This work was supported by JSPS KAKENHI grant Number 16H06037. We sincerely thank Dr. Yuji Sasaki in Hokkaido University for technical assistance for HR-DSC.

1. Preparation of the Liquid Crystal Alignment Layer of a Perfluoropolymer onto Glass Substrates
<ol>
	<li>Preparation of the perfluoropolymer solution
	<ol>
		<li>Prepare 1 mL of the perfluoropolymer solution by dissolving a perfluoropolymer solution (9 wt% polymer) in a commercial solvent at a ratio of 1:2; this ensures uniform films 0.5-1 &#181;m thick to be spin-coated. 
		NOTE: Please see the Materials List for the solution and solvent used.</li>
	</ol>
	</li>
	<li>Coating of the perf...

<ol>
	<li>Woltman, S. J., Jay, G. D., Crawford, G. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Liquid-Crystal+Materials+Find+a+New+Order+in+Biomedical+Applications.">Liquid-Crystal Materials Find a New Order in Biomedical Applications.</a> Nat. Mater. 6 (12), 929-938 (2007).</li><li>Carlton, R. J., 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=Chemical+and+Biological+Sensing+Using+Liquid+Crystals.">Chemical and Biological Sensing Using Liquid Crystals.</a> Liq. Cryst.Rev. 1 (1), 29-51 (2013).</li><li>Patel, J. S., Yokoyama, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Continuous+Anchoring+Transition+in+Liquid+Crystals.">Continuous Anchoring Transition in Liquid Crystals.</a> Nature. 362, 525-527 (1993).</li><li>Senyuk, B., 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=Surface+alignment,+anchoring+transitions,+optical+properties,+and+topological+defects+in+the+nematic+phase+of+thermotropic+bent-core+liquid+crystal+A131.">Surface alignment, anchoring transitions, optical properties, and topological defects in the nematic phase of thermotropic bent-core liquid crystal A131.</a> Phys Rev E. 82 (4 Pt 1), 041711 (2010).</li><li>Bechhoefer, J., 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=Critical+Behavior+in+Anchoring+Transitions+of+Nematic+Liquid+Crystals.">Critical Behavior in Anchoring Transitions of Nematic Liquid Crystals.</a> Phys. Rev. Lett. 64 (16), 1911-1914 (1990).</li><li>Dhara, S., 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=Anchoring+Transitions+of+Transversely+Polar+Liquid-Crystal+Molecules+on+Perfluoropolymer+Surfaces.">Anchoring Transitions of Transversely Polar Liquid-Crystal Molecules on Perfluoropolymer Surfaces.</a> Phys. Rev. E. 79 (6 Pt 1), 60701 (2009).</li><li>Aya, S., 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=Stepwise+heat-capacity+change+at+an+orientation+transition+in+liquid+crystals.">Stepwise heat-capacity change at an orientation transition in liquid crystals.</a> Phys. Rev. E. 86 (2), 022512 (2014).</li><li>Aya, S., 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=Thermodynamically+Anchoring-Frustrated+Surface+to+Trigger+Bulk+Discontinuous+Orientational+Transition.">Thermodynamically Anchoring-Frustrated Surface to Trigger Bulk Discontinuous Orientational Transition.</a> Langmuir. 32 (41), 10545-10550 (2016).</li><li>Dhara, S., Madhusudana, N. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Physical+characterisation+of+4'-butyl-4-heptyl-bicyclohexyl-4-carbonitrile.">Physical characterisation of 4'-butyl-4-heptyl-bicyclohexyl-4-carbonitrile.</a> Phase Trans. 81 (6), 561-569 (2008).</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>Perkowski, P., 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=Technical+aspects+of+dielectric+spectroscopy+measurements+of+liquid+crystals.">Technical aspects of dielectric spectroscopy measurements of liquid crystals.</a> Opto-Electronics Review. 16 (3), 271-276 (2008).</li><li>Inaba, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nano-watt+stabilized+DSC+and+ITS+applications.">Nano-watt stabilized DSC and ITS applications.</a> J Therm Anal Calorim. 79 (3), 605-613 (2005).</li><li>Leveiller, F., Boehm, C., Jacquemain, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Two-dimensional+crystal+structure+of+cadmium+arachidate+studied+by+synchrotron+X-ray+diffraction+and+reflectivity.">Two-dimensional crystal structure of cadmium arachidate studied by synchrotron X-ray diffraction and reflectivity.</a> Langmuir. 10 (3), 819-829 (1994).</li><li>de Gennes, P. G., Prost, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> The Physics of Liquid Crystals (Second Edition). , (1993).</li><li>Aya, S., 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=Critical+Behavior+in+an+Electric-Field-Induced+Anchoring+Transition+in+a+Liquid+Crystal.">Critical Behavior in an Electric-Field-Induced Anchoring Transition in a Liquid Crystal.</a> Phys. Rev. E. 86 (1 Pt 1), 10701 (2012).</li><li>Avrami, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Kinetics+of+Phase+Change.+I+General+Theory.">Kinetics of Phase Change. I General Theory.</a> J. Chem. Phys. 7, 1103-1112 (1939).</li><li>Avrami, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Kinetics+of+Phase+Change.+II+Transformation-Time+Relations+for+Random+Distribution+of+Nuclei.">Kinetics of Phase Change. II Transformation-Time Relations for Random Distribution of Nuclei.</a> J. Chem. Phys. 8 (2), 212-224 (1939).</li><li>Avrami, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Granulation+Phase+Change,+and+Microstructure+Kinetics+of+Phase+Change.+III.">Granulation Phase Change, and Microstructure Kinetics of Phase Change. III.</a> J. Chem. Phys. 9, 177-184 (1941).</li><li>Sasaki, 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=Distinctive+Thermal+Behavior+and+Nanoscale+Phase+Separation+in+the+Heterogeneous+Liquid-+Crystal+B4+Matrix+of+Bent-Core+Molecules.">Distinctive Thermal Behavior and Nanoscale Phase Separation in the Heterogeneous Liquid- Crystal B4 Matrix of Bent-Core Molecules.</a> Phys. Rev. Lett. 107 (23), 237802 (2011).</li></ol>

