Name: measuring magnetically-tuned ferroelectric polarization in liquid crystals
Uploaded: 2018-08-15T14:45:00
Description: Watch this Scientific Journal Video about Measuring Magnetically-Tuned Ferroelectric Polarization in Liquid Crystals at JoVE.com

We thank Prof. Takanishi for his help in our experiment. We also thank DIC Corporation for providing the compounds studied here. This work was supported by Grant-in-Aid for the JSPS Fellow (16J02711), JSPS KAKENHI Grant Number 17H01143, and the Program for Leading Graduate Schools &#34;Interactive Materials Cadet Program&#34;.

1. Preparation of Liquid-Crystal Cells and the Determination of the Cell Gap
<ol>
	<li>Preparation of liquid-crystal cells 
	<ol>
		<li>Cut glass substrates coated with indium/tin-oxide (ITO) on one side into the desired size (typical size: 10 x 10 x 1.1 mm, Figure 2A). To cut the substrates, scratch a line on their face with a glass cutter and break off excess glass manually.</li>
		<li>Wash the cut glass substrates using a detergent in an ultrasonic bath at 35 kHz for 30...

<ol>
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W., Mostovoy, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multiferroics:+A+magnetic+twist+for+ferroelectricity.">Multiferroics: A magnetic twist for ferroelectricity.</a> Nature Materials. 6, 13-20 (2007).</li><li>Tokura, Y., Seki, S., Nagaosa, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multiferroics+of+spin+origin.">Multiferroics of spin origin.</a> Reports on Progress in Physics. 77, 076501 (2014).</li><li>Fiebig, M., Lottermoser, T., Meier, D., Trassin, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+evolution+of+multiferroics.">The evolution of multiferroics.</a> Nature Reviews Materials. 1, 16046 (2016).</li><li>Kagawa, F., Horiuchi, S., Tokunaga, M., Fujioka, M., Tokura, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ferroelectricity+in+a+one-dimensional+organic+quantum+magnet.">Ferroelectricity in a one-dimensional organic quantum magnet.</a> Nature Physics. 6, 169-172 (2010).</li><li>Stroppa, A., 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=Electric+Control+of+magnetization+and+interplay+between+orbital+ordering+and+ferroelectricity+in+a+multiferroic+metal-organic+framework.">Electric Control of magnetization and interplay between orbital ordering and ferroelectricity in a multiferroic metal-organic framework.</a> Angewandte Chemie International Edition. 50, 5847-5850 (2011).</li><li>Wang, W., 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=Magnetoelectric+coupling+in+the+paramagnetic+state+of+a+metal-organic+framework.">Magnetoelectric coupling in the paramagnetic state of a metal-organic framework.</a> Science Reports. 3, 2024 (2011).</li><li>G&#243;mez-Aguirre, L. 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F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Room-temperature+multiferroic+magnetoelectrics.">Room-temperature multiferroic magnetoelectrics.</a> NPG Asia Materials. 5, e72 (2013).</li><li>Suzuki, 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=Influence+of+applied+electric+fields+on+the+positive+magneto-LC+effects+observed+in+the+ferroelectric+liquid+crystalline+phase+of+a+chiral+nitroxide+radical+compound.">Influence of applied electric fields on the positive magneto-LC effects observed in the ferroelectric liquid crystalline phase of a chiral nitroxide radical compound.</a> Soft Matter. 9, 4687-4692 (2013).</li><li>Domracheva, N. E., Ovchinnikov, I. V., Turanov, A. N., Konstantinov, V. N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=EPR+detection+of+presumable+magnetoelectric+interactions+in+the+liquid-crystalline+state+of+an+iron+mesogen.">EPR detection of presumable magnetoelectric interactions in the liquid-crystalline state of an iron mesogen.</a> Journal of Magnetism and Magnetic Materials. 269, 385-392 (2004).</li><li>Toma&#353;ovi&#269;ov&#225;, N., 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=Capacitance+changes+in+ferronematic+liquid+crystals+induced+by+low+magnetic+fields.">Capacitance changes in ferronematic liquid crystals induced by low magnetic fields.</a> Phys. Rev. E. 87, 014501 (2013).</li><li>Lin, T. -. J., Chen, C. -. C., Lee, W., Cheng, S., Chen, Y. -. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrical+manipulation+of+magnetic+anisotropy+in+the+composite+of+liquid+crystals+and+ferromagnetic+nanorods.">Electrical manipulation of magnetic anisotropy in the composite of liquid crystals and ferromagnetic nanorods.</a> Applied Physics Letters. 93, 013108 (2008).