Name: preparation of janus particles and alternating current electrokinetic measurements with a rapidly fabricated indium tin oxide electrode array
Uploaded: 2017-06-23T14:00:00
Description: Watch this Scientific Journal Video about Preparation of Janus Particles and Alternating Current Electrokinetic Measurements with a Rapidly Fabricated Indium Tin Oxide Electrode Array at JoVE.com

This work was supported by the Ministry of Science and Technology, Taiwan, R.O.C., under Grant NSC 103-2112-M-002-008-MY3.

1. Fabrication of the Microchip
<ol>
	<li>Preparation of the ITO electrode
	<ol>
		<li>Use commercial illustration software to draw a cross pattern. Set the distance between the diagonal electrodes to 160 &#181;m and make the arms of the cross pattern 30 mm wide and 55 mm long, as shown in Figure 1. Save the illustration file as a DXF file.</li>
		<li>Use a glass cutter to trim the ITO glass to a size of 25 mm x 50 mm (width x length). Use 75% ethanol and DI water to rinse...

<ol>
	<li>Walther, A., M&#252;ller, A. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Janus+particles.">Janus particles.</a> Soft Matter. 4 (4), 663-668 (2008).</li><li>Chen, Y. -. L., Jiang, H. -. 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J., Bazant, M. Z., Velev, O. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Induced-charge+electrophoresis+of+metallodielectric+particles.">Induced-charge electrophoresis of metallodielectric particles.</a> Phys Rev Lett. 100 (5), 058302 (2008).</li><li>Peng, C., Lazo, I., Shiyanovskii, S. V., Lavrentovich, O. 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W. L., Lahann, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multicompartmental+microcylinders.">Multicompartmental microcylinders.</a> Angewandte Chemie International Edition. 48 (25), 4589-4593 (2009).</li><li>Nie, Z., Li, W., Seo, M., Xu, S., Kumacheva, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Janus+and+ternary+particles+generated+by+microfluidic+synthesis:+design,+synthesis,+and+self-assembly.">Janus and ternary particles generated by microfluidic synthesis: design, synthesis, and self-assembly.</a> J Am Chem Soc. 128 (29), 9408-9412 (2006).</li><li>Jiang, H. -. 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J., Morgan, H., Ramos, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Alternating+current+electrokinetic+properties+of+gold-coated+microspheres.">Alternating current electrokinetic properties of gold-coated microspheres.</a> Langmuir. 28 (39), 13861-13870 (2012).</li><li>Ren, Y. K., Morganti, D., Jiang, H. Y., Ramos, A., Morgan, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrorotation+of+metallic+microspheres.">Electrorotation of metallic microspheres.</a> Langmuir. 27 (6), 2128-2131 (2011).</li><li>Jones, T. B., Jones, T. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electromechanics of particles. , (2005).</li><li>Morganti, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> AC electrokinetic analysis of chemically modified microparticles. , (2012).</li><li>Morgan, H., Hughes, M. P., Green, N. 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Fabricating ITO electrode arrays using the fiber laser marking machine provides a rapid method to prepare electrodes with arbitrary patterns. However, there are still some disadvantages to this method, such as fewer charge carriers and the lower fabrication accuracy of ITO electrodes compared to metal electrodes created by traditional methods. These disadvantages could limit some experiments. For example, fewer charges carriers could affect the distribution of the electric field when there is a large distance between ele...

