Name: experimental methods for spin- and angle-resolved photoemission spectroscopy combined with polarization-variable laser
Uploaded: 2018-06-28T13:00:00
Description: Watch this Scientific Journal Video about Experimental Methods for Spin- and Angle-Resolved Photoemission Spectroscopy Combined with Polarization-Variable Laser at JoVE.com

We thank M. Nakayama, S. Toyohisa, A. Fukushima and Y. Ishida for supports to the experimental setup. We gratefully acknowledge funding from the JSPS Grantin-Aid for Scientific Research (B) through Project No. 26287061 and for Young Scientists (B) through Project No. 15K17675. This work was also supported by MEXT of Japan (Innovative Area &#34;Topological Materials Science,&#34; Grant No. 16H00979) and JSPS KAKENHI (Grant No. 16H02209)

1. Sample Mount and Installation
<ol>
	<li>Cut single-crystal samples of Bi2Se313 in an approximate size of 1 &#215; 1 &#215; 0.5 mm3 and use sliver-based epoxy to glue the sample to the sample holder.</li>
	<li>Paste the scotch tape on the sample surface. 
	NOTE: The scotch tape is used to cleave the sample in ultrahigh vacuum (UHV) chamber to obtain an atomically clean surface.</li>
	<li>Install the sample into the sample magazine in the load lock, and sta...

<ol>
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Instrum. 81 (5), 053904 (2010).</li><li>Okuda, T., 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=Efficient+spin+resolved+spectroscopy+observation+machine+at+Hiroshima+Synchrotron+Radiation+Center.">Efficient spin resolved spectroscopy observation machine at Hiroshima Synchrotron Radiation Center.</a> Rev. Sci. Instrum. 82 (10), 103302 (2011).</li><li>Yaji, K., 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-resolution+three-dimensional+spin-+and+angle-resolved+photoelectron+spectrometer+using+vacuum+ultraviolet+laser+light.">High-resolution three-dimensional spin- and angle-resolved photoelectron spectrometer using vacuum ultraviolet laser light.</a> Rev. Sci. Instrum. 87 (5), 053111 (2016).</li><li>Shimojima, T., Okazaki, K., Shin, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Low-temperature+and+high-energy-resolution+laser+photoemission+spectroscopy.">Low-temperature and high-energy-resolution laser photoemission spectroscopy.</a> J. Phys. Soc. Jpn. 84 (7), 072001 (2015).</li><li>Augustine, S., Mathai, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Growth,+morphology,+and+microindentation+analysis+of+Bi2Se3,+Bi1.8In0.2Se3,+and+Bi2Se2.8Te0.2+single+crystals.">Growth, morphology, and microindentation analysis of Bi2Se3, Bi1.8In0.2Se3, and Bi2Se2.8Te0.2 single crystals.</a> Mater. Res. Bull. 36 (13), 2251-2261 (2001).</li><li>Hasan, M. Z., Kane, C. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Colloquium:+Topological+insulators.">Colloquium: Topological insulators.</a> Rev. Mod. Phys. 82 (4), 3045-3067 (2010).</li><li>Ando, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Topological+insulator+materials.">Topological insulator materials.</a> J. Phys. Soc. Jpn. 82 (10), 102011 (2013).</li><li>Zhang, H., Liu, C. -. X., Qi, X. -. L., Dai, X., Fang, Z., Zhang, S. -. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Topological+insulators+in+Bi2Se3,+Bi2Te3+and+Sb2Te3+with+a+single+Dirac+cone+on+the+surface.">Topological insulators in Bi2Se3, Bi2Te3 and Sb2Te3 with a single Dirac cone on the surface.</a> Nature Phys. 5 (6), 438-442 (2009).</li><li>Cao, Y., 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=Mapping+the+orbital+wavefunction+of+the+surface+states+in+three-dimensional+topological+insulators.">Mapping the orbital wavefunction of the surface states in three-dimensional topological insulators.</a> Nature Phys. 9 (8), 499-504 (2013).</li><li>Zhang, H., Liu, C. -. X., Zhang, S. -. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Spin-orbital+texture+in+topological+insulators.">Spin-orbital texture in topological insulators.</a> Phys. Rev. Lett. 111 (6), 066801 (2013).</li><li>Kuroda, K., 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=Coherent+control+over+three-dimensional+spin-polarization+for+the+spin-orbit+coupled+surface+state+of+Bi2Se3.">Coherent control over three-dimensional spin-polarization for the spin-orbit coupled surface state of Bi2Se3.</a> Phys. Rev. B. 94 (16), 165162 (2016).</li><li>Meier, F., 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=Interference+of+spin+states+in+photoemission+from+Sb/Ag(111)+surface+alloys.">Interference of spin states in photoemission from Sb/Ag(111) surface alloys.</a> J Phys-Condens Mat. 23 (7), 072207 (2011).</li><li>Dil, J. H., Meier, F., Osterwalder, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Rashba-type+spin+splitting+and+spin+interference+of+the+Cu(111)+surface+state+at+room+temperature.">Rashba-type spin splitting and spin interference of the Cu(111) surface state at room temperature.</a> J Electron Spectrosc. 201, 42-46 (2015).</li><li>Yaji, K., 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=Spin-dependent+quantum+interference+in+photoemission+process+from+spin-orbit+coupled+states.">Spin-dependent quantum interference in photoemission process from spin-orbit coupled states.</a> Nature Commun. 8, 14588 (2017).</li><li>Noguchi, R., 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=Direct+mapping+of+spin+and+orbital+entangled+wave+functions+under+interband+spin-orbit+coupling+of+giant+Rashba+spin-split+surface+states.">Direct mapping of spin and orbital entangled wave functions under interband spin-orbit coupling of giant Rashba spin-split surface states.</a> Phys. Rev. B. 95 (6), 04111(R) (2017).</li></ol>