</li><li>Mertelj, A., Osterman, N., Lisjak, D., &#268;opi&#269;, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Magneto-optic+and+converse+magnetoelectric+effects+in+a+ferromagnetic+liquid+crystal.">Magneto-optic and converse magnetoelectric effects in a ferromagnetic liquid crystal.</a> Soft Matter. 10, 9065-9072 (2014).</li><li>Ueda, H., Akita, T., Uchida, Y., Kimura, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Room-temperature+magnetoelectric+effect+in+a+chiral+smectic+liquid+crystal.">Room-temperature magnetoelectric effect in a chiral smectic liquid crystal.</a> Applied Physics Letters. 111, 262901 (2017).</li><li>Clark, N. A., Lagerwall, S. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Submicrosecond+bistable+electro-optic+switching+in+liquid+crystals.">Submicrosecond bistable electro-optic switching in liquid crystals.</a> Applied Physics Letters. 36, 899-901 (1980).</li><li>Vantomme, G., Gelebart, A. H., Broer, D. J., Meijer, E. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+of+liquid+crystal+networks+for+macroscopic+oscillatory+motion+induced+by+light.">Preparation of liquid crystal networks for macroscopic oscillatory motion induced by light.</a> Journal of Visualized Experiments. (127), e56266 (2017).</li><li>Yang, K. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Measurements+of+empty+cell+gap+for+liquid-crystal+displays+using+interferometric+methods.">Measurements of empty cell gap for liquid-crystal displays using interferometric methods.</a> Journal of Applied Physics. 64 (9), 4780-4781 (1988).</li><li>Born, M., Wolf, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Principles of Optics. , (1987).</li><li>Dierking, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Textures of Liquid Crystals. , (2003).</li><li>Filipi&#269;, C., 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=Dielectric+properties+near+the+smectic-C*+-smectic-A+phase+transition+of+some+ferroelectric+liquid-crystalline+systems+with+a+very+large+spontaneous+polarization.">Dielectric properties near the smectic-C* -smectic-A phase transition of some ferroelectric liquid-crystalline systems with a very large spontaneous polarization.</a> Physics Review A. 38, 5833-5839 (1988).</li><li>Carlsson, T., &#381;ek&#353;, B., Filipi&#269;, C., Levstik, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Theoretical+model+of+the+frequency+and+temperature+dependence+of+the+complex+dielectric+constant+of+ferroelectric+liquid+crystals+near+the+smectic-C*+-smectic-A+phase+transition.">Theoretical model of the frequency and temperature dependence of the complex dielectric constant of ferroelectric liquid crystals near the smectic-C* -smectic-A phase transition.</a> Physics Review A. 42, 877-889 (1990).</li><li>Michelson, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Physical+realization+of+a+Lifshitz+point+in+liquid+crystals.">Physical realization of a Lifshitz point in liquid crystals.</a> Physical Review Letters. 39, 464 (1977).</li><li>Mu&#353;evi&#269;, I., &#381;ek&#353;, B., Blinc, R., Rasing, T., Wyder, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Phase+diagram+of+a+ferroelectric+chiral+smectic+liquid+crystal+near+the+Lifshitz+point.">Phase diagram of a ferroelectric chiral smectic liquid crystal near the Lifshitz point.</a> Physical Review Letters. 48, 192 (1982).</li><li>Mu&#353;evi&#269;, I., &#381;ek&#353;, B., Blinc, R., Rasing, T., Wyder, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dielectric+study+of+the+modulated+smectic+C*-uniform+smectic+C+transition+in+a+magnetic+field.">Dielectric study of the modulated smectic C*-uniform smectic C transition in a magnetic field.</a> Physica Status Solidi(b). 119, 727-733 (1983).</li><li>Blinc, R., Mu&#353;evi&#269;, I., &#381;ek&#353;, B., Seppen, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ferroelectric+liquid+crystals+in+a+static+magnetic+field.">Ferroelectric liquid crystals in a static magnetic field.</a> Physica Scripta. 35, 38-43 (1991).</li><li>Blinov, L. 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The experimental results showed that the methods described here successfully demonstrated the ME coupling in the liquid crystal. The observed ME and magneto-dielectric effects can be associated with the orientational transition of molecular orientation in a fixed smectic layer structure. However, the layer normal direction n0 in the layer structure can be also changed by applying a magnetic field through magnetic anisotropy. This is because the molecules prefer to have a parallel arra...