The 10x POM images taken using a 5-&#181;m LC cell (Figures 1a and b) clearly show that the orientational state of the bulk LC molecules transits between the P and the V orientations upon temperature variation in a first-order manner. This is marked by the domain nucleation and growth processes, with a new orientation differing from the initial orientation by 90&#176;. The transition temperatures upon cooling and heating are 321.5 K and 325.3 K, respectively. Since CCN47 has a birefringe...

In recent years, there has been growing interest in learning how dynamic molecular features and structures of surface molecules in response to external stimuli might affect the bulk orientation of materials in LC states. One example is to use LC biosensors as a new application of LCs1,2. To quantify how many target bio-species are detected, it is important to know how the interfacial LCs that contact adhering target molecules change and evolve, while also detecting and how they transfer/translate their properties into the bulk.
Using models to pursue these answers, we started with systems that have their surface molecular orientation and short-range orderings varying thermodynamically. These systems allow us to correlate the changes in surface orientation and orderings with the resulting bulk orientation in a systematic way. Recently, we found several LC systems that exhibit orientational transitions, where a spontaneous bulk molecular orientation changes with temperature. In principle, orientational transitions can be categorized into either quasi-second-order3,4 or quasi-first-order transition5,6,7,8. The former is accompanied by a continuous bulk molecular reorientation upon changes in temperature, whereas the latter demonstrates a discontinuous one. In this article, we describe an orientational transition in the quasi-first-order manner between the P and the V orientational states. It proceeds in the single nematic (N) phase by changing the temperature. Details will be provided in the Representative Results and the Discussion.
Since orientational change in the bulk should be governed by a change in the surface molecular orientation and short-range orderings, it is apparent that this system can potentially offer insights into how the thermodynamic variation in surface molecular orientation and short-range orderings affects the bulk orientation. In this article, with the goal of understanding the abovementioned issues, we tackled three problems using four complementary methods (i.e., POM, DS, HR-DSC, and GI-XRD): (1) What does the orientational transition look like? (2) Is the orientational transition thermally detectable? (3) Why and how does the orientational transition occur?