Janus particles, named after the Roman god with a double face, are asymmetric particles whose two sides have physically or chemically different surface properties1,2. Due to this asymmetric feature, Janus particles exhibit special responses under electric fields, such as DEP3,4,5,6, EROT2, and induced-charge electrophoresis (ICEP)7,8,9. Recently, several methods to prepare Janus particles have been reported, including the Pickering emulsion method10, the electrohydrodynamic co-jetting method11, and the microfluidic photopolymerization method12. However, these methods require a series of complicated apparatus and procedures. This article introduces a simple method to prepare Janus particles and fully coated metallic particles. A monolayer of micro-scaled silica particles is prepared in a drying process and is put into a sputtering device to be coated with Au. One hemisphere of the particle is shaded, and only the other hemisphere is coated with Au2,13. The monolayer of the Janus particle is stamped with a polydimethylsiloxane (PDMS) stamp and then treated with a second coating process to prepare fully coated metallic particles14.
To characterize the electrical properties of a Janus particle, different AC electrokinetic responses, such as DEP, EROT, and electro-orientation, are widely used9,15,16,17,18,19. For example, EROT is the steady-state rotational response of a particle under an externally imposed rotating electric field2,9,15,16. By measuring the EROT, the interaction between the induced dipole of the particles and the electric fields can be obtained. DEP, which arises from the interaction between the induced dipoles and a non-uniform electric field, is capable of leading to particle movement3,4,5,9,15. Different kinds of particles can be attracted to (positive DEP) or repelled from (negative DEP) the electrode edges, which serves as a general method for manipulating and characterizing particles in the microfluidic device. The translational (DEP) and rotational (EROT) characteristics of the particle under the electric field are dominated by the real and imaginary part of the Clausius-Mossotti (CM) factor, respectively. The CM factor depends on the electrical properties of the particles and the surrounding liquid, which are revealed from the characteristic frequency, &#969;c = 2&#963; / aCDL, of DEP and EROT, where &#963; is the liquid conductivity, a is the particle radius, and CDL is the capacitance of the electrical double layer15,16. To measure the EROT and DEP of particles, specially designed electrode array patterns are needed. Traditionally, a photolithographic technique is used to create electrode arrays and requires a series of complicated procedures, including photoresist spin-coating, mask alignment, exposure, and development15,18,19,20.
In this article, the rapid fabrication of electrode arrays is demonstrated by direct optical patterning. A transparent thin-film ITO layer, which is coated on the glass substrate, is partially removed by a fiber laser marking machine (1,064 nm, 20 W, 90 to 120 ns pulse width, and 20 to 80 kHz pulse repetition frequency) to form a four-phase electrode array. The distance between the diagonal electrodes is 150-800 &#181;m, which can be adjusted to suit the experiments. The four-phase electrode array can be used to characterize and concentrate particles in different microfluidic devices15,16,18. To generate the four-phase electric field, the electrode array is connected to a 2-channel function generator and to two invertors. The phase shift between the adjacent electrodes is set at either 90&#176; (for EROT) or 180&#176; (for DEP)15. The AC signal is applied at a 0.5 to 4 Vpp voltage amplitude, and the frequency ranges from 100 Hz to 5 MHz during the operation process. Janus particles, metallic particles, and silica particles are used as samples to measure their AC electrokinetic properties. Suspensions of the particles are placed on the center region of the electrode array and are observed under an inverted optical microscope with a 40X, NA 0.6 objective. Particle motion and rotation are recorded with a digital camera. The DEP movement is recorded at the annular region, between 40 and 65 &#181;m radially away from the array center, and EROT is recorded at the circular region, 65 &#181;m radially away from the array center. Particle velocity and angular velocity are measured by the particle-tracking method. The particle centroids are distinguished by gray scale or geometry of particles using software. The particle velocity and angular velocity are obtained by measuring the movements of the particle centroids.
This article provides a simple method to rapidly fabricate arbitrarily patterned electrode arrays. It introduces the preparation of fully or partially coated metallic particles, which can be used in different fields, with uses ranging from biology to industry applications.