Research on the magnetoelectric (ME) effect, the induction of electric polarization (magnetization) by a magnetic (electric) field, has been focused towards the novel types of applications such as sensors and storage technologies. With recent studies on ME multiferroics1,2,3,4, the target systems in the field of ME study are extended to various types of solid-state materials, including inorganic, organic, and metal-organic frameworks, by utilizing spin-lattice couplings dexterously5,6,7,8,9. However, room-temperature operation, which must be accomplished for practical utilization of ME materials with their ME couplings, is still a challenging issue, and a very limited number of single-phase materials have been reported as room-temperature magnetoelectrics to date10.
Liquid crystals, which possess an orientational order, sometimes with a partial positional one, have also been examined with respect to ME materials in recent years11,12,13,14,15. One of the advantages of liquid crystals as ME materials is their operation temperature, as liquid-crystal phases are typically stabilized around room temperature. An example of ME liquid crystals reported so far is a composite between magnetic nano-platelets with perpendicular magnetic anisotropy and liquid crystals showing the nematic phase, known as the simplest liquid-crystal phase possessing only one-dimensional orientational order15. It shows the converse ME effect, the induction of magnetization by an electric field, through the electric-field manipulation of the coupled platelet and molecular orientations.
More recently, another unique strategy to establish the ME effect in liquid crystals was proposed16. The focus of this strategy is to create a chiral smectic C (SmC*) phase with one-dimensional positional order, resulting in a diffused layer structure called the smectic layer. One characteristic of the SmC* phase is that a molecular orientation vector n is coupled with a local electric dipole moment p. This correlation is provided by the combination of tilted orientation of the rod-like constituent molecules with respect to the smectic layer normal n0 and the chirality-induced mirror (and inversion) symmetry breaking in the molecules. From the viewpoint of symmetries, the former changes the symmetry from D&#8734;h (the so-called SmA phase, Figure 1A) into C2h (the so-called SmC phase, Figure 1B), and the latter breaks the mirror symmetry of C2h so that the symmetry is reduced into C2 (the SmC* phase, see each layer in Figure 1C). In each SmC* layer, the presence of finite polarization is allowed along the C2 axis, which is normal to both n0 and n. The strong coupling between n and p is essential for ferroelectricity in liquid crystals. In the SmC* phase, n aligns in the helicoidal manner through layer by layer (Figure 1C), and thus there is no macroscopic polarization. Ferroelectricity in such liquid crystals is achieved by using strong surface effects, which stabilize the homogeneously oriented state of n known as a surface-stabilized ferroelectric liquid-crystal (SSFLC) state (Figure 1D). It should be noted that ferroelectric polarization reversal always accompanies a switching of the bi-stable orientation states through the coupling between n and p17. As the inverse effect, a change in molecular orientation of the SmC* phase is expected to give rise to a change in electric polarization. Through magnetic anisotropy caused by spins on magnetic elements and/or aromatic rings in liquid-crystal molecules and the flexibility of n in a liquid-crystal state due to weaker molecular interactions than in a solid crystal state, n is also tunable by a magnetic field. Thus, the SmC* phase can be transformed into a magnetic-field-induced homogeneously oriented state similar to an SSFLC state. Therefore, the direct ME effect, the induction of electric polarization by a magnetic field, is achieved as the development of macroscopic electric polarization is induced by a homogeneous alignment of n coupled with p, in all the layers.
We introduce procedures to prepare liquid-crystal cells for the investigation of ME couplings and methodologies to detect the ME effect. A method for the preparation of liquid-crystal cells was reported in detail previously18. Here, we modified this method for dielectric and ME measurements. With the method detailed here, we detected magnetically-tuned electric polarization, that is, the direct ME effect, in a liquid crystal showing the SmC* phase at room temperature.