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>CYTOP</td>
			<td>Asahi Glass Co. Ltd.</td>
			<td>CTX-809A</td>
			<td></td>
		</tr>
		<tr>
			<td>Solvent for CYTOP</td>
			<td>Asahi Glass Co. Ltd.</td>
			<td>CT-180 Sol.</td>
			<td></td>
		</tr>
		<tr>
			<td>Alkaline detergent</td>
			<td>Merck KGaA</td>
			<td>Extran MA01</td>
			<td></td>
		</tr>
		<tr>
			<td>NOA61</td>
			<td>Norland Products, Inc.</td>
			<td>#37-322</td>
			<td>Purchasable from Edmund Optics</td>
		</tr>
		<tr>
			<td>AL1254</td>
			<td>JSR Corporation</td>
			<td></td>
			<td>Planar alignment material in self-made cells</td>
		</tr>
		<tr>
			<td>4&#8217;-butyl-4-heptyl-bicyclohexyl-4-carbonitrile</td>
			<td>Nematel GmbH &#38; Co. KG</td>
			<td></td>
			<td>Custom-made</td>
		</tr>
		<tr>
			<td>UV-O3 cleaner</td>
			<td>Technovision Inc.</td>
			<td>UV-208</td>
			<td></td>
		</tr>
		<tr>
			<td>Hot-stage system</td>
			<td>Mettler Toledo</td>
			<td>HS82</td>
			<td></td>
		</tr>
		<tr>
			<td>High-Definition Color Camera Head</td>
			<td>Nikon</td>
			<td>DS-Fi1</td>
			<td></td>
		</tr>
		<tr>
			<td>Impedance/gain-phase analyzer</td>
			<td>Solartron Analytical</td>
			<td>1260</td>
			<td></td>
		</tr>
		<tr>
			<td>Indium Tin Oxide (ITO)-coated substrate</td>
			<td>GEOMATEC Co. Ltd.</td>
			<td></td>
			<td>Custom-made</td>
		</tr>
	</tbody>
</table>

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.

POM images, DS data, HR-DSC data, and GI-XRD patterns were collected during temperature variation, especially in the vicinity of the orientational transition upon both cooling and heating.
Figure 1 represents the evolution of the texture made by POM and DS measurements during the POM observation of the orientational transition from the P (V) to the V (P) orientational state during cooling (heating)....

Watch this Scientific Journal Video about Orientational Transition in a Liquid Crystal Triggered by the Thermodynamic Growth of Interfacial Wetting Sheets at JoVE.com

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

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 ...

The overall goal of this procedure is to trigger an orientational transition of a liquid crystal in response to temperature. And to characterize the transition. This method can help answer key questions in the liquid crystal field, such as thermodynamic surface anchoring behaviors.And the advantage of this protocol is that the orientational transition can be clearly visualized in this continuous manner. And if the involved physical properties can be systematically probed. To begin this procedure, prepare one milliliter of perfluoropolymer solution by dissolving the desired perfluoropolymer in a commercial solvent at a ratio of one to two to ensure uniform films 0.5 to 1 micrometer thick for spin coating.Next, wash glass substrates by sonication at 42 kilohertz in an alkaline detergent. Then, repeatedly rinse each substrate with distilled water. After rinsing and drying the substrates, subject them to UV ozone cleaner for 10 minutes.Following this, drip 20 microliters of the perfluoropolymer solution onto each cleaned glass substrate. Immediately spin coat the solution at 3, 500 rpm and room temperature for 70 seconds. Then, bake the film at 80 degrees Celsius for 60 minutes to remove the solvent, and at 200 degrees Celsius for 60 minutes for curing.Apply a photo-curable resin pre-mixed with micrometer sized glass particles to one of the film-coated glass substrates. Then, place a second film coated glass substrate on top of the first substrate And use an LED lamp with a wavelength of 365 nanometers to glue the two substrates together. Next introduce 0.2 to 10 microliters of CCN47 to each of the prepared LC cells using a spatula under capillary force at a temperature higher than the isotropic nematic phase transition temperature.Now, observe the LC cells under polarizing optical microscopy with four to 100X objective lenses in conjunction with a hot stage to control the sample temperature with plus or minus 0.1 Kelvin accuracy. Using a digital color camera, record the textures in more than five frames, at even intervals per Kelvin, both upon cooling and heating in the range of 291 to 343 Kelvin. For dielectric spectroscopy, prepare an LC cell with ITO electrodes by soldering lead wire to each substrate.To measure the capacitance of the LC cells, wire the cells to the terminals of a commercial impedance gain phase analyzer. Then, measure the time dependence of capacitance of the LC cells every five minutes with the analyzer. For HR-DSC analysis place the LC cells into a homemade HR-DSC to be examined.Perform measurements with scan rates of 0.05 to 0.10 Kelvin per minute to enhance the minimum temperature resolving power. The evolution of the texture made by polarizing optical microscopy and dielectric spectroscopy measurements during the orientational transition from the planar to vertical orientational state during cooling and heating is depicted here. Upon cooling, the planar orientation is right below the isotropic nematic transition temperature.With the appearance of two and four brush Schlieren textures. By annealing or further cooling, the field of vision becomes completely dark, suggesting the completion of the orientational transition. HR-DSC data representing the heat flow through the sample as a function of temperature and time is shown here.The variation of heat flow with time data was used to analyze the Avrami exponent after the orientational transition. Grazing incidents x-ray diffraction patterns in droplet geometry and in C2 LC cell geometry at various temperatures. Demonstrate short range ordering of quasi-smectic a-wetting sheets.With layer structures formed near the surface. Even in the temperature range of the planar orientational states, quasi-smectic a-wetting sheets persist, indicating that the surface orientational condition is frustrated. The hysteresis range is consistent with the hysteresis range confirmed by polarizing optical microscopy and dielectric spectroscopy, which suggests that the orientational transition is triggered by quasi-smectic a-wetting sheet growth.So once mastered, the observation of the orientational transition can be done in four hours if the preparation procedures are performed properly. Following this procedure, other methods like fluorescent confocal microscopy and non-linear optical analysis can be performed in order to answer additional questions, like the special distribution of orientations of the liquid crystal director. After its development, this technique paved the way for researchers in the field of surface science of liquid crystals to explore links between the microscopic structures near surfaces and the microscopic structures and properties.After watching this video you should have a good understanding of how to prepare a sample to observe the orientational transition and how to characterize the important physical properties.