ARPES and SARPES techniques have been commonly used for studying electronic band structures through the band mapping and spin-detection1,2. In addition to these general advantages shown above, laser-SARPES based on orbital selection rule in optical dipole excitation can be employed as a novel technique for visualizing the spin-orbital coupling effect in the wavefunction and quantum spin interference. As demonstrated in Figure 9<stron...

Angle-resolved photoemission spectroscopy (ARPES) technique has developed into one of the most powerful tool to investigate quasiparticle band structures in solid states1. The most of attractive feature of ARPES is the capability for band mapping to characterize electronic states in energy and momentum space. Spin-resolved ARPES (SARPES), which is here equipped with spin-detectors, e.g. Mott detector2,3, further enables us to resolve the spin character of the observed band structures4. Since the Mott detector can measure the spin with two axes (x and z, or y and z), the combination of the two Mott detectors further allows one to obtain the spin orientation in three dimension4,5. For several decades, however, the SARPES experiments were suffered from their low efficiency (typically 1/10000 compared to that for spin-integrated ARPES measurement)3,4,5,6,7, which had limited the energy and angular-resolutions. Recently, the energy resolution of SARPES has been increased with a high-efficient spin detector based on exchange scattering, the so-called very-low-energy electron-diffraction (VLEED) detector7,8,9,10. With this detector, the data quality has been significantly improved and the data acquisition time has been shortened. Recently, SARPES has succeeded greatly to address spin-polarized electronic states and particularly spin-orbit coupling effect resulting in the spin texture of the surface bands7.
Here, we employ SARPES measurements with a polarization-variable vacuum ultraviolet laser light (laser-SARPES) and demonstrate the great advantages of this combined technique. Through the investigation on the spin-orbit coupled surface states in Bi2Se3, we present two capabilities of laser-SARPES. Firstly, due to the orbital selection rule of linearly polarized lasers in dipole transition regime, p- and s-polarized lights selectively excite a part of eigen-wavefunctions with different orbital symmetry. Such an orbital selective excitation is thereby available in SARPES, namely, orbital-selective SARPES. Secondly, three-dimensional (3D) spin-detection in SARPES shows the direction of the spin quantum axis and directly displays full information of the light-polarization dependence. In this protocol, we briefly describe a methodology to perform this state-of-the-art laser-SARPES technique to study the strong spin-orbit coupling effects.
Our laser-SARPES system is located at The Institute for Solid State Physics, The University of Tokyo11. The schematic drawing of our laser-SAPRES machine is shown in Figure 1. The polarization-variable 7-eV laser light12 illuminates the sample surface and the photoelectrons are emitted from the sample. The polarization of laser is automatically controlled by MgF2-based &#955;/2- and &#955;/4-waveplates to selectively use linear and circular polarizations. A hemispherical electron analyzer corrects the photoelectrons, and analyzes their kinetic energy (Ekin) and emission angle (&#952;x and &#952;y). The photoelectron intensities are mapped on the Ekin-&#952;x screen monitored by a CCD camera. This image is directly transformed into the energy band structure in reciprocal space.
For SARPES measurement, the photoelectrons with a specific emission angle and kinetic energy analyzed by the electron analyzer are&#160;guided to two VLEED-type spin detectors with a 90-degree photoelectron deflector and the photoelectron beams are focused onto two different targets of Fe(001)-p(1&#215;1) films terminated by oxygen. The photoelectrons reflected by the targets are detected in single channel detection by using a channeltron placed in each spin detector. The VLEED targets can be magnetized with Helmholtz-type electric coils which are arranged with orthogonal geometry with respect to each other. The magnetization direction is controlled by the bipolar condenser bank. The double VLEED spin detectors thereby enable us to analyze the spin-polarization vector of the photoelectron in three dimensions.