<table>
	<tbody>
		<tr>
			<td>Material</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Compound 1: Figure 4(A)</td>
			<td>DIC Co., Ltd.</td>
			<td>&#8211;N/A</td>
			<td>PYP-8O8</td>
		</tr>
		<tr>
			<td>Compound 2: Figure 4(B)</td>
			<td>DIC Co., Ltd.</td>
			<td>N/A</td>
			<td>PYP-10O10F</td>
		</tr>
		<tr>
			<td>ITO-coated glass substrates</td>
			<td>Sigma-Aldrich Inc.</td>
			<td>703192-10PK</td>
			<td></td>
		</tr>
		<tr>
			<td>Detergent</td>
			<td>Wako Pure Chemical Industries, Ltd.</td>
			<td>031-10401</td>
			<td></td>
		</tr>
		<tr>
			<td>Alignment layer planer</td>
			<td>JSR Co., Ltd.</td>
			<td>AL1254</td>
			<td></td>
		</tr>
		<tr>
			<td>Spacer</td>
			<td>Teijin Film Solutions Co., Ltd.</td>
			<td>Q51-12</td>
			<td></td>
		</tr>
		<tr>
			<td>Glue</td>
			<td>Huntsman Inc.</td>
			<td>ARALDITE RT30</td>
			<td>For gluing two substrates</td>
		</tr>
		<tr>
			<td>Glue</td>
			<td>M&#38;I Materials ltd.</td>
			<td>Apiezon H Grease</td>
			<td>For gluing a cell and homemade insert</td>
		</tr>
		<tr>
			<td>Silver paste</td>
			<td>Fujikura Kasei Co., Ltd.</td>
			<td>D-753</td>
			<td></td>
		</tr>
		<tr>
			<td>Equipment</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Ultrasonic cleaner</td>
			<td>AS ONE Corp.</td>
			<td>AS52GTU</td>
			<td></td>
		</tr>
		<tr>
			<td>Spin coater</td>
			<td>Mikasa Co. Ltd.</td>
			<td>1H-D7</td>
			<td></td>
		</tr>
		<tr>
			<td>Polarized optical microscope</td>
			<td>Nikon Co., Ltd.</td>
			<td>ECLIPSE LV100N POL</td>
			<td></td>
		</tr>
		<tr>
			<td>Short-pass filter</td>
			<td>Thorlabs Inc.</td>
			<td>FB600-40</td>
			<td></td>
		</tr>
		<tr>
			<td>Optical spectrometer</td>
			<td>Ocean Optics Inc.</td>
			<td>USB2000+UV-VIS</td>
			<td></td>
		</tr>
		<tr>
			<td>Differential thermal analyzer</td>
			<td>Rigaku Co., Ltd.</td>
			<td>Thermo plus EVO2</td>
			<td></td>
		</tr>
		<tr>
			<td>Superconducting magnet</td>
			<td>Quantum Design Inc.</td>
			<td>PPMS</td>
			<td></td>
		</tr>
		<tr>
			<td>LCR meter</td>
			<td>Keysight Technologies Ltd.</td>
			<td>E4980A</td>
			<td></td>
		</tr>
		<tr>
			<td>Electrometer</td>
			<td>Keithley Instruments Inc.</td>
			<td>6517A</td>
			<td></td>
		</tr>
	</tbody>
</table>

