice and view energy dispersive X-ray mapping in the scanning electron microscope provide elementally sensitive three dimensional imaging but are typically limited to spatial resolutions of &gt; 20 nm. Atom probe tomography provides near atomic resolution but preparing nanoparticle samples for atom probe analysis is often challenging. Thus, elementally sensitive techniques applied within the scanning transmission electron microscope are uniquely placed to study elemental distributions within nanoparticles of dimensions 10-100 nm.
Here, energy dispersive X-ray (EDX) spectroscopy within the STEM is applied to investigate the distribution of elements in single AgAu nanoparticles. The surface segregation of both Ag and Au, at different nanoparticle compositions, has been observed.

The use of energy dispersive X-ray tomography in the scanning transmission electron microscope to characterize elemental distributions within single nanoparticles in three dimensions is described.

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial ...

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Measurement of X-ray Beam Coherence along Multiple Directions Using 2-D Checkerboard Phase Grating

A procedure for a technique to measure the transverse coherence of synchrotron radiation X-ray sources using a single phase grating interferometer is reported. The measurements were demonstrated at the 1-BM bending magnet beamline of the Advanced Photon Source (APS) at Argonne National Laboratory (ANL). By using a 2-D checkerboard &#960;/2 phase-shift grating, transverse coherence lengths were obtained along the vertical and horizontal directions as well as along the 45&#176; and 135&#176; directions to the horizontal direction. Following the technical details specified in this paper, interferograms were measured at different positions downstream of the phase grating along the beam propagation direction. Visibility values of each interferogram were extracted from analyzing harmonic peaks in its Fourier Transformed image. Consequently, the coherence length along each direction can be extracted from the evolution of visibility as a function of the grating-to-detector distance. The simultaneous measurement of coherence lengths in four directions helped identify the elliptical shape of the coherence area of the Gaussian-shaped X-ray source. The reported technique for multiple-direction coherence characterization is important for selecting the appropriate sample size and orientation as well as for correcting the partial coherence effects in coherence scattering experiments. This technique can also be applied for assessing coherence preserving capabilities of X-ray optics.

The measurement protocol and data analysis procedure are given for obtaining transverse coherence of a synchrotron radiation X-ray source along four directions simultaneously using a single 2-D checkerboard phase grating. This simple technique can be applied for complete transverse coherence characterization of X-ray sources and X-ray optics.

A procedure for a technique to measure the transverse coherence of synchrotron radiation X-ray sources using a single phase grating interferometer is ...

Dynamic Pore-scale Reservoir-condition Imaging of Reaction in Carbonates Using Synchrotron Fast Tomography

Underground storage permanence is a major concern for carbon capture and storage. Pumping CO2 into carbonate reservoirs has the potential to dissolve geologic seals and allow CO2 to escape. However, the dissolution processes at reservoir conditions are poorly understood. Thus, time-resolved experiments are needed to observe and predict the nature and rate of dissolution at the pore scale. Synchrotron fast tomography is a method of taking high-resolution time-resolved images of complex pore structures much more quickly than traditional &#181;-CT. The Diamond Lightsource Pink Beam was used to dynamically image dissolution of limestone in the presence of CO2-saturated brine at reservoir conditions. 100 scans were taken at a 6.1 &#181;m resolution over a period of 2 hours. The images were segmented and the porosity and permeability were measured using image analysis and network extraction. Porosity increased uniformly along the length of the sample; however, the rate of increase of both porosity and permeability slowed at later times.

Synchrotron fast tomography was used to dynamically image dissolution of limestone in the presence of CO2-saturated brine at reservoir conditions. 100 scans were taken at a 6.1 &#181;m resolution over a period of 2 h.

Underground storage permanence is a major concern for carbon capture and storage. Pumping CO2 into carbonate reservoirs has the potential to dissolve ...