<table>
	<tbody>
		<tr>
			<td>DA30-L hemispherical analyzer</td>
			<td>ScientaOmicron</td>
			<td></td>
			<td>http://www.scientaomicron.com/en/products/353/1170</td>
		</tr>
		<tr>
			<td>Silver-based epoxy</td>
			<td>Epoxy Technology</td>
			<td>H20E</td>
			<td></td>
		</tr>
		<tr>
			<td>Sctoch tape</td>
			<td>3M</td>
			<td>801-1-18C</td>
			<td></td>
		</tr>
		<tr>
			<td>UHV valve</td>
			<td>VAT</td>
			<td>01034-KE01</td>
			<td></td>
		</tr>
		<tr>
			<td>linear/rotary feedthrough</td>
			<td>Ferrovac</td>
			<td>MD40</td>
			<td></td>
		</tr>
		<tr>
			<td>transfer rod</td>
			<td>UHV design</td>
			<td>PP series</td>
			<td></td>
		</tr>
		<tr>
			<td>wobble stick</td>
			<td>Ferrovac</td>
			<td>WM40</td>
			<td></td>
		</tr>
		<tr>
			<td>Paladin compact 355</td>
			<td>Coherent</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>half waveplate</td>
			<td>Kogakugiken</td>
			<td></td>
			<td>order made</td>
		</tr>
		<tr>
			<td>Bipolar condenser bank</td>
			<td>Tsuji electronics</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

experimental methods for spin- and angle-resolved photoemission spectroscopy combined with polarization-variable laser

The goal of this protocol is to present how to perform spin- and angle-resolved photoemission spectroscopy combined with polarization-variable 7-eV laser (laser-SARPES), and demonstrate a power of this technique for studying solid state physics. Laser-SARPES achieves two great capabilities. Firstly, by examining orbital selection rule of linearly polarized lasers, orbital selective excitation can be carried out in SAPRES experiment. Secondly, the technique can show full information of a variation of the spin quantum axis as a function of the light polarization. To demonstrate the power of the collaboration of these capabilities in laser-SARPES, we apply this technique for the investigations of spin-orbit coupled surface states of Bi2Se3. This technique affords to decompose spin and orbital components from the spin-orbit coupled wavefunctions. Moreover, as a representative advantage of using the direct spin detection collaborated with the polarization-variable laser, the technique unambiguously visualizes the light polarization dependence of the spin quantum axis in three-dimension. Laser-SARPES dramatically increases a capability of photoemission technique.