orientational-transition-liquid-crystal-triggered-thermodynamic

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7.0K ビュー.  RIKEN Center for Emergent Matter Science (CEMS). The overall goal of this procedure is to trigger an orientational transition of a liquid crystal in response to temperature. And to characterize the transition. This method can help answer key questions in the liquid crystal field, such as thermodynamic surface anchoring behaviors.And the advantage of this protocol is that the orientational transition can be clearly visualized in this continuous manner. And if the involved physical properties can be systematically probed. To begin this...

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

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...

determination of aggregate surface morphology at the interfacial transition zone (itz)

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone ITZ

Hereby, we proposed a protocol to illustrate the effect of aggregate surface morphology on the ITZ microstructure. The SEM-BSE image were quantitatively analyzed to obtain ITZ's porosity gradient via digital image processing and a K-means clustering algorithm was further employed to establish a relationship between porosity gradient and surface...

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone (ITZ)

preparation of monodomain liquid crystal elastomers and liquid crystal elastomer nanocomposites

Preparation of Monodomain Liquid Crystal Elastomers and Liquid Crystal Elastomer Nanocomposites

We demonstrate the preparation of siloxane-based and epoxy-based liquid crystal elastomers (LCEs) and LCE nanocomposites. The LCEs are characterized with respect to reversible strain, liquid crystal ordering, and stiffness. As a potential application, we demonstrate their use as shape-responsive substrates in a custom device for active cell...

preparation of liquid crystal networks for macroscopic oscillatory motion induced by light

Preparation of Liquid Crystal Networks for Macroscopic Oscillatory Motion Induced by Light

The goal of the protocol is to create liquid crystalline polymer films that can mechanically oscillate under continuous light irradiation. We describe in great detail the conception of free-standing films, from the liquid crystal alignment method to the photo-actuation. The experimental protocol applied to prepare this material is broadly...

high-contrast and fast photorheological switching of a twist-bend nematic liquid crystal

High-Contrast and Fast Photorheological Switching of a Twist-Bend Nematic Liquid Crystal

This protocol demonstrates the preparation of a photorheological material that exhibits a solid phase, various liquid crystalline phases, and an isotropic liquid phase by increasing temperature. Presented here are methods for measuring the structure-viscoelasticity relationship of the...

optimization of crystal growth for neutron macromolecular crystallography

Optimization of Crystal Growth for Neutron Macromolecular Crystallography

Structural studies of biomacromolecules by crystallography require high-quality crystals. Here we demonstrate a protocol that can be used by OptiCrys (a fully automated instrument developed in our lab) and/or microdialysis buttons for growing large high-quality crystals based on knowledge of the crystallization phase...

targeted plasma membrane delivery of a hydrophobic cargo encapsulated in a liquid crystal nanoparticle carrier

Targeted Plasma Membrane Delivery of a Hydrophobic Cargo Encapsulated in a Liquid Crystal Nanoparticle Carrier

A liquid crystal nanoparticle (LCNP) nanocarrier is exploited as a vehicle for the controlled delivery of a hydrophobic cargo to the plasma membrane of living...

determination of thermodynamic properties of alkaline earth-liquid metal alloys using the electromotive force technique

Determination of Thermodynamic Properties of Alkaline Earth-liquid Metal Alloys Using the Electromotive Force Technique

This protocol describes the measurement of the electromotive force of alkaline-earth elements in liquid metal alloys at high temperatures (723-1,123 K) to determine their thermodynamic properties, including activity, partial molar entropy, partial molar enthalpy, and phase transition temperatures, over a wide composition...