Comprehensive Characterization of Extended Defects in Semiconductor Materials by a Scanning Electron Microscope

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications of semiconductor materials. However, it is still under debate how the defect structure determines the band structure, and therefore, the recombination behavior of electron-hole pairs responsible for the optical and electrical properties of the extended defects. The present paper is a survey of procedures for the spatially resolved investigation of structural and of physical properties of extended defects in semiconductor materials with a scanning electron microscope (SEM). Representative examples are given for crystalline silicon. The luminescence behavior of extended defects can be investigated by cathodoluminescence (CL) measurements. They are particularly valuable because spectrally and spatially resolved information can be obtained simultaneously. For silicon, with an indirect electronic band structure, CL measurements should be carried out at low temperatures down to 5 K due to the low fraction of radiative recombination processes in comparison to non-radiative transitions at room temperature. For the study of the electrical properties of extended defects, the electron beam induced current (EBIC) technique can be applied. The EBIC image reflects the local distribution of defects due to the increased charge-carrier recombination in their vicinity. The procedure for EBIC investigations is described for measurements at room temperature and at low temperatures. Internal strain fields arising from extended defects can be determined quantitatively by cross-correlation electron backscatter diffraction (ccEBSD). This method is challenging because of the necessary preparation of the sample surface and because of the quality of the diffraction patterns which are recorded during the mapping of the sample. The spatial resolution of the three experimental techniques is compared.

The optical, electrical, and structural properties of dislocations and of grain boundaries in semiconductor materials can be determined by experiments performed in a scanning electron microscope. Electron microscopy has been used to investigate cathodoluminescence, electron beam induced current, and diffraction of backscattered electrons.

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications ...

Studying Dynamic Processes of Nano-sized Objects in Liquid using Scanning Transmission Electron Microscopy

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a microfluidic chamber assembled in the specimen holder for Transmission Electron Microscopy (TEM) and STEM. The microfluidic system consists of two silicon microchips supporting thin Silicon Nitride (SiN) membrane windows. This article describes the basic steps of sample loading and data acquisition. Most important of all is to ensure that the liquid compartment is correctly assembled, thus providing a thin liquid layer and a vacuum seal. This protocol also includes a number of tests necessary to perform during sample loading in order to ensure correct assembly. Once the sample is loaded in the electron microscope, the liquid thickness needs to be measured. Incorrect assembly may result in a too-thick liquid, while a too-thin liquid may indicate the absence of liquid, such as when a bubble is formed. Finally, the protocol explains how images are taken and how dynamic processes can be studied. A sample containing AuNPs is imaged both in pure water and in saline.

This protocol describes the operation of a liquid flow specimen holder for scanning transmission electron microscopy of AuNPs in water, as used for the observation of nanoscale dynamic processes.

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a ...

Precision Milling of Carbon Nanotube Forests Using Low Pressure Scanning Electron Microscopy

A nanoscale fabrication technique appropriate for milling carbon nanotube (CNT) forests is described. The technique utilizes an environmental scanning electron microscope (ESEM) operating with a low pressure water vapor ambient. In this technique, a portion of the electron beam interacts with the water vapor in the vicinity of the CNT sample, dissociating the water molecules into hydroxyl radicals and other species by radiolysis. The remainder of the electron beam interacts with the CNT forest sample, making it susceptible to oxidation from the chemical products of radiolysis. This technique may be used to trim a selected region of an individual CNT, or it may be used to remove hundreds of cubic microns of material by adjusting ESEM parameters. The machining resolution is similar to the imaging resolution of the ESEM itself. The technique produces only small quantities of carbon residue along the boundaries of the cutting zone, with minimal effect on the native structural morphology of the CNT forest.

Low pressure scanning electron microscopy in a water vapor ambient is used to machine nanoscale to microscale features in carbon nanotube forests.

A nanoscale fabrication technique appropriate for milling carbon nanotube (CNT) forests is described. The technique utilizes an environmental scanning ...

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder microdiffraction two-dimensional (2D) maps at beamline 12.3.2 of the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. Measurements can be performed on any sample that is less than 10 cm x 10 cm x 5 cm, with a flat exposed surface. The experimental geometry is calibrated using standard materials (elemental standards for XRF, and crystalline samples such as Si, quartz, or Al2O3 for diffraction). Samples are aligned to the focal point of the x-ray microbeam, and raster scans are performed, where each pixel of a map corresponds to one measurement, e.g., one XRF spectrum or one diffraction pattern. The data are then processed using the in-house developed software XMAS, which outputs text files, where each row corresponds to a pixel position. Representative data from moissanite and an olive snail shell are presented to demonstrate data quality, collection, and analysis strategies.