Before starting SARPES experiments, k positions need to be accurately determined for taking spin-resolved spectrum by using high statistic spin-integrated ARPES results with high energy- and angular-resolutions (protocol 5.1-5.5). This is demonstrated in Figure 7 where the ARPES results for a Bi2Se3 single crystal are presented. This material is known as a prototypical topological insulator with a spin-polarized surface states<s...

Watch this Scientific Journal Video about Experimental Methods for Spin- and Angle-Resolved Photoemission Spectroscopy Combined with Polarization-Variable Laser at JoVE.com

Experimental Methods for Spin- and Angle-Resolved Photoemission Spectroscopy Combined with Polarization-Variable Laser

Here, we combine polarization-variable 7-eV laser with spin- and angle-resolved photoemission technique to visualize the spin-orbital coupling effect in solid states.

The goal of this protocol is to present how to perform spin- and angle-resolved photoemission spectroscopy combined with polarization-variable 7-eV laser ...

Spin and angle-resolved photoemission spectroscopy, the so called SARPES, is a powerful technique to investigate solid state electron structures including their spin information. In our method, we combined this technique with the polarization-variable 7-eV laser which enabled us to determine the electron spin structures, very precisely. SARPES was generally performed with synchrotron radiation or noble-gas-discharge lamp.Compared to this method, using a polarization-variable 7-eV laser is a large improvement. The polarization with the laser beam can be easily controlled using the waveplate. By using this property, we can completely trace the behavior of electron spin, which is sensitive to the light polarization.The photoelectron spin reaction depends on the light polarization. And that shows many physical meanings such as, spin-orbit coupling and spin-interference. For this reason, our technique can be gradually used for studying condensed matter physics.To begin, cut single crystal samples of bismuth selenide, and use a silver-based epoxy to glue them to a sample holder. Once the epoxy has cured, place a piece of scotch tape onto the surface of the samples. Then, transfer the sample magazine into the ultrahigh vacuum load lock and start the pump until the pressure of the load lock is lower than one times ten to the negative five pascal.Next, open the ultrahigh vacuum valve between the load lock and the preparation chamber, and move the sample magazine from the load lock to the preparation chamber, using the feedthrough mechanism attached to the load lock chamber. Now, use a transfer rod to pick up the sample from the sample magazine and then place the sample magazine back into the load lock and close the ultrahigh vacuum valve. Wait until the pressure of the preparation chamber is below five times ten to the negative seven pascal, and then peel the scotch tape from the surface of the bismuth selenide using the wobble stick in the preparation chamber.This will cleave the sample, producing an atomically clean surface. Transfer the sample to the UHV measurement chamber. There, use a screwdriver to fix the sample to the main gonio stage.Then, move the stage to the measurement position and use a micrometer stage to precisely position the sample onto the focus of the spectrometer. Next, turn on the neodymium-doped yttrium orthovanadate laser, and allow it to warm up for ten to 15 minutes. Open the laser beam shutter and make sure that the laser passes through a potassium beryllium fluoroborate crystal to generate a second harmonic wave of 177 nanometers.Optimize the power of the seven electron volt laser, by changing the power of the 355 nanometer laser using a variable attenuator. First, open the analyzer control software. In the sequence menu, select setup and then choose ARPES configuration, and ARPES mapping, in the list, to perform Fermi surface mapping with the photoelectron deflector.Click on edit, and configure the Fermi surface mapping so that the emission angle ranges from 12 degrees to 12 degrees with the step size of 0.5 degrees and 49 for the number of steps. Once set, go back into the sequence menu and select run. The hemispherical analyzer has a electron deflector which enable us to map the Fermi surface without rotating the sample.Manually change the machine setup for spin and angle-resolved photoemission spectroscopy measurement. This includes changing both the analyzer entrance slit and the aperture size. In the software, select setup and choose spin configuration, and normal from the list of options and click okay.Next, select DA30 on the menu bar and navigate to control theta. This will open the setting panel for the DA30 angle configuration. In the panel, choose the emission angle for theta x to be negative six degrees, and for theta y to be zero degrees.Then, use a command prompt to apply the magnetic field by controlling the bipolar condenser bank. This will magnetize the v-lead's target in the position direction along the x, y, or z-axis. Once set, click on run, to take the intensity spectrum.Next, apply a magnetic field to magnetize the v-lead target in the negative direction along the axis and run the scan to take another intensity spectrum. When finished, calculate the spin-polarization and the spin-resolved spectra. Using the command prompt, power the step motor to precisely change the angle of the half waveplate in order to tune the light polarization of the seven electron volt laser.Then, take the spin-resolved spectra for each of the x, y and z-axes. Scan the spin-resolved spectra as a function of the light polarization, while varying the half waveplate angle from zero degrees to 102 degrees with the step size of three degrees. Bismuth selenide, is a prototypical topological insulator with spin-polarized surface states.The obtained Fermi surface map of the surface state in bismuth selenide, shows an almost circled shape. Then, perform band mapping along the high symmetry line. It shows the X-shaped energy dispersion, the so called Dirac cone.From these results, one can now choose the specific emission angle for the SARPES experiment. When taking a theta x equals negative six degrees and theta y equals zero degrees across negative kF of the surface band, the energy distribution curves for different magnetization directions, peak in intensity near the Fermi energy. The intensities in the two spectra are different near the peak.From the difference between their intensities, one can calculate the spin-polarization as a function of the energy and the spin-resolved spectra. Apparently, the up spin spectrum has a peak structure but the down spin spectra is relatively flat. This reflects the almost 100%spin-polarization.When taking the same measurement for a different axis and with different light polarization, the spin direction of the electrons and its polarization dependence are clearly visible. For p-polarization, the data clearly shows the positively 100%spin-polarization only along y and there is no spin-polarization along the x and z directions. Interestingly, when one switches the light polarization from p to s, the sign of spin-polarization also switches to the negatively 100%for s-polarization without x and z spin component.As a consequence of full spin information, the electron's spin rotation is completely unraveled in three dimension. We have demonstrated the power of the SARPES, with the polarization-variable laser, for starting spin-polarized state of bismuth selenide. This allows us to directly visualize electron spin and its variations, as a function of light polarizations.This technique can be easily applied for many other physical systems. Our experiment show that, even small changes in the light fields really can remodify the photoelectron spin in three dimension. How the sample is illuminated is very important.One must take care of the experimental geometry to correctly understand the data.