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			<td height="21" style="height:21px;width:287px;">Silica Microsphere-2.34 &#181;m</td>
			<td style="width:187px;">Bangs Laboratories</td>
			<td style="width:129px;">SS04N</td>
			<td style="width:167px;"></td>
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			<td height="21" style="height:21px;width:287px;">Ethyl Alcohol (99.5%)</td>
			<td style="width:187px;">KATAYAMA CHEMICAL</td>
			<td style="width:129px;">E-0105</td>
			<td></td>
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		<tr height="42">
			<td height="42" style="height:42px;width:287px;">SYLGARD 184 A&#38;B Silicone Elastomer(PDMS)</td>
			<td>DOW CORNING</td>
			<td style="width:129px;"></td>
			<td>PDMS&#160;</td>
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			<td height="21" style="height:21px;width:287px;">&#160;ITO glass</td>
			<td style="width:187px;">Luminescence Technology</td>
			<td style="width:129px;">LT-G001</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:287px;">Fiber laser marking machine</td>
			<td style="width:187px;">Taiwan 3Axle Technology</td>
			<td style="width:129px;">TAFB-R-20W</td>
			<td></td>
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			<td height="21" style="height:21px;width:287px;">&#160;2-channel function generator</td>
			<td style="width:187px;">Gwinsek</td>
			<td style="width:129px;">AFG-2225</td>
			<td></td>
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			<td height="21" style="height:21px;width:287px;">CMOS camera</td>
			<td style="width:187px;">Point Grey</td>
			<td style="width:129px;">GS3-U3-32S4M-C</td>
			<td></td>
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			<td height="21" style="height:21px;width:287px;">Sputter</td>
			<td style="width:187px;">JEOL</td>
			<td style="width:129px;">JFC-1100E</td>
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			<td height="21" style="height:21px;width:287px;">Operational Amplifiers</td>
			<td style="width:187px;">Texas Instruments</td>
			<td style="width:129px;">LM6361N</td>
			<td>OP invertor&#160;</td>
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		<tr height="42">
			<td height="42" style="height:42px;width:287px;">Ultrasonic Cleaner</td>
			<td style="width:187px;">Gui Lin Yiyuan Ultrasonic Machinery Co.</td>
			<td style="width:129px;">DG-1</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:287px;">Microcentrifuge</td>
			<td style="width:187px;">Scientific Specialties, Inc.</td>
			<td style="width:129px;"></td>
			<td>1.5ml</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:287px;">Mini Centrifuge</td>
			<td style="width:187px;">LMS</td>
			<td style="width:129px;">MC-MCF-2360</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:287px;">Microscope cover glass</td>
			<td style="width:187px;">Marienfeld-Superior</td>
			<td style="width:129px;"></td>
			<td>18*18mm</td>
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			<td height="21" style="height:21px;width:287px;">Inverted optical microscope</td>
			<td style="width:187px;">Olympus</td>
			<td style="width:129px;">OX-71&#160;</td>
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		<tr height="21">
			<td height="21" style="height:21px;width:287px;">Parafilm</td>
			<td style="width:187px;">bemis</td>
			<td style="width:129px;"></td>
			<td>spacer</td>
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preparation of janus particles and alternating current electrokinetic measurements with a rapidly fabricated indium tin oxide electrode array

This article provides a simple method to prepare partially or fully coated metallic particles and to perform the rapid fabrication of electrode arrays, which can facilitate electrical experiments in microfluidic devices. Janus particles are asymmetric particles that contain two different surface properties on their two sides. To prepare Janus particles, a monolayer of silica particles is prepared by a drying process. Gold (Au) is deposited on one side of each particle using a sputtering device. The fully coated metallic particles are completed after the second coating process. To analyze the electrical surface properties of Janus particles, alternating current (AC) electrokinetic measurements, such as dielectrophoresis (DEP) and electrorotation (EROT)- which require specifically designed electrode arrays in the experimental device- are performed. However, traditional methods to fabricate electrode arrays, such as the photolithographic technique, require a series of complicated procedures. Here, we introduce a flexible method to fabricate a designed electrode array. An indium tin oxide (ITO) glass is patterned by a fiber laser marking machine (1,064 nm, 20 W, 90 to 120 ns pulse-width, and 20 to 80 kHz pulse repetition frequency) to create a four-phase electrode array. To generate the four-phase electric field, the electrodes are connected to a 2-channel function generator and to two invertors. The phase shift between the adjacent electrodes is set at either 90&#176; (for EROT) or 180&#176; (for DEP). Representative results of AC electrokinetic measurements with a four-phase ITO electrode array are presented.