studying the effects of temperature on the nucleation and growth of nanoparticles by liquid-cell transmission electron microscopy

Studying the Effects of Temperature on the Nucleation and Growth of Nanoparticles by Liquid-Cell Transmission Electron Microscopy

Temperature control during liquid-phase electron microscopy experiments opens up new perspectives of studying the dynamic of nanoparticles in liquid environments mimicking their formation or application media. Using recently developed heating liquid cells, we directly observed the influence of temperature on the nucleation and growth processes of gold nanoparticles in water.

molecular analysis of endothelial-mesenchymal transition induced by transforming growth factor-&#946; signaling

Molecular Analysis of Endothelial-mesenchymal Transition Induced by Transforming Growth Factor-&amp;#946; Signaling

A protocol for in vitro induction of endothelial-mesenchymal transition (EndMT), which is useful for investigating cellular signaling pathways involved in EndMT, is described. In this experimental model, EndMT is induced by treatment with TGF-&#946; in MS-1 endothelial...

Molecular Analysis of Endothelial-mesenchymal Transition Induced by Transforming Growth Factor-&#946; Signaling

preparation of liquid-exfoliated transition metal dichalcogenide nanosheets with controlled size and thickness: a state of the art protocol

Preparation of Liquid-exfoliated Transition Metal Dichalcogenide Nanosheets with Controlled Size and Thickness: A State of the Art Protocol

A protocol for the liquid exfoliation of layered materials to nanosheets, their size selection and size measurement by microscopic and spectroscopic techniques is...

preparation of large-area vertical 2d crystal hetero-structures through the sulfurization of transition metal films for device fabrication

Preparation of Large-area Vertical 2D Crystal Hetero-structures Through the Sulfurization of Transition Metal Films for Device Fabrication

Through the sulfurization of pre-deposited transition metals, large-area and vertical 2D crystal hetero-structures can be fabricated. The film transferring and device fabrication procedures are also demonstrated in this...

pattern-triggered oxidative burst and seedling growth inhibition assays in arabidopsis thaliana

Pattern-Triggered Oxidative Burst and Seedling Growth Inhibition Assays in Arabidopsis thaliana

This paper describes two methods for quantifying defense responses in Arabidopsis thaliana following exposure to immune elicitors: the transient oxidative burst, and the inhibition of seedling...

Pattern-Triggered Oxidative Burst and Seedling Growth Inhibition Assays in Arabidopsis thaliana

synthesis of biocompatible liquid crystal elastomer foams as cell scaffolds for 3d spatial cell cultures

Synthesis of Biocompatible Liquid Crystal Elastomer Foams as Cell Scaffolds for 3D Spatial Cell Cultures

This study presents a methodology to prepare 3D, biodegradable, foam-like cell scaffolds based on biocompatible side-chain liquid crystal elastomers (LCEs). Confocal microscopy experiments show that foam-like LCEs allow for cell attachment, proliferation, and the spontaneous alignment of C2C12s...

visualization of vascular ca2+ signaling triggered by paracrine derived ros

Visualization of Vascular Ca2+ Signaling Triggered by Paracrine Derived ROS

An efficient method to gain insights into visualizing the paracrine-derived ROS induction of endothelial Ca2+ signaling is described. This method takes advantage of measuring paracrine derived ROS triggered Ca2+ mobilization in vascular endothelial cells in a co-culture...

Visualization of Vascular Ca2+ Signaling Triggered by Paracrine Derived ROS

using the dot assay to analyze migration of cell sheets

Using the Dot Assay to Analyze Migration of Cell Sheets

Cell migration is essential for development, tissue maintenance and repair, and tumorigenesis, and is regulated by growth factors, chemokines, and cytokines. This protocol describes the dot assay, a two-dimensional, unconstrained migration assay to assess the migratory phenotype of attached, cohesive cell sheets in response to microenvironmental...

tissue engineering: construction of a multicellular 3d scaffold for the delivery of layered cell sheets

Tissue Engineering: Construction of a Multicellular 3D Scaffold for the Delivery of Layered Cell Sheets

For creation of highly organized structures of complex tissue, one must assemble multiple material and cell types into an integrated composite.  This combinatorial design incorporates organ-specific layered cell sheets with two distinct biologically-derived materials containing a strong fibrous matrix base, and endothelial cells for enhancing new vessels...

recurrent escherichia coli urinary tract infection triggered by gardnerella vaginalis bladder exposure in mice

Recurrent Escherichia coli Urinary Tract Infection Triggered by Gardnerella vaginalis Bladder Exposure in Mice

A mouse model of uropathogenic E. coli (UPEC) transurethral inoculation to establish latent intracellular bladder reservoirs and subsequent bladder exposure to G. vaginalis to induce recurrent UPEC UTI is demonstrated. Also demonstrated are the enumeration of bacteria, urine cytology, and in situ bladder fixation and processing for scanning electron...