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Engineering

Angle-resolved Photoemission Spectroscopy At Ultra-low Temperatures

The physical properties of a material are defined by its electronic structure. Electrons in solids are characterized by energy (&omega;) and momentum (k) and the probability to find them in a particular state with given &omega; and k is described by the spectral function A(k, &omega;). This function can be directly measured in an experiment based on the well-known photoelectric effect, for the explanation of which Albert Einstein received the Nobel Prize back in 1921. In the photoelectric effect the light shone on a surface ejects electrons from the material. According to Einstein, energy conservation allows one to determine the energy of an electron inside the sample, provided the energy of the light photon and kinetic energy of the outgoing photoelectron are known. Momentum conservation makes it also possible to estimate k relating it to the momentum of the photoelectron by measuring the angle at which the photoelectron left the surface. The modern version of this technique is called Angle-Resolved Photoemission Spectroscopy (ARPES) and exploits both conservation laws in order to determine the electronic structure, i.e. energy and momentum of electrons inside the solid. In order to resolve the details crucial for understanding the topical problems of condensed matter physics, three quantities need to be minimized: uncertainty* in photon energy, uncertainty in kinetic energy of photoelectrons and temperature of the sample.
In our approach we combine three recent achievements in the field of synchrotron radiation, surface science and cryogenics. We use synchrotron radiation with tunable photon energy contributing an uncertainty of the order of 1 meV, an electron energy analyzer which detects the kinetic energies with a precision of the order of 1 meV and a He3 cryostat which allows us to keep the temperature of the sample below 1 K. We discuss the exemplary results obtained on single crystals of Sr2RuO4 and some other materials. The electronic structure of this material can be determined with an unprecedented clarity.