The four-phase electrode array is created by a fiber laser marking machine. The ITO conductive layer coated on the glass is removed by a focus laser to form a cross pattern with a gap of 160 &#181;m, as shown in Figure 1B.
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/55950/55950fig1.jpg" /> 
Figure 1: Preparation of the ITO El...

Watch this Scientific Journal Video about Preparation of Janus Particles and Alternating Current Electrokinetic Measurements with a Rapidly Fabricated Indium Tin Oxide Electrode Array at JoVE.com

Preparation of Janus Particles and Alternating Current Electrokinetic Measurements with a Rapidly Fabricated Indium Tin Oxide Electrode Array

In this article, a simple method to prepare partially or fully coated metallic particles and to perform AC electrokinetic property measurements with a rapidly fabricated indium tin oxide (ITO) electrode array is demonstrated.

This article provides a simple method to prepare partially or fully coated metallic particles and to perform the rapid fabrication of electrode arrays, ...

The overall goal of this procedure is to rapidly fabricate indium tin oxide electrodes and prepare metal-coated particles for electrokinetic experiments. This method can facilitate experiment in electrokinetics field, such as electrorotation, dielectrophoresis, and microfluidics. The main advantage of this technique is that it provides a rapid and convenient method to fabricate ITO electrode and prepare metal coat particles.To begin fabricating the electrode, place a clean piece of 25 millimeter by 50 millimeter ITO-coated glass on the stage of a pulsed fiber laser engraving machine. Position the laser 279.5 millimeters above the ITO glass. Import the electrode pattern into the instrument control software.Select Frame, Fill, and Fill First. Set the engraving speed to 800 millimeters per second, the laser power to 60%and the frequency to 40 kilohertz. Preview the engraving pattern, and manually adjust the glass position to center the pattern on the glass.Once the pattern is centered, perform the engraving to divide the conductive surface into quadrants. Use polyimide tape to affix an insulated stranded wire to each conductive quadrant of the engraved ITO glass. Then, split each channel output of a two-function generator with double BNC connectors.Equip one output of each channel with an inverting operational amplifier. To prepare an electrode array for electrorotation measurements, first connect the upper left electrode directly to the double BNC connector of the first channel. Connect the corresponding inverter output to the non-adjacent electrode.Then, connect the lower left electrode to the second channel. Connect the corresponding inverter output to the last wire to produce an electrode array with a 90 degree phase shift between adjacent electrodes. To prepare an electrode array for dielectrophoresis, instead connect the inverted first channel to the lower left electrode.Connect the lower right electrode to the second channel. Connect the last electrode to the corresponding inverter output to produce an array with a 180 degree phase shift between adjacent electrodes. To begin preparing the Janus particles, centrifuge a 10%by weight aqueous suspension of two micrometer silica particles at 2, 200 times g for one minute.Transfer two microliters of the resulting sedimentary silica particles to a 1.5 milliliter microcentrifuge tube. Add 500 microliters of 99.5%ethanol to the silica particles. Sonicate the suspension for one minute, and then centrifuge the suspension at 2, 200 times g for three minutes.Decant the supernatant, and add another 500 microliters of ethanol to the sample. Repeat the sonication and centrifugation three more times, refreshing the ethanol each time. Then, decant the supernatant and add eight microliters of ethanol to the sample.Sonicate the sample for three minutes. Pipette two microliters of the resulting suspension onto a glass slide. Use a cover slide to slowly spread the droplet over the slide to form a monolayer of silica particles.Once the solvent has evaporated, place the slide in a sputter coater with a gold target. Sputter coat the slide at 15 milliamps for 200 seconds to prepare the Janus particles. Apply 20 microliters of deionized water to the slide.Carefully dislodge the Janus particles with a 200 microliter pipette tip so that