The authors are grateful to the University of California and the NANO3 facility at UC San Diego for provision of funds and facilities in support of this work. This work was performed in part at the San Diego Nanotechnology Infrastructure (SDNI) of UCSD, a member of the National Nanotechnology Coordinated Infrastructure, which is supported by the National Science Foundation (Grant ECCS&#8211;1542148). The work presented here was generously supported by a research grant from the W.M. Keck Foundation. The authors are also grateful for the support of this work by the Office of Naval Research (via Grant 12368098).

1. Nano-height channel mask preparation
<ol>
	<li>Photolithography: With a pattern describing the desired shape of the nanoheight channels (Figure 1B), use normal photolithography and lift-off procedures to produce nanoheight depressions in an LN wafer. These depressions will become nanoheight channels upon wafer bonding in a later step. 
	NOTE: The lateral dimensions of the nanoscale depressions are microscale in this protocol. Electron beam or He/Ne ion beam lithography can be used to fabricate channels with nanoscale lateral dimensions; Ga+-based ion beam lithography causes swelling and uneven substrate profiles23. The orientation of the two LN wafers should match, otherwise, thermal stress may cause the wafers or the bond between them to fail.</li>
	<li>Sputter deposition to protect regions from dry etching: Place the wafer into the sputter deposition system. Draw down the chamber vacuum to 5 x 10-6 mTorr, allow Ar to flow at 2.5 mTorr, and sputter Cr at 200 W to produce a 400-nm thick sacrificial mask where reactive ion etching will be prevented when used in step 3 below.</li>
	<li>Lift-off: Transfer the wafer into a beaker with sufficient acetone to completely immerse the wafer. Sonicate at medium intensity for 10 min. Rinse with DI water and dry the wafer with dry N2 flow.</li>
	<li>Dicing: Use a dicing saw to dice the entire wafer into individual chips with (typically) one nanoslit pattern per chip. 
	NOTE: The protocol can be paused here.</li>
</ol>
2. Nano-height channel fabrication
<ol>
	<li>Reactive ion etching (RIE): Use RIE to etch nanoscale depressions into the uncovered regions of the LN substrate. Regions left covered by sacrificial Cr will be protected from etching. Set the RIE power to 200W, heat the chamber to 50 &#176;C, draw down the chamber vacuum to 20 mTorr, set the SF6 flow rate to 10 sccm, and etch for 20 min to produce a 120-nm deep nanoslit in LN.</li>
	<li>Hole drilling for channel inlets and outlets: With double-sided tape, attach an etched LN chip to a small steel plate and the plate to the bottom of a petri dish. The Petri dish should be large enough to permit complete immersion of the LN chip and steel plate. Fill the Petri dish with water to fully immerse the chip. Attach a 0.5-mm diameter diamond drill bit to a drill press, and drill at a high speed of at least 10,000 rpm to machine the desired inlets and outlets. Drilling through a 0.5 mm thick substrate should take about 10 to 15 s24 (Figure 1B). 
	NOTE: Immersion while drilling prevents excessive local heating and particulate jamming at the drill site. Other types of drill bits are unlikely to work, and hand drilling is not possible at any speed to our knowledge. Drill bit rotation speeds of 10,000 rpm or greater are recommended to avoid shattering the LN.</li>
	<li>Cr wet etching: Use a diamond tip engraving pen to clearly mark the flat, unetched face of the drilled LN to keep track of which side the nanoheight channel is located in the remaining steps. Sonicate the chips in Cr etchant. 
	NOTE: The protocol can be paused here. It is exceedingly difficult to determine which side of the LN chip has the etched nanoscale depression after the Cr is removed. The sonication time depends upon the etching rate and the Cr mask thickness.</li>
</ol>
3. Room-temperature Plasma Activated Bonding
<ol>