measuring magnetically-tuned ferroelectric polarization in liquid crystals

Materials showing coupling phenomena between magnetism and (ferro)electricity, i.e., magnetoelectric effects, have attracted a great deal of attention due to their potential applications for future device technologies such as sensors and storage. However, conventional approaches, which usually utilize materials containing magnetic metal ions (or radicals), have a major problem: only a few materials have been found to show the coupling phenomena at room temperature. Recently, we proposed a new approach to achieve room-temperature magnetoelectrics. In contrast to conventional approaches, our alternative proposal focuses on a completely different material, a &#34;liquid crystal&#34;, free from magnetic metal ions. In such liquid crystals, a magnetic field can be utilized to control the orientational state of constituent molecules and the corresponding electric polarization through magnetic anisotropy of the molecules; it is an unprecedented mechanism of the magnetoelectric effect. In this context, this paper provides a protocol to measure ferroelectric properties induced by a magnetic field, that is, the direct magnetoelectric effect, in a liquid crystal. With the method detailed here, we successfully detected magnetically-tuned electric polarization in the chiral smectic C phase of a liquid crystal at room temperature. Taken together with the flexibility of constituent molecules, which directly affects the magnetoelectric responses, the introduced method will serve to allow liquid crystal cells to acquire more functions as room-temperature magnetoelectrics and associated optical materials.

The protocol is deemed a success only if the ME effect in liquid-crystal samples is observed. Here we measured the direct ME effect in a liquid-crystal sample prepared by the aforementioned procedures. For the measurements, an in-plane magnetic field was applied with the angle tilted by about 45&#176; from the rubbing direction (normal to smectic layers), because the largest magnetic-field-induced polarization was detected in this configuration16.
<p class="jov...

Watch this Scientific Journal Video about Measuring Magnetically-Tuned Ferroelectric Polarization in Liquid Crystals at JoVE.com

Measuring Magnetically-Tuned Ferroelectric Polarization in Liquid Crystals

In this report, we present a protocol to examine direct magnetoelectric effects, i.e., induction of ferroelectric polarization by applying magnetic fields, in liquid crystals. This protocol provides a unique approach, supported by the softness of liquid crystals, to achieve room-temperature magnetoelectrics.

Materials showing coupling phenomena between magnetism and (ferro)electricity, i.e., magnetoelectric effects, have attracted a great deal of attention due ...