The overall goal of this method is to determine the low-energy electronic structure of solids at ultra-low temperatures using Angle-Resolved Photoemission Spectroscopy with synchrotron radiation.

The physical properties of a material are defined by its  electronic structure. Electrons in solids are characterized by energy (&omega;)  and momentum ...

Spatial Separation of Molecular Conformers and Clusters

Gas-phase molecular physics and physical chemistry experiments commonly use supersonic expansions through pulsed valves for the production of cold molecular beams. However, these beams often contain multiple conformers and clusters, even at low rotational temperatures. We present an experimental methodology that allows the spatial separation of these constituent parts of a molecular beam expansion. Using an electric deflector the beam is separated by its mass-to-dipole moment ratio, analogous to a bender or an electric sector mass spectrometer spatially dispersing charged molecules on the basis of their mass-to-charge ratio. This deflector exploits the Stark effect in an inhomogeneous electric field and allows the separation of individual species of polar neutral molecules and clusters. It furthermore allows the selection of the coldest part of a molecular beam, as low-energy rotational quantum states generally experience the largest deflection. Different structural isomers (conformers) of a species can be separated due to the different arrangement of functional groups, which leads to distinct dipole moments. These are exploited by the electrostatic deflector for the production of a conformationally pure sample from a molecular beam. Similarly, specific cluster stoichiometries can be selected, as the mass and dipole moment of a given cluster depends on the degree of solvation around the parent molecule. This allows experiments on specific cluster sizes and structures, enabling the systematic study of solvation of neutral molecules.

We present a technique that allows the spatial separation of different conformers or clusters present in a molecular beam. An electrostatic deflector is used to separate species by their mass-to-dipole moment ratio, leading to the production of gas-phase ensembles of a single conformer or cluster stoichiometry.

Gas-phase molecular physics and physical chemistry experiments commonly use supersonic expansions through pulsed valves for the production of cold ...

Laser-induced Breakdown Spectroscopy: A New Approach for Nanoparticle's Mapping and Quantification in Organ Tissue

Emission spectroscopy of laser-induced plasma was applied to elemental analysis of biological samples. Laser-induced breakdown spectroscopy (LIBS) performed on thin sections of rodent tissues: kidneys and tumor, allows the detection of inorganic elements such as (i) Na, Ca, Cu, Mg, P, and Fe, naturally present in the body and (ii) Si and Gd, detected after the injection of gadolinium-based nanoparticles. The animals were euthanized 1&#160;to 24 hr&#160;after intravenous injection of particles. A two-dimensional scan of the sample, performed using a motorized micrometric 3D-stage, allowed the infrared laser beam exploring the surface with a lateral resolution less than 100 &#956;m. Quantitative chemical images of Gd element inside the organ were obtained with sub-mM sensitivity. LIBS offers a simple and robust method to study the distribution of inorganic materials without any specific labeling. Moreover, the compatibility of the setup with standard optical microscopy emphasizes its potential to provide multiple images of the same biological tissue with different types of response:&#160;elemental, molecular, or cellular.

Laser-induced breakdown spectroscopy performed on thin organ and tumor tissue successfully detected natural elements and artificially injected gadolinium (Gd), issued from Gd-based nanoparticles. Images of chemical elements reached a resolution of 100 &#956;m and quantitative sub-mM sensitivity. The compatibility of the setup with standard optical microscopy emphasizes its potential to provide multiple images of a same biological tissue.

Emission spectroscopy of laser-induced plasma was applied to elemental analysis of biological samples. Laser-induced breakdown spectroscopy (LIBS) ...