	<li>Solvent cleaning LN chips: Collect chip pairs&#8212;one SAW device (fabricated by normal photolithography, sputter deposition, and lift-off procedures) and one etched nanoscale depression chip&#8212;together to prepare them for bonding. Immerse the chip pairs in a beaker of acetone placed in a sonication bath and sonicate for 2 min. Transfer the chips to methanol and sonicate for 1 min. Transfer the chips to DI water.</li>
	<li>Piranha cleaning: Prepare piranha acid in a glass beaker in a well-ventilated hood, dedicated to the use of acid, by adding H2O2 (30% in water) to H2SO4 (96%) at a ratio of 1:3. Place all chips in a Teflon holder. Place the holder in the beaker and immerse all chips into the piranha solution for 10 min, then rinse the chips and holder sequentially in two separate DI water baths. Dry the chips with dry N2 and immediately transfer them into oxygen (O2) plasma activation equipment, keeping them covered during handling to avoid contamination. 
	CAUTION: Piranha solutions are highly corrosive, are strongly oxidizing, and are dangerous. Follow the specific rules handling them at your institution, but at least take extreme care and wear the proper safety equipment. Upon completion of the work, the piranha solution must be cooled for at least one hour before pouring into a dedicated waste container. 
	NOTE: It is necessary to rinse the LN chips twice in two DI water baths. Rinsing them once leaves residue behind that will likely ruin the bonding. Gold electrodes are used for IDTs because of their good resistance to piranha solution.</li>
	<li>Plasma surface activation: Activate the chip surfaces using plasma with 120 W of power while exposed to O2 flow at 120 sccm for 150 s. Immediately transfer the samples to a fresh DI water bath for at least 2 min. 
	NOTE: Plasma surface treatment quickly followed by DI water immersion will form hydroxyl groups upon the LN surface, increasing its free surface energy to later promote bonding.</li>
	<li>Room-temperature bonding: Dry the samples with dry N2 flow and carefully lay the nanoslit chip onto the SAW device chip in the desired position. Realign to produce the desired orientation. Then use tweezers or similar to push down upon the sample from its center to initiate the bond. Gently push down in areas that failed to bond after the initial push. 
	NOTE: The bonding may be easily seen through the transparent LN. Bonded regions are entirely transparent. LN that is not double-side polished will be more difficult to assess.</li>
	<li>Heating after bonding: Place bonded samples in a sprung clamp to safely exert loads on it despite thermal expansion, and place the clamped samples into an oven at room temperature (25 &#176;C). Set the oven heating temperature to 300 &#176;C, ramp rate to 2 &#176;C/min maximum, dwell time to 2 h, and then to automatically shut off to allow it and the clamped samples within to naturally cool to room temperature. 
	NOTE: The protocol can be paused here. The bonding between hydroxyl groups produces water at the bond, and heating removes the water to drastically increase the bond strength. Modest clamping forces are sufficient. Attempting to bond two chips of different orientations or materials may cause cracks due to mismatched thermal expansion and consequent stress.</li>
</ol>
4. Experimental setup and testing
<ol>
	<li>Observation: Observe the nanoslit under an inverted microscope. Include and rotate a linear polarizing filter in the optical path to suitably block birefringence-based image doubling in the LN. Use ultrapure DI water via the inlet to observe fluid motion in the completed nanoslit. 
	NOTE: Ultrapure liquid is strongly recommended to prevent clogging, especially after evaporation.</li>
	<li>SAW actuation: Attach absorbers at the ends of the SAW device to prevent reflected acoustic waves. Use a signal generator to apply a sinusoidal electric field to the IDT at its resonance frequency of around 40 MHz. Use an amplifier to amplify the signal. Use an oscilloscope to measure the actual voltage, current, and power applied to the device. Record the fluid motion during SAW actuation within the nanoslit using a camera attached to the microscope.</li>
</ol>