This method can help answer key questions in the field of condensed matter physics and materials science on the room-temperature operation of the magnet electric effect. The main advantage of this technique is that it tests the magnet electric effect in liquid crystal with high fluidity. Begin with two glass substrates to create each liquid crystal cell.Start with clean substrates with ITO on one side, typically one square centimeter. Make a scratch on the edge of each substrate to help orient them in later steps. At a spin coater, drip polyimide solution onto the ITO-coded side of the substrates before spin coating.When done, bake the substrates at 200 degrees Celsius for one hour. Then take the substrates to an XZ stage that is under a velvet roller that can rotate. Orient a substrate ITO-side up and with its marked edge toward the roller, and fix it on the stage.Start the roller in the translation stage so the substrate moves back and forth under the roller five times. The substrate should experience soft, uniform pressure when in contact with the roller. Then stop the roller in translation stage to retrieve the substrate.When done, place the substrate in isopropyl alcohol for one minute. Then dry the substrates at 80 degrees Celsius for a few minutes. Now work with two rubbed substrates.In addition to the substrates, have flat resin film for a spacer. Place one substrate with its ITO and polyimide side up, and deposit glue at its edges. Next, orient the second substrate over the first with its coded side down.Orient the marked edges to be on opposite sides of the cell. Shift the two slightly before adhering them. Use the regions created by shifting the substrates to glue conducting wires with silver paste to the coded sides of the substrates.Bake the assembly at 150 degrees Celsius for one hour. Now use a setup similar to this to perform measurements of the cell gap. Place the cell so that it is perpendicular to a white light source and in front of an optical spectrometer for measuring the transmission spectrum.The measured transmittance as a function of wavelength allows determination of the cell gap, which is about 12 micrometers for this cell. To proceed, have the liquid crystal mixture in a cell ready. The liquid crystal mixture is comprised of these two pyrimidine compounds.75 milligrams of compound one, along with 25 milligrams of compound two. Put the prepared cell on a hot stage at 80 degrees Celsius. With a spatula, introduce the liquid crystal mixture to the cell, and rely on capillary action.Maintain the cell at 80 degrees Celsius for half an hour before cooling it to room temperature. The next step is to characterize the mixture. At a microscope, place a prepared sample in a hot stage between two crossed polarizers that are in line with the light source.Focus the microscope to observe the textures in the cell. Heat the sample at a rate of 5 degrees Celsius per minute from room temperature up to 80 degrees Celsius, and identify the liquid crystal phases from the polarization micrographs. Use the observations to determine the transition temperatures.The measurements require a superconducting magnet capable of a 9-Tesla field. Prepare an insert for the magnet that has a rod to house coaxial cables. At its head, there should be a connector terminal.At its end, there should be a sample space capable of holding a cell. Glue the cell on the sample space of the insert so the magnetic field is parallel to the substrate surfaces. Solder the cell's wires to the high and low terminals.Also place a thermometer on the widest length of the cell. When ready, introduce the insert into the superconducting magnet. With coaxial cables, connect the terminals of the insert to measurement instruments and gather data.Here is the electric polarization as a function of temperature, found by integrating the displacement current measured with an electrometer. In the smectic C-star phase, a finite polarization develops on applying a magnetic field at about 328 Kelvin. As the system undergoes a phase transition to the smectic A-star phase, the polarization disappears.These data are for the dielectric constant measured at 100 hertz using a quasi four-terminal method with an LCR meter. In the smectic C-star phase, it is suppressed as the magnetic field increases. This can be ascribed to the change in the molecular orientation state, coupled with the electric dipole moment.In the smectic A-star phase, the dielectric constant is independent of the magnetic field. Fixing the temperature allows for a clear demonstration of magnetoelectric activity. At 300 Kelvin, the sample is in the smectic C-star phase.Here the electric polarization varies with the changing magnetic field. The dielectric constant taken at 100 hertz shows similar behavior. Measurements performed at 335 Kelvin when the liquid crystal is in the smectic A-star phase do not depend on the magnetic field.So this method can provide insight into magnetically tunable electric polarization in liquid crystals. It can also be applied to other measurements, such as electrically controllable magnetism, and lighting optical effects in liquid crystals. After each development, this technique paves the way for researchers in the field of condensed matter physics and materials science, magnetoelectric coupling in liquid crystals.

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Engineering

Revealing Dynamic Processes of Materials in Liquids Using Liquid Cell Transmission Electron Microscopy

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted significant interests across the research fields of materials science, physics, chemistry and biology. The key enabling technology is a liquid cell. We fabricate liquid cells with thin viewing windows through a sequential microfabrication process, including silicon nitride membrane deposition, photolithographic patterning, wafer etching, cell bonding, etc. A liquid cell with the dimensions of a regular TEM grid can fit in any standard TEM sample holder. About 100 nanoliters reaction solution is loaded into the reservoirs and about 30 picoliters liquid is drawn into the viewing windows by capillary force. Subsequently, the cell is sealed and loaded into a microscope for in situ imaging. Inside the TEM, the electron beam goes through the thin liquid layer sandwiched between two silicon nitride membranes. Dynamic processes of nanoparticles in liquids, such as nucleation and growth of nanocrystals, diffusion and assembly of nanoparticles, etc., have been imaged in real time with sub-nanometer resolution. We have also applied this method to other research areas, e.g., imaging proteins in water. Liquid cell TEM is poised to play a major role in revealing dynamic processes of materials in their working environments. It may also bring high impact in the study of biological processes in their native environment.