the particles are suspended in the water droplet. Then, transfer the Janus particle suspension to a 1.5 milliliter microcentrifuge tube. Dilute the suspension with deionized water as needed to achieve a suitable Janus particle concentration for the experiment.To begin preparing fully-coated metallic particles, mix together a polydimethylsiloxane polymer base and its curing agent in a 10 to one weight ratio. Apply tape to the edges of a glass slide to form a container. Pour the PDMS mixture into the tape-walled container to a depth of two to three millimeters.Degas the PDMS under vacuum for 30 minutes, and cure the PDMS at 70 degrees Celsius for two hours. Then, separate the cured PDMS from the tape and the slide to obtain a smooth PDMS stamp. Prepare a monolayer of Janus particles on a glass slide.Then, lay the PDMS stamp smooth side down on the slide and apply even pressure to transfer the Janus particles to the stamp. Carefully separate the slide from the PDMS stamp to expose the silica faces of the Janus particles. Sputter coat the particles on the PDMS stamp with another thin layer of gold to obtain the fully-coated particles.Use a droplet of deionized water and a pipette tip to dislodge the particles from the stamp surface to be suspended in the droplet. Transfer the suspension to a microcentrifuge tube, and dilute the suspension as needed. To begin the experiment, cover the ITO four-phase electrode array with five sheets of paraffin laboratory film.Use a heat gun to fix the paraffin layers to the electrode array, forming a 500 micrometer spacer. Then, place the electrode array on the stage of an inverted microscope with a 40X 0.6 NA objective lens. Place eight microliters of a particle suspension at the center of the array, and cover it with a cover glass.Set the function generator phase shift to 90 degrees for an electrorotation experiment or zero degrees for a dielectrophoresis experiment. Select a sine wave as the waveform, and set the peak-to-peak voltage and frequency. Start the signal generator, and use the inverted microscope camera to capture images of particle motion and rotation.Use image processing software to determine the particle velocities for further analysis. Alternating current electrokinetic property measurements were performed on silica particles with varying degrees of gold coating. Janus particles were found to rotate in the same direction as the electric field at low frequencies and counter-field at higher frequencies.The maximum angular speed was observed at a characteristic frequency. Electrorotation measurements of bare silica particles showed co-field rotation at all measured frequencies. The maximum angular speed was observed at the lowest measured frequency.In contrast, gold-coated silica particles showed counter-field rotation at all measured frequencies. The maximum angular speed for the gold-coated particles was observed at a lower characteristic frequency than in the Janus particles. These results, overall, suggested that the Janus particle behavior could not be attributed to a simple, two-hemisphere superposition model.Dielectrophoresis measurements of the fully gold-coated particles showed an N-dielectrophoresis response at low frequencies and a P-dielectrophoresis response at high frequencies. The crossover frequency closely matched the characteristic frequency at which the maximum angular speed had been observed. After its development, these techniques paved the way for the researchers in the field of soft matter to explore electrode canopy for laminar in microfluidic synthesis.After watching this video, you should have a good understanding of how to fabricate ITO electrode with a laser marking machine and prepare metal coat particle for electrokinetic experiments.

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Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

We present a unique platform for characterizing electrode surfaces in solid oxide fuel cells (SOFCs) that allows simultaneous performance of multiple characterization techniques (e.g. in situ Raman spectroscopy and scanning probe microscopy alongside electrochemical measurements). Complementary information from these analyses may help to advance toward a more profound understanding of electrode reaction and degradation mechanisms, providing insights into rational design of better materials for SOFCs.