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The authors have nothing to disclose.

Room-temperature bonding is key to fabricating SAW-integrated nanoslit devices. Five aspects need to be considered to ensure successful bonding and sufficient bonding strength.
Time and power for plasma surface activation 
Increasing the plasma power will help increase the surface energy and accordingly increase the bonding strength. But the downside of increasing the power during plasma surface activation is the increase in surface roughness, which may adversely affect t...

Controllable nanoscale fluid transport in nanochannels&#8212;nanofluidics1&#8212;occurs on the same length scales as most biological macromolecules, and is promising for biological analysis and sensing, medical diagnosis, and material processing. Various designs and simulations have been developed in nanofluidics to manipulate fluids and particle suspensions based on temperature gradients2, Coulomb dragging3, surface waves4, static electric fields5,6,7, and thermophoresis8 over the last fifteen years. Recently, SAW has been shown9 to produce nanoscale fluid pumping and draining with sufficient acoustic pressure to overcome the dominance of surface and viscous forces that otherwise prevent effective fluid transport in nanochannels. The key benefit of acoustic streaming is its ability to drive useful flow in nanostructures without concern over the details of the chemistry of the fluid or particle suspension, making devices that utilize this technique immediately useful in biological analysis, sensing, and other physicochemical applications.
Fabrication of SAW-integrated nanofluidic devices requires fabrication of the electrodes&#8212;the interdigital transducer (IDT)&#8212;on a piezoelectric substrate, lithium niobate10, to facilitate generating the SAW. Reactive ion etching (RIE) is used to form a nanoscale depression in a separate LN piece, and LN-LN bonding of the two pieces produces a useful nanochannel. The fabrication process for SAW devices has been presented in many publications, whether using normal or lift-off ultraviolet photolithography alongside metal sputter or evaporation deposition11. For the LN RIE process to etch a channel in a specific shape, the effects on the etch rate and the channel&#39;s final surface roughness from choosing different LN orientations, mask materials, gas flow, and plasma power have been investigated12,13,14,15,16. Plasma surface activation has been used to significantly increase surface energy and hence improve the strength of bonding in oxides such as LN17,18,19,20. It is likewise possible to heterogeneously bond LN with other oxides, such as SiO2 (glass) via a two-step plasma activated bonding method21. Room-temperature LN-LN bonding, in particular, has been investigated using different cleaning and surface activation treatments22.
Here, we describe in detail the process to fabricate 40 MHz SAW-integrated 100-nm height nanochannels, often called nanoslit channels (Figure 1A). Effective fluid capillary filling and fluid draining by SAW actuation demonstrates the validity of both nanoslit fabrication and SAW performance in such a nanoscale channel. Our approach offers a nano-acoustofluidic system enabling investigation of a variety of physical problems and biological applications.