We have developed a self-contained liquid cell, which allows imaging through liquids using a transmission electron microscope. Dynamic processes of nanoparticles in liquids can be revealed in real time with sub-nanometer resolution.

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted ...

Ultrasound Velocity Measurement in a Liquid Metal Electrode

A growing number of electrochemical technologies depend on fluid flow, and often that fluid is opaque. Measuring the flow of an opaque fluid is inherently more difficult than measuring the flow of a transparent fluid, since optical methods are not applicable. Ultrasound can be used to measure the velocity of an opaque fluid, not only at isolated points, but at hundreds or thousands of points arrayed along lines, with good temporal resolution. When applied to a liquid metal electrode, ultrasound velocimetry involves additional challenges: high temperature, chemical activity, and electrical conductivity. Here we describe the experimental apparatus and methods that overcome these challenges and allow the measurement of flow in a liquid metal electrode, as it conducts current, at operating temperature. Temperature is regulated within &#177;2 &#176;C using a Proportional-Integral-Derivative (PID) controller that powers a custom-built furnace. Chemical activity is managed by choosing vessel materials carefully and enclosing the experimental setup in an argon-filled glovebox. Finally, unintended electrical paths are carefully prevented. An automated system logs control settings and experimental measurements, using hardware trigger signals to synchronize devices. This apparatus and these methods can produce measurements that are impossible with other techniques, and allow optimization and control of electrochemical technologies like liquid metal batteries.

Ultrasound velocimetry is used to study mixing by fluid flow in liquid metal electrodes. The focus of this manuscript is to illustrate the methods used for making precise, spatially-resolved ultrasound measurements while limiting oxidation and controlling and monitoring temperature, applied current, and the heater power being supplied.

A growing number of electrochemical technologies depend on fluid flow, and often that fluid is opaque. Measuring the flow of an opaque fluid is inherently ...

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 ...

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 ...

Sub-nanometer Resolution Imaging with Amplitude-modulation Atomic Force Microscopy in Liquid

Atomic force microscopy (AFM) has become a well-established technique for nanoscale imaging of samples in air and in liquid. Recent studies have shown that when operated in amplitude-modulation (tapping) mode, atomic or molecular-level resolution images can be achieved over a wide range of soft and hard samples in liquid. In these situations, small oscillation amplitudes (SAM-AFM) enhance the resolution by exploiting the solvated liquid at the surface of the sample. Although the technique has been successfully applied across fields as diverse as materials science, biology and biophysics and surface chemistry, obtaining high-resolution images in liquid can still remain challenging for novice users. This is partly due to the large number of variables to control and optimize such as the choice of cantilever, the sample preparation, and the correct manipulation of the imaging parameters. Here, we present a protocol for achieving high-resolution images of hard and soft samples in fluid using SAM-AFM on a commercial instrument. Our goal is to provide a step-by-step practical guide to achieving high-resolution images, including the cleaning and preparation of the apparatus and the sample, the choice of cantilever and optimization of the imaging parameters. For each step, we explain the scientific rationale behind our choices to facilitate the adaptation of the methodology to every user's specific system.

We present a method for achieving sub-nanometer resolution images with amplitude-modulation (tapping mode) atomic force microscopy in liquid. The method is demonstrated on commercial atomic force microscopes. We explain the rationale behind our choices of parameters and suggest strategies for resolution optimization.

Atomic force microscopy (AFM) has become a well-established technique for nanoscale imaging of samples in air and in liquid. Recent studies have shown ...

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 ...