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

Development of a 3D Graphene Electrode Dielectrophoretic Device

The design and fabrication of a novel 3D electrode microdevice using 50 &#181;m thick graphene paper and 100 &#181;m double sided tape is described. The protocol details the procedures to construct a versatile, reusable, multiple layer, laminated dielectrophoresis chamber. Specifically, six layers of 50 &#181;m x&#160;0.7 cm x&#160;2 cm graphene paper and five layers of double sided tape were alternately stacked together, then clamped to a glass slide. Then a 700 &#956;m diameter micro-well was drilled through the laminated structure using a computer-controlled micro drilling machine. Insulating properties of the tape layer between adjacent graphene layers were assured by resistance tests. Silver conductive epoxy connected alternate layers of graphene paper and formed stable connections between the graphene paper and external copper wire electrodes. The finished device was then clamped and sealed to a glass slide. The electric field gradient was modeled within the multi-layer device. Dielectrophoretic behaviors of 6 &#956;m polystyrene beads were demonstrated in the 1 mm deep micro-well, with medium conductivities ranging from 0.0001 S/m to 1.3 S/m, and applied signal frequencies from 100 Hz to 10 MHz. Negative dielectrophoretic responses were observed in three dimensions over most of the conductivity-frequency space and cross-over frequency values are consistent with previously reported literature values. The device did not prevent AC electroosmosis and electrothermal flows, which occurred in the low and high frequency regions, respectively. The graphene paper utilized in this device is versatile and could subsequently function as a biosensor after dielectrophoretic characterizations are complete.

A microdevice with high throughput potential is used to demonstrate three-dimensional (3D) dielectrophoresis (DEP) with novel materials. Graphene nanoplatelet paper and double sided tape were alternately stacked; a 700 &#956;m micro-well was drilled transverse to the layers. DEP behavior of polystyrene beads was demonstrated in the micro-well.

The design and fabrication of a novel 3D electrode microdevice using 50 &#181;m thick graphene paper and 100 &#181;m double sided tape is described. The ...

Writing and Low-Temperature Characterization of Oxide Nanostructures

Oxide nanoelectronics is a rapidly growing field which seeks to develop novel materials with multifunctional behavior at nanoscale dimensions. Oxide interfaces exhibit a wide range of properties that can be controlled include conduction, piezoelectric behavior, ferromagnetism, superconductivity and nonlinear optical properties. Recently, methods for controlling these properties at extreme nanoscale dimensions have been discovered and developed. Here are described explicit step-by-step procedures for creating LaAlO3/SrTiO3 nanostructures using a reversible conductive atomic force microscopy technique. The processing steps for creating electrical contacts to the LaAlO3/SrTiO3 interface are first described. Conductive nanostructures are created by applying voltages to a conductive atomic force microscope tip and locally switching the LaAlO3/SrTiO3 interface to a conductive state. A versatile nanolithography toolkit has been developed expressly for the purpose of controlling the atomic force microscope (AFM) tip path and voltage. Then, these nanostructures are placed in a cryostat and transport measurements are performed. The procedures described here should be useful to others wishing to conduct research in oxide nanoelectronics.

Oxide nanostructures provide new opportunities for science and technology. The interfacial conductivity between LaAlO3 and SrTiO3 can be controlled with near-atomic precision using a conductive atomic force microscopy technique. The protocol for creating and measuring conductive nanostructures at LaAlO3/SrTiO3 interfaces is demonstrated.

Oxide nanoelectronics is a rapidly growing field which seeks to develop novel materials with multifunctional behavior at nanoscale dimensions.  Oxide ...

Preparation and Friction Force Microscopy Measurements of Immiscible, Opposing Polymer Brushes

Solvated polymer brushes are well known to lubricate high-pressure contacts, because they can sustain a positive normal load while maintaining low friction at the interface. Nevertheless, these systems can be sensitive to wear due to interdigitation of the opposing brushes. In a recent publication, we have shown via molecular dynamics simulations and atomic force microscopy experiments, that using an immiscible polymer brush system terminating the substrate and the slider surfaces, respectively, can eliminate such interdigitation. As a consequence, wear in the contacts is reduced. Moreover, the friction force is two orders of magnitude lower compared to traditional miscible polymer brush systems. This newly proposed system therefore holds great potential for application in industry. Here, the methodology to construct an immiscible polymer brush system of two different brushes each solvated by their own preferred solvent is presented. The procedure how to graft poly(N-isopropylacrylamide) (PNIPAM) from a flat surface and poly(methyl methacrylate) (PMMA) from an atomic force microscopy (AFM) colloidal probe is described. PNIPAM is solvated in water and PMMA in acetophenone. Via friction force AFM measurements, it is shown that the friction for this system is indeed reduced by two orders of magnitude compared to the miscible system of PMMA on PMMA solvated in acetophenone.