We describe a beamline setup meant to carry out rapid two-dimensional x-ray fluorescence and x-ray microdiffraction mapping of single crystal or powder samples using either Laue (polychromatic radiation) or powder (monochromatic radiation) diffraction. The resulting maps give information about strain, orientation, phase distribution, and plastic deformation.

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder ...

X-ray Beam Induced Current Measurements for Multi-Modal X-ray Microscopy of Solar Cells

X-ray beam induced current (XBIC) measurements allow mapping of&#160;the nanoscale performance of electronic devices such as solar cells. Ideally, XBIC is employed simultaneously with other techniques within a multi-modal X-ray microscopy approach. An example is given herein combining XBIC with X-ray fluorescence to enable point-by-point correlations of the electrical performance with chemical composition. For the highest signal-to-noise ratio in XBIC measurements, lock-in amplification plays a crucial role. By this approach, the X-ray beam is modulated by an optical chopper upstream of the sample. The modulated X-ray beam induced electrical signal is amplified and demodulated to the chopper frequency using a lock-in amplifier. By optimizing low-pass filter settings, modulation frequency, and amplification amplitudes, noise can efficiently be suppressed for the extraction of a clear XBIC signal. A similar setup can be used to measure the X-ray beam induced voltage (XBIV). Beyond standard XBIC/XBIV measurements, XBIC can be measured with bias light or bias voltage applied such that outdoor working conditions of solar cells can be reproduced during in-situ and operando measurements. Ultimately, the multi-modal and multi-dimensional evaluation of electronic devices at the nanoscale enables new insights into the complex dependencies between composition, structure, and performance, which is an important step towards solving the materials&#39; paradigm.

A setup for X-ray beam induced current measurements at synchrotron beamlines is described. It unveils the nanoscale performance of solar cells and extends the suite of techniques for multi-modal X-ray microscopy. From wiring to signal-to-noise optimization, it is shown how to perform state-of-the-art XBIC measurements at a hard X-ray microprobe.

X-ray beam induced current (XBIC) measurements allow mapping of&#160;the nanoscale performance of electronic devices such as solar cells. Ideally, XBIC is ...

Graphene-Assisted Quasi-van der Waals Epitaxy of AlN Film on Nano-Patterned Sapphire Substrate for Ultraviolet Light Emitting Diodes

This protocol demonstrates a method for graphene-assisted quick growth and coalescence of AlN on nano-pattened sapphire substrate (NPSS). Graphene layers are directly grown on NPSS using catalyst-free atmospheric-pressure chemical vapor deposition (APCVD). By applying nitrogen reactive ion etching (RIE) plasma treatment, defects are introduced into the graphene film to enhance chemical reactivity. During metal-organic chemical vapor deposition (MOCVD) growth of AlN, this N-plasma treated graphene buffer enables AlN quick growth, and coalescence on NPSS is confirmed by cross-sectional scanning electron microscopy (SEM). The high quality of AlN on graphene-NPSS is then evaluated by X-ray rocking curves (XRCs) with narrow (0002) and (10-12) full width at half-maximum (FWHM) as 267.2 arcsec and 503.4 arcsec, respectively. Compared to bare NPSS, AlN growth on graphene-NPSS shows significant reduction of residual stress from 0.87 GPa to 0.25 Gpa, based on Raman measurements. Followed by AlGaN multiple quantum wells (MQWS) growth on graphene-NPSS, AlGaN-based deep ultraviolet light-emitting-diodes (DUV LEDs) are fabricated. The fabricated DUV-LEDs also demonstrate obvious, enhanced luminescence performance. This work provides a new solution for the growth of high quality AlN and fabrication of high performance DUV-LEDs using a shorter process and less costs.

A protocol for graphene-assisted growth of high-quality AlN films on nano-patterned sapphire substrate is presented.

This protocol demonstrates a method for graphene-assisted quick growth and coalescence of AlN on nano-pattened sapphire substrate (NPSS). Graphene layers ...