Orientational Transition in a Liquid Crystal Triggered by the Thermodynamic Growth of Interfacial Wetting Sheets

In liquid crystal (LC) physical chemistry, molecules near the surface play a great role in controlling bulk orientation. Thus far, mainly to achieve desired molecular orientation states in LC displays, the "static" surface property of LCs, so-called surface anchoring, has been intensively studied. As a rule of thumb, once the initial orientation of LCs is "locked" by specific surface treatments, such as rubbing or treatment with a specific alignment layer, it hardly changes with temperature. Here, we present a system exhibiting an orientational transition upon temperature variation, which conflicts with the consensus. Right on the transition, the bulk LC molecules experience the orientational rotation, with 90&#176; between the planar (P) orientation at high temperatures and the vertical (V) orientation at low temperatures in the first-order transitional manner. We have tracked thermodynamic surface anchoring behavior by means of polarizing optical microscopy (POM), dielectric spectroscopy (DS), high-resolution differential scanning calorimetry (HR-DSC), and grazing incidence X-ray diffraction (GI-XRD) and reached a plausible physical explanation: that the transition is triggered by a growth of surface wetting sheets, which impose the V orientation locally against the P orientation in the bulk. This landscape would provide a general link explaining how the equilibrium bulk orientation is affected by surface-localized orientation in many LC systems. In our characterization, POM and DS are advantageous by offering information on the spatial distribution of the orientation of LC molecules. HR-DSC gives information about the precise thermodynamic information on transitions, which cannot be addressed by conventional DSC instruments due to limited resolution. GI-XRD provides information on surface-specific molecular orientation and short-range orderings. The goal of this paper is to present a protocol for preparing a sample that exhibits the transition and to demonstrate how the thermodynamic structural variation, both in the bulk and on surfaces, can be analyzed through the abovementioned methods.

Here, we present a protocol to trigger an orientational transition of a liquid crystal in response to temperature. Methodologies are described for preparing a sample in order to observe the transition and the detailed transitional evolution.

In liquid crystal (LC) physical chemistry, molecules near the surface play a great role in controlling bulk orientation. Thus far, mainly to achieve ...

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.

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 ...

A Fabrication and Measurement Method for a Flexible Ferroelectric Element Based on Van Der Waals Heteroepitaxy

Flexible non-volatile memories have received much attention as they are applicable for portable smart electronic device in the future, relying on high-density data storage and low-power consumption capabilities. However, the high-quality oxide based nonvolatile memory on flexible substrates is often constrained by the material characteristics and the inevitable high-temperature fabrication process. In this paper, a protocol is proposed to directly grow an epitaxial yet flexible lead zirconium titanate memory element on muscovite mica. The versatile deposition technique and measurement method enable the fabrication of flexible yet single-crystalline non-volatile memory elements necessary for the next generation of smart devices.

In this paper, we present a protocol to directly grow an epitaxial yet flexible lead zirconium titanate memory element on muscovite mica.

Flexible non-volatile memories have received much attention as they are applicable for portable smart electronic device in the future, relying on ...

Measurement of Dynamic Force Acted on Water Strider Leg Jumping Upward by the PVDF Film Sensor

This study aimed to make an explanation for the phenomenon in nature that water strider usually jumps or glides on the water surface easily but quickly, with its peak locomotion speed reaching 150 cm/s. First of all, we observed the microstructure and hierarchy of water strider legs using the scanning electron microscope. On the basis of the observed morphology of the legs, a theoretical model of the detachment from water surface was established, which explained water striders' capability to slide on water surface effortlessly in terms of energy reduction. Secondly, a dynamic force measurement system was devised using the PVDF film sensor with excellent sensitivity, which could detect the whole interaction process. Subsequently, a single leg in contact with water was pulled upward at different speeds, and the adhesion force was measured at the same time. The results of the departing experiment suggested a deep understanding of the fast jumping of water striders.

The protocol here is dedicated to investigating the free and quick maneuvering of water strider on water surface. The protocol includes observing the microstructure of legs and measuring the adhesion force when departing from water surface at different speeds.

This study aimed to make an explanation for the phenomenon in nature that water strider usually jumps or glides on the water surface easily but quickly, ...