The methodology to perform friction force microscopy experiments for contacting brushes is presented: Two polymer brushes that are grafted from (a) substrates and (b) colloidal probes are slid to show that, by using two contacting immiscible brush systems, friction in sliding contacts is reduced compared to miscible brush systems.

Solvated polymer brushes are well known to lubricate high-pressure contacts, because they can sustain a positive normal load while maintaining low ...

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 ...

Surface Enhanced Raman Spectroscopy Detection of Biomolecules Using EBL Fabricated Nanostructured Substrates

Fabrication and characterization of conjugate nano-biological systems interfacing metallic nanostructures on solid supports with immobilized biomolecules is reported. The entire sequence of relevant experimental steps is described, involving the fabrication of nanostructured substrates using electron beam lithography, immobilization of biomolecules on the substrates, and their characterization utilizing surface-enhanced Raman spectroscopy (SERS). Three different designs of nano-biological systems are employed, including protein A, glucose binding protein, and a dopamine binding DNA aptamer. In the latter two cases, the binding of respective ligands, D-glucose and dopamine, is also included. The three kinds of biomolecules are immobilized on nanostructured substrates by different methods, and the results of SERS imaging are reported. The capabilities of SERS to detect vibrational modes from surface-immobilized proteins, as well as to capture the protein-ligand and aptamer-ligand binding are demonstrated. The results also illustrate the influence of the surface nanostructure geometry, biomolecules immobilization strategy, Raman activity of the molecules and presence or absence of the ligand binding on the SERS spectra acquired.

We describe the fabrication and characterization of nano-biological systems interfacing nanostructured substrates with immobilized proteins and aptamers. The relevant experimental steps involving lithographic fabrication of nanostructured substrates, bio-functionalization, and surface-enhanced Raman spectroscopy (SERS) characterization, are reported. SERS detection of surface-immobilized proteins, and probing of protein-ligand and aptamer-ligand binding is demonstrated.

Fabrication and characterization of conjugate nano-biological systems interfacing metallic nanostructures on solid supports with immobilized biomolecules ...

Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational analysis. Testing of lithium-ion batteries in an academic setting has taken on several forms, but at the most basic level lies the coin cell construction. In traditional LIB electrode preparation, a multi-phase slurry composed of active material, binder, and conductive additive is cast out onto a substrate. An electrode disc can then be punched from the dried sheet and used in the construction of a coin cell for electrochemical evaluation. Utilization of the potential of the active material in a battery is critically dependent on the microstructure of the electrode, as an appropriate distribution of the primary components are crucial to ensuring optimal electrical conductivity, porosity, and tortuosity, such that electrochemical and transport interaction is optimized. Processing steps ranging from the combination of dry powder, wet mixing, and drying can all critically affect multi-phase interactions that influence the microstructure formation. Electrochemical probing necessitates the construction of electrodes and coin cells with the utmost care and precision. This paper aims at providing a step-by-step guide of non-aqueous electrode processing and coin cell construction for lithium-ion batteries within an academic setting and with emphasis on deciphering the influence of drying and calendaring.

Non-aqueous electrode processing is central to the construction of coin cells and the evaluation of new electrode chemistries for lithium-ion batteries. A step-by-step guide to the basic practices needed as an electrochemical engineer working with batteries in an academic experimental setting is furnished.

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational ...