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>Absorber</td>
			<td>Dragon Skin, Smooth-On, Inc., Macungie, PA, USA</td>
			<td>Dragon Skin 10 MEDIUM</td>
			<td></td>
		</tr>
		<tr>
			<td>Amplifier</td>
			<td>Mini-Circuits, Brooklyn, NY, USA</td>
			<td>ZHL&#8211;1&#8211;2W&#8211;S+</td>
			<td></td>
		</tr>
		<tr>
			<td>Camera</td>
			<td>Nikon, Minato, Tokyo, Japan</td>
			<td>D5300</td>
			<td></td>
		</tr>
		<tr>
			<td>Developer</td>
			<td>Futurrex, NJ, USA</td>
			<td>RD6</td>
			<td></td>
		</tr>
		<tr>
			<td>Diamond tip engraving pen</td>
			<td>Malco, Memphis, TN, USA</td>
			<td>Malco A50 USA Made Carbide Tipped Scribe</td>
			<td></td>
		</tr>
		<tr>
			<td>Dicing saw</td>
			<td>Disco, Tokyo, Japan</td>
			<td>Disco Automatic Dicing Saw 3220</td>
			<td></td>
		</tr>
		<tr>
			<td>Heating oven</td>
			<td>Carbolite, Hope Valley, UK</td>
			<td>HTCR 6/28</td>
			<td>High Temperature Clean Room Oven - HTCR</td>
		</tr>
		<tr>
			<td>Hole driller</td>
			<td>Dremel, Mount Prospect, Illinois</td>
			<td>Model #4000</td>
			<td>4000 High Performance Variable Speed Rotary</td>
		</tr>
		<tr>
			<td>Inverted microscope</td>
			<td>Amscope, Irvine, CA, USA</td>
			<td>IN480TC-FL-MF603</td>
			<td></td>
		</tr>
		<tr>
			<td>Lithium niobate substrate</td>
			<td>PMOptics, Burlington, MA, USA</td>
			<td>PWLN-431232</td>
			<td>4&#34; double-side polished 0.5 mm thick 128&#176; Y-rotated cut lithium niobate</td>
		</tr>
		<tr>
			<td>Mask aligner</td>
			<td>Heidelberg Instruments, Heidelberg, Germany</td>
			<td>MLA150</td>
			<td></td>
		</tr>
		<tr>
			<td>Nano3 cleanroom facility</td>
			<td>UCSD, La Jolla, CA, USA</td>
			<td></td>
			<td>Fabrication process is performed in it.</td>
		</tr>
		<tr>
			<td>Negative photoresist</td>
			<td>Futurrex, NJ, USA</td>
			<td>NR9-1500PY</td>
			<td></td>
		</tr>
		<tr>
			<td>Oscilloscope</td>
			<td>Keysight Technologies, Santa Rosa, CA, USA</td>
			<td>InfiniiVision 2000 X-Series</td>
			<td></td>
		</tr>
		<tr>
			<td>Plasma surface activation</td>
			<td>PVA TePla, Corona, CA, USA</td>
			<td>PS100</td>
			<td>Tepla Asher</td>
		</tr>
		<tr>
			<td>Polarizer sheet</td>
			<td>Edmund Optics, Barrington, NJ, USA</td>
			<td>#86-182</td>
			<td></td>
		</tr>
		<tr>
			<td>RIE etcher</td>
			<td>Oxford Instruments, Abingdon, UK</td>
			<td>Plasmalab 100</td>
			<td></td>
		</tr>
		<tr>
			<td>Signal generator</td>
			<td>NF Corporation, Yokohama, Japan</td>
			<td>WF1967 multifunction generator</td>
			<td></td>
		</tr>
		<tr>
			<td>Sputter deposition</td>
			<td>Denton Vacuum, NJ, USA</td>
			<td>Denton 18</td>
			<td>Denton Discovery 18 Sputter System</td>
		</tr>
		<tr>
			<td>Teflon wafer dipper</td>
			<td>ShapeMaster, Ogden, IL, USA</td>
			<td>SM4WD1</td>
			<td>Wafer Dipper 4&#34;</td>
		</tr>
	</tbody>
</table>

fabrication of nanoheight channels incorporating surface acoustic wave actuation via lithium niobate for acoustic nanofluidics

Controlled nanoscale manipulation of fluids is known to be exceptionally difficult due to the dominance of surface and viscous forces. Megahertz-order surface acoustic wave (SAW) devices generate tremendous acceleration on their surface, up to 108 m/s2, in turn responsible for many of the observed effects that have come to define acoustofluidics: acoustic streaming and acoustic radiation forces. These effects have been used for particle, cell, and fluid manipulation at the microscale, although more recently SAW has been used to produce similar phenomena at the nanoscale through an entirely different set of mechanisms. Controllable nanoscale fluid manipulation offers a broad range of opportunities in ultrafast fluid pumping and biomacromolecule dynamics useful for physical and biological applications. Here, we demonstrate nanoscale-height channel fabrication via room-temperature lithium niobate (LN) bonding integrated with a SAW device. We describe the entire experimental process including nano-height channel fabrication via dry etching, plasma-activated bonding on lithium niobate, the appropriate optical setup for subsequent imaging, and SAW actuation. We show representative results for fluid capillary filling and fluid draining in a nanoscale channel induced by SAW. This procedure offers a practical protocol for nanoscale channel fabrication and integration with SAW devices useful to build upon for future nanofluidics applications.

We perform fluid capillary filing and SAW-induced fluid draining in nano-height LN slits after successful fabrication and bonding of SAW integrated nanofluidic devices. Surface acoustic waves are generated by IDTs actuated by an amplified sinusoidal signal at the IDTs&#39; resonance frequency of 40 MHz, and the SAW propagates into the nanoslit via a piezoelectric LN substrate. The behavior of the fluid in the nanoslit interacting with SAW may be observed using an inverted microscope.
We demons...