Proton Transfer and Protein Conformation Dynamics in Photosensitive Proteins by Time-resolved Step-scan Fourier-transform Infrared Spectroscopy

Monitoring the dynamics of protonation and protein backbone conformation changes during the function of a protein is an essential step towards understanding its mechanism. Protonation and conformational changes affect the vibration pattern of amino acid side chains and of the peptide bond, respectively, both of which can be probed by infrared (IR) difference spectroscopy. For proteins whose function can be repetitively and reproducibly triggered by light, it is possible to obtain infrared difference spectra with (sub)microsecond resolution over a broad spectral range using the step-scan Fourier transform infrared technique. With ~102-103 repetitions of the photoreaction, the minimum number to complete a scan at reasonable spectral resolution and bandwidth, the noise level in the absorption difference spectra can be as low as ~10-4, sufficient to follow the kinetics of protonation changes from a single amino acid. Lower noise levels can be accomplished by more data averaging and/or mathematical processing. The amount of protein required for optimal results is between 5-100 &#181;g, depending on the sampling technique used. Regarding additional requirements, the protein needs to be first concentrated in a low ionic strength buffer and then dried to form a film. The protein film is hydrated prior to the experiment, either with little droplets of water or under controlled atmospheric humidity. The attained hydration level (g of water / g of protein) is gauged from an IR absorption spectrum. To showcase the technique, we studied the photocycle of the light-driven proton-pump bacteriorhodopsin in its native purple membrane environment, and of the light-gated ion channel channelrhodopsin-2 solubilized in detergent.

Key steps of protein function, in particular backbone conformational changes and proton transfer reactions, often take place in the microsecond to millisecond time scale. These dynamical processes can be studied by time-resolved step-scan Fourier-transform infrared spectroscopy, in particular for proteins whose function is triggered by light.

Monitoring the dynamics of protonation and protein backbone conformation changes during the function of a protein is an essential step towards ...

Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film synthesis) for the purpose of exploratory materials research. Certain materials pose a challenge wherein the traditional bulk Hall bar device fabrication method is insufficient to produce a measureable device for sample transport measurement, principally because the single crystal size is too small to attach wire leads to the sample in a Hall bar configuration. This can be, for example, because the first batch of a new material synthesized yields very small single crystals or because flakes of samples of one to very few monolayers are desired. In order to enable rapid characterization of materials that may be carried out in parallel with improvements to their growth methodology, a method of device fabrication for very small samples has been devised to permit the characterization of novel materials as soon as a preliminary batch has been produced. A slight variation of this methodology is applicable to producing devices using exfoliated samples of two-dimensional materials such as graphene, hexagonal boron nitride (hBN), and transition metal dichalcogenides (TMDs), as well as multilayer heterostructures of such materials. Here we present detailed protocols for the experimental device fabrication of fragments and flakes of novel materials with micron-sized dimensions onto substrate and subsequent measurement in a commercial superconducting magnet, dry helium close-cycle cryostat magnetotransport system at temperatures down to 0.300 K and magnetic fields up to 12 T.

We describe the methodology of mechanical exfoliation and deposition of flakes of novel materials with micron-sized dimensions onto substrate, fabrication of experimental device structures for transport experimentation, and the magnetotransport measurement in a dry helium close-cycle cryostat at temperatures down to 0.300 K and magnetic fields up to 12 T.

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film ...

SSVEP-based Experimental Procedure for Brain-Robot Interaction with Humanoid Robots

Brain-Robot Interaction (BRI), which provides an innovative communication pathway between human and a robotic device via brain signals, is prospective in helping the disabled in their daily lives. The overall goal of our method is to establish an SSVEP-based experimental procedure by integrating multiple software programs, such as OpenViBE, Choregraph, and Central software as well as user developed programs written in C++ and MATLAB, to enable the study of brain-robot interaction with humanoid robots.
This is achieved by first placing EEG electrodes on a human subject to measure the brain responses through an EEG data acquisition system. A user interface is used to elicit SSVEP responses and to display video feedback in the closed-loop control experiments. The second step is to record the EEG signals of first-time subjects, to analyze their SSVEP features offline, and to train the classifier for each subject. Next, the Online Signal Processor and the Robot Controller are configured for the online control of a humanoid robot. As the final step, the subject completes three specific closed-loop control experiments within different environments to evaluate the brain-robot interaction performance.
The advantage of this approach is its reliability and flexibility because it is developed by integrating multiple software programs. The results show that using this approach, the subject is capable of interacting with the humanoid robot via brain signals. This allows the mind-controlled humanoid robot to perform typical tasks that are popular in robotic research and are helpful in assisting the disabled.