Methods for Measuring the Orientation and Rotation Rate of 3D-printed Particles in Turbulence

Experimental methods are presented for measuring the rotational and translational motion of anisotropic particles in turbulent fluid flows. 3D printing technology is used to fabricate particles with slender arms connected at a common center. Shapes explored are crosses (two perpendicular rods), jacks (three perpendicular rods), triads (three rods in triangular planar symmetry), and tetrads (four arms in tetrahedral symmetry). Methods for producing on the order of 10,000 fluorescently dyed particles are described. Time-resolved measurements of their orientation and solid-body rotation rate are obtained from four synchronized videos of their motion in a turbulent flow between oscillating grids with R&#955; = 91. In this relatively low-Reynolds number flow, the advected particles are small enough that they approximate ellipsoidal tracer particles. We present results of time-resolved 3D trajectories of position and orientation of the particles as well as measurements of their rotation rates.

We use 3D printing to fabricate anisotropic particles in the shapes of jacks, crosses, tetrads, and triads, whose alignments and rotations in turbulent fluid flow can be measured from multiple simultaneous video images.

Experimental methods are presented for measuring the rotational and translational motion of anisotropic particles in turbulent fluid flows. 3D printing ...

Fabrication and Operation of Acoustofluidic Devices Supporting Bulk Acoustic Standing Waves for Sheathless Focusing of Particles

Acoustophoresis refers to the displacement of suspended objects in response to directional forces from sound energy. Given that the suspended objects must be smaller than the incident wavelength of sound and the width of the fluidic channels are typically tens to hundreds of micrometers across, acoustofluidic devices typically use ultrasonic waves generated from a piezoelectric transducer pulsating at high frequencies (in the megahertz range). At characteristic frequencies that depend on the geometry of the device, it is possible to induce the formation of standing waves that can focus particles along desired fluidic streamlines within a bulk flow. Here, we describe a method for the fabrication of acoustophoretic devices from common materials and clean room equipment. We show representative results for the focusing of particles with positive or negative acoustic contrast factors, which move towards the pressure nodes or antinodes of the standing waves, respectively. These devices offer enormous practical utility for precisely positioning large numbers of microscopic entities (e.g., cells) in stationary or flowing fluids for applications ranging from cytometry to assembly.

Acoustofluidic devices use ultrasonic waves within microfluidic channels to manipulate, concentrate and isolate suspended micro and nanoscopic entities. This protocol describes the fabrication and operation of such a device supporting bulk acoustic standing waves to focus particles in a central streamline without the aid of sheath fluids.

Acoustophoresis refers to the displacement of suspended objects in response to directional forces from sound energy. Given that the suspended objects must ...

Measurements of Soil Carbon by Neutron-Gamma Analysis in Static and Scanning Modes

The herein described application of the inelastic neutron scattering (INS) method for soil carbon analysis is based on the registration and analysis of gamma rays created when neutrons interact with soil elements. The main parts of the INS system are a pulsed neutron generator, NaI(Tl) gamma detectors, split electronics to separate gamma spectra due to INS and thermo-neutron capture (TNC) processes, and software for gamma spectra acquisition and data processing. This method has several advantages over other methods in that it is a non-destructive in situ method that measures the average carbon content in large soil volumes, is negligibly impacted by local sharp changes in soil carbon, and can be used in stationary or scanning modes. The result of the INS method is the carbon content from a site with a footprint of ~2.5 - 3 m2 in the stationary regime, or the average carbon content of the traversed area in the scanning regime. The measurement range of the current INS system is &#62;1.5 carbon weight % (standard deviation &#177; 0.3 w%) in the upper 10 cm soil layer for a 1 hmeasurement.

Here, we present the protocol for in situ measurement of soil carbon using the neutron-gamma technique for single point measurements (static mode) or field averages (scanning mode). We also describe system construction and elaborate data treatment procedures.

The herein described application of the inelastic neutron scattering (INS) method for soil carbon analysis is based on the registration and analysis of ...