Recurrent Escherichia coli Urinary Tract Infection Triggered by Gardnerella vaginalis Bladder Exposure in Mice

determining the thermodynamic and kinetic association of a dna aptamer and tetracycline using isothermal titration calorimetry

Determining the Thermodynamic and Kinetic Association of a DNA Aptamer and Tetracycline Using Isothermal Titration Calorimetry

The present protocol describes the use of Isothermal Titration Calorimetry (ITC) to analyze the association and dissociation kinetics of the binding between a DNA aptamer and tetracycline, including sample preparation, running standards and samples, and interpreting the resulting data.

Dry Oxidation and Vacuum Annealing Treatments for Tuning the Wetting Properties of Carbon Nanotube Arrays

In this article, we describe a simple method to reversibly tune the wetting properties of vertically aligned carbon nanotube (CNT) arrays. Here, CNT arrays are defined as densely packed multi-walled carbon nanotubes oriented perpendicular to the growth substrate as a result of a growth process by the standard thermal chemical vapor deposition (CVD) technique.1,2 These CNT arrays are then exposed to vacuum annealing treatment to make them more hydrophobic or to dry oxidation treatment to render them more hydrophilic. The hydrophobic CNT arrays can be turned hydrophilic by exposing them to dry oxidation treatment, while the hydrophilic CNT arrays can be turned hydrophobic by exposing them to vacuum annealing treatment. Using a combination of both treatments, CNT arrays can be repeatedly switched between hydrophilic and hydrophobic.2 Therefore, such combination show a very high potential in many industrial and consumer applications, including drug delivery system and high power density supercapacitors.3-5
The key to vary the wettability of CNT arrays is to control the surface concentration of oxygen adsorbates. Basically oxygen adsorbates can be introduced by exposing the CNT arrays to any oxidation treatment. Here we use dry oxidation treatments, such as oxygen plasma and UV/ozone, to functionalize the surface of CNT with oxygenated functional groups. These oxygenated functional groups allow hydrogen bond between the surface of CNT and water molecules to form, rendering the CNT hydrophilic. To turn them hydrophobic, adsorbed oxygen must be removed from the surface of CNT. Here we employ vacuum annealing treatment to induce oxygen desorption process. CNT arrays with extremely low surface concentration of oxygen adsorbates exhibit a superhydrophobic behavior.

This article describes a simple method to fabricate vertically aligned carbon nanotube arrays by CVD and to subsequently tune their wetting properties by exposing them to vacuum annealing or dry oxidation treatment.

In this article, we describe a simple method to reversibly  tune the wetting properties of vertically aligned carbon nanotube (CNT) arrays.  Here, CNT ...

Characterization of Recombination Effects in a Liquid Ionization Chamber Used for the Dosimetry of a Radiosurgical Accelerator

Most modern radiation therapy devices allow the use of very small fields, either through beamlets in Intensity-Modulated Radiation Therapy (IMRT) or via stereotactic radiotherapy where positioning accuracy allows delivering very high doses per fraction in a small volume of the patient. Dosimetric measurements on medical accelerators are conventionally realized using air-filled ionization chambers. However, in small beams these are subject to nonnegligible perturbation effects. This study focuses on liquid ionization chambers, which offer advantages in terms of spatial resolution and low fluence perturbation. Ion recombination effects are investigated for the microLion detector (PTW) used with the Cyberknife system (Accuray). The method consists of performing a series of water tank measurements at different source-surface distances, and applying corrections to the liquid detector readings based on simultaneous gaseous detector measurements. This approach facilitates isolating the recombination effects arising from the high density of the liquid sensitive medium and obtaining correction factors to apply to the detector readings. The main difficulty resides in achieving a sufficient level of accuracy in the setup to be able to detect small changes in the chamber response.

A growing number of radiation therapy devices offer the advantage of delivering the dose through very small beams to the tumor, allowing for increased conformity and higher doses per fraction. Many different detectors can be used for the dosimetry of these small fields. In the present study, the effect of ion recombination is investigated for a liquid ionization chamber using a stereotactic radiation therapy system.

Most modern radiation therapy devices allow the use of very small fields, either through beamlets in Intensity-Modulated Radiation Therapy (IMRT) or via ...

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 ...