Watch this Scientific Journal Video about Fabrication of Nanoheight Channels Incorporating Surface Acoustic Wave Actuation via Lithium Niobate for Acoustic Nanofluidics at JoVE.com

Fabrication of Nanoheight Channels Incorporating Surface Acoustic Wave Actuation via Lithium Niobate for Acoustic Nanofluidics

We demonstrate fabrication of nanoheight channels with the integration of surface acoustic wave actuation devices upon lithium niobate for acoustic nanofluidics via liftoff photolithography, nano-depth reactive ion etching, and room-temperature plasma surface-activated multilayer bonding of single-crystal lithium niobate, a process similarly useful for bonding lithium niobate to oxides.

Controlled nanoscale manipulation of fluids is known to be exceptionally difficult due to the dominance of surface and viscous forces. Megahertz-order ...

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5.7K Views.  University of California San Diego. We demonstrate fabrication of nanoheight channels with the integration of surface acoustic wave actuation devices upon lithium niobate for acoustic nanofluidics via liftoff photolithography, nano-depth reactive ion etching, and room-temperature plasma surface-activated multilayer bonding of single-crystal lithium niobate, a process similarly useful for bonding lithium niobate to oxides.

Video: Fabrication of Nanoheight Channels Incorporating Surface Acoustic Wave Actuation via Lithium Niobate for Acoustic Nanofluidics

Synthesis of Phase-shift Nanoemulsions with Narrow Size Distributions for Acoustic Droplet Vaporization and Bubble-enhanced Ultrasound-mediated Ablation

High-intensity focused ultrasound (HIFU) is used clinically to thermally ablate tumors. To enhance localized heating and improve thermal ablation in tumors, lipid-coated perfluorocarbon droplets have been developed which can be vaporized by HIFU. The vasculature in many tumors is abnormally leaky due to their rapid growth, and nanoparticles are able to penetrate the fenestrations and passively accumulate within tumors. Thus, controlling the size of the droplets can result in better accumulation within tumors. In this report, the preparation of stable droplets in a phase-shift nanoemulsion (PSNE) with a narrow size distribution is described. PSNE were synthesized by sonicating a lipid solution in the presence of liquid perfluorocarbon. A narrow size distribution was obtained by extruding the PSNE multiple times using filters with pore sizes of 100 or 200 nm. The size distribution was measured over a 7-day period using dynamic light scattering. Polyacrylamide hydrogels containing PSNE were prepared for in vitro experiments. PSNE droplets in the hydrogels were vaporized with ultrasound and the resulting bubbles enhanced localized heating. Vaporized PSNE enables more rapid heating and also reduces the ultrasound intensity needed for thermal ablation. Thus, PSNE is expected to enhance thermal ablation in tumors, potentially improving therapeutic outcomes of HIFU-mediated thermal ablation treatments.

Phase-shift nanoemulsions (PSNE) can be vaporized using high intensity focused ultrasound to enhance localized heating and improve thermal ablation in tumors. In this report, the preparation of stable PSNE with a narrow size distribution is described. Furthermore, the impact of vaporized PSNE on ultrasound-mediated ablation is demonstrated in tissue-mimicking phantoms.

High-intensity  focused ultrasound (HIFU) is used clinically to thermally ablate tumors. To  enhance localized heating and improve thermal ablation in ...

Solid-state Graft Copolymer Electrolytes for Lithium Battery Applications

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 &deg;C), flammable, and volatile organic electrolytes. These organic based electrolyte systems are viable at ambient temperatures, but require a cooling system to ensure that temperatures do not exceed 80 &deg;C. These cooling systems tend to increase battery costs and can malfunction which can lead to battery malfunction and explosions, thus endangering human life. Increases in petroleum prices lead to a huge demand for safe, electric hybrid vehicles that are more economically viable to operate as oil prices continue to rise. Existing organic based electrolytes used in lithium ion batteries are not applicable to high temperature automotive applications. A safer alternative to organic electrolytes is solid polymer electrolytes. This work will highlight the synthesis for a graft copolymer electrolyte (GCE) poly(oxyethylene) methacrylate (POEM) to a block with a