The overall goal of this method is to establish an SSVEP-based experimental procedure by integrating multiple software programs to enable the study of brain-robot interaction with humanoid robots, which is prospective in assisting the sick and elderly as well as performing unsanitary or dangerous jobs.

Brain-Robot Interaction (BRI), which provides an innovative communication pathway between human and a robotic device via brain signals, is prospective in ...

Experimental Methods for Investigation of Shape Memory Based Elastocaloric Cooling Processes and Model Validation

Shape Memory Alloys (SMA) using elastocaloric cooling processes have the potential to be an environmentally friendly alternative to the conventional vapor compression based cooling process. Nickel-Titanium (Ni-Ti) based alloy systems, especially, show large elastocaloric effects. Furthermore, exhibit large latent heats which is a necessary material property for the development of an efficient solid-state based cooling process. A scientific test rig has been designed to investigate these processes and the elastocaloric effects in SMAs. The realized test rig enables independent control of an SMA&#39;s mechanical loading and unloading cycles, as well as conductive heat transfer between SMA cooling elements and a heat source/sink. The test rig is equipped with a comprehensive monitoring system capable of synchronized measurements of mechanical and thermal parameters. In addition to determining the process-dependent mechanical work, the system also enables measurement of thermal caloric aspects of the elastocaloric cooling effect through use of a high-performance infrared camera. This combination is of particular interest, because it allows illustrations of localization and rate effects &#8212; both important for efficient heat transfer from the medium to be cooled.
The work presented describes an experimental method to identify elastocaloric material properties in different materials and sample geometries. Furthermore, the test rig is used to investigate different cooling process variations. The introduced analysis methods enable a differentiated consideration of material, process and related boundary condition influences on the process efficiency. The comparison of the experimental data with the simulation results (of a thermomechanically coupled finite element model) allows for better understanding of the underlying physics of the elastocaloric effect. In addition, the experimental results, as well as the findings based on the simulation results, are used to improve the material properties.

Experimental methods for investigation of solid state cooling processes and characterization of elastocaloric material properties of Shape Memory Alloys (SMA) are presented. A custom-built test rig has been designed for controlling and comprehensive monitoring of elastocaloric cooling processes. Furthermore, it provides a validation platform for thermomechanically coupled modeling approaches.

Shape Memory Alloys (SMA) using elastocaloric cooling processes have the potential to be an environmentally friendly alternative to the conventional vapor ...

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 ...

Free-form Light Actuators &#8212; Fabrication and Control of Actuation in Microscopic Scale

Liquid crystalline elastomers (LCEs) are smart materials capable of reversible shape-change in response to external stimuli, and have attracted researchers&#39; attention in many fields. Most of the studies focused on macroscopic LCE structures (films, fibers) and their miniaturization is still in its infancy. Recently developed lithography techniques, e.g., mask exposure and replica molding, only allow for creating 2D structures on LCE thin films. Direct laser writing (DLW) opens access to truly 3D fabrication in the microscopic scale. However, controlling the actuation topology and dynamics at the same length scale remains a challenge.
In this paper we report on a method to control the liquid crystal (LC) molecular alignment in the LCE microstructures of arbitrary three-dimensional shape. This was made possible by a combination of direct laser writing for both the LCE structures as well as for micrograting patterns inducing local LC alignment. Several types of grating patterns were used to introduce different LC alignments, which can be subsequently patterned into the LCE structures. This protocol allows one to obtain LCE microstructures with engineered alignments able to perform multiple opto-mechanical actuation, thus being capable of multiple functionalities. Applications can be foreseen in the fields of tunable photonics, micro-robotics, lab-on-chip technology and others.

Here, we fabricate 3D polymeric micro/nano structures in which both the shape and the molecular alignment can be engineered with nanometer scale accuracy by the use of direct laser writing. Light induced deformation of several types of liquid crystalline elastomer microstructures can be controlled in the microscopic scale.

Liquid crystalline elastomers (LCEs) are smart materials capable of reversible shape-change in response to external stimuli, and have attracted ...

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.

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 ...