How to Ignite an Atmospheric Pressure Microwave Plasma Torch without Any Additional Igniters

This movie shows how an atmospheric pressure plasma torch can be ignited by microwave power with no additional igniters. After ignition of the plasma, a stable and continuous operation of the plasma is possible and the plasma torch can be used for many different applications. On one hand, the hot (3,600 K gas temperature) plasma can be used for chemical processes and on the other hand the cold afterglow (temperatures down to almost RT) can be applied for surface processes. For example chemical syntheses are interesting volume processes. Here the microwave plasma torch can be used for the decomposition of waste gases which are harmful and contribute to the global warming but are needed as etching gases in growing industry sectors like the semiconductor branch. Another application is the dissociation of CO2. Surplus electrical energy from renewable energy sources can be used to dissociate CO2 to CO and O2. The CO can be further processed to gaseous or liquid higher hydrocarbons thereby providing chemical storage of the energy, synthetic fuels or platform chemicals for the chemical industry. Applications of the afterglow of the plasma torch are the treatment of surfaces to increase the adhesion of lacquer, glue or paint, and the sterilization or decontamination of different kind of surfaces. The movie will explain how to ignite the plasma solely by microwave power without any additional igniters, e.g., electric sparks. The microwave plasma torch is based on a combination of two resonators &#8212; a coaxial one which provides the ignition of the plasma and a cylindrical one which guarantees a continuous and stable operation of the plasma after ignition. The plasma can be operated in a long microwave transparent tube for volume processes or shaped by orifices for surface treatment purposes.

This movie shows how an atmospheric plasma torch can be ignited by microwaves with no additional igniters and provides a stable and continuous plasma operation suitable for plenty of applications.

This movie shows how an atmospheric pressure plasma torch can be ignited by microwave power with no additional igniters. After ignition of the plasma, a ...

How to Build a Vacuum Spring-transport Package for Spinning Rotor Gauges

The spinning rotor gauge (SRG) is a high-vacuum gauge often used as a secondary or transfer standard for vacuum pressures in the range of 1.0 x 10-4 Pa to 1.0 Pa. In this application, the SRGs are frequently transported to laboratories for calibration. Events can occur during transportation that change the rotor surface conditions, thus changing the calibration factor. To assure calibration stability, a spring-transport mechanism is often used to immobilize the rotor and keep it under vacuum during transport. It is also important to transport the spring-transport mechanism using packaging designed to minimize the risk of damage during shipping. In this manuscript, a detailed description is given on how to build a robust spring-transport mechanism and shipping container. Together these form a spring-transport package. The spring-transport package design was tested using drop-tests and the performance was found to be excellent. The present spring-transport mechanism design keeps the rotor immobilized when experiencing shocks of several hundred g (g = 9.8 m/sec2 and is the acceleration due to gravity), while the shipping container assures that the mechanism will not experience shocks greater than about 100 g during common shipping mishaps (as defined by industry standards).

Here we describe how to build a robust spring-transport mechanism for a spinning rotor gauge. This device securely immobilizes the rotor and keeps it under vacuum during transportation. We also describe packaging that minimizes the risk of damage during transport. Tests show our design works for typical shocks during transport.

The spinning rotor gauge (SRG) is a high-vacuum gauge often used as a secondary or transfer standard for vacuum pressures in the range of 1.0 x 10-4 Pa to ...

Effect of Bending on the Electrical Characteristics of Flexible Organic Single Crystal-based Field-effect Transistors

The charge transport in an organic semiconductor depends highly on the molecular packing in the crystal, which influences the electronic coupling immensely. However, in soft electronics, in which organic semiconductors play a critical role, the devices will be bent or folded repeatedly. The effect of bending on the crystal packing and thus the charge transport is crucial to the performance of the device. In this manuscript, we describe the protocol to bend a single crystal of 5,7,12,16-tetrachloro-6,13-diazapentacene (TCDAP) in the field-effect transistor configuration and to obtain reproducible I-V characteristics upon bending the crystal. The results show that bending a field-effect transistor prepared on a flexible substrate results in nearly reversible yet opposite trends in charge mobility, depending on the bending direction. The mobility increases when the device is bent toward the top gate/dielectric layer (upward, compressive state) and decreases when bent toward the crystal/substrate side (downward, tensile state). The effect of bending curvature was also observed, with greater mobility change resulting from higher bending curvature. It is suggested that the intermolecular &#960;-&#960; distance changes upon bending, thereby influencing the electronic coupling and the subsequent carrier transport ability.

This manuscript describes the bending process of an organic single crystal-based field-effect transistor to maintain a functioning device for electronic property measurement. The results suggest that bending causes changes in the molecular spacing in the crystal and thus in the charge hopping rate, which is important in flexible electronics.

The charge transport in an organic semiconductor depends highly on the molecular packing in the crystal, which influences the electronic coupling ...

We summarize recent advances in the production of liquid-exfoliated transition metal dichalcogenide (TMD) nanosheets with controlled size and thickness. Layered crystals of molybdenum disulphide (MoS2) and tungsten disulphide (WS2) are exfoliated in aqueous surfactant solution by sonication. This yields highly polydisperse mixtures containing nanosheets with broad size and thickness distributions. However, for most purposes, specific sizes (in terms of both lateral dimension and thickness) are required. For example, large and thin nanosheets are desired for (opto) electronic applications, while laterally small nanosheets are interesting for catalytic applications. Therefore, post-exfoliation size selection is an important step that we address here. We provide a detailed protocol on the efficient size selection in large quantities by liquid cascade centrifugation and the size and thickness quantification by statistical microscopic analysis (atomic force microscopy and transmission electron microscopy). The comparison of MoS2 and WS2 shows that both materials are size-selected in a similar way by the same procedure. Importantly, the dispersions of size-selected nanosheets show systematic changes in their optical extinction spectra with size due to edge and confinement effects. We show how these optical changes are related quantitatively to the nanosheets dimensions and describe how mean nanosheets length and layer number can be extracted reliably from the extinction spectra. The exfoliation and size selection protocol can be applied to a broad range of layered crystals as we have previously demonstrated for graphene, gallium sulphide (GaS) and black phosphorus.

A protocol for the liquid exfoliation of layered materials to nanosheets, their size selection and size measurement by microscopic and spectroscopic techniques is presented.

We summarize recent advances in the production of liquid-exfoliated transition metal dichalcogenide (TMD) nanosheets with controlled size and thickness. ...

Fabrication of 1-D Photonic Crystal Cavity on a Nanofiber Using Femtosecond Laser-induced Ablation

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using femtosecond laser-induced ablation. We show that thousands of periodic nano-craters are fabricated on an optical nanofiber by irradiating with just a single femtosecond laser pulse. For a typical sample, periodic nano-craters with a period of 350 nm and with diameter gradually varying from 50 - 250 nm over a length of 1 mm are fabricated on a nanofiber with diameter around 450 - 550 nm. A key aspect of such a nanofabrication is that the nanofiber itself acts as a cylindrical lens and focuses the femtosecond laser beam on its shadow surface. Moreover, the single-shot fabrication makes it immune to mechanical instabilities and other fabrication imperfections. Such periodic nano-craters on nanofiber, act as a 1-D PhC and enable strong and broadband reflection while maintaining the high transmission out of the stopband. We also present a method to control the profile of the nano-crater array to fabricate apodized and defect-induced PhC cavities on the nanofiber. The strong confinement of the field, both transverse and longitudinal, in the nanofiber-based PhC cavities and the efficient integration to the fiber networks, may open new possibilities for nanophotonic applications and quantum information science.

We present a protocol for fabricating 1-D photonic crystal cavities on subwavelength diameter silica fibers (optical nanofibers) using femtosecond laser-induced ablation.

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using ...

A strategy based on doped liquid crystalline networks is described to create mechanical self-sustained oscillations of plastic films under continuous light irradiation. The photo-excitation of dopants that can quickly dissipate light into heat, coupled with anisotropic thermal expansion and self-shadowing of the film, gives rise to the self-sustained deformation. The oscillations observed are influenced by the dimensions and the modulus of the film, and by the directionality and intensity of the light. The system developed offers applications in energy conversion and harvesting for soft-robotics and automated systems.
The general method described here consists of creating free-standing liquid crystalline films and characterizing the mechanical and thermal effects observed. The molecular alignment is achieved using alignment layers (rubbed polyimide), commonly used in the display manufacturing industry. To obtain actuators with large deformation, the mesogens are aligned and polymerized in a splay/bend configuration, i.e., with the director of the liquid crystals (LCs) going gradually from planar to homeotropic through the film thickness. Upon irradiation, the mechanical and thermal oscillations obtained are monitored with a high-speed camera. The results are further quantified by image analysis using an image processing program.

The goal of the protocol is to create liquid crystalline polymer films that can mechanically oscillate under continuous light irradiation. We describe in great detail the conception of free-standing films, from the liquid crystal alignment method to the photo-actuation. The experimental protocol applied to prepare this material is broadly applicable.

A strategy based on doped liquid crystalline networks is described to create mechanical self-sustained oscillations of plastic films under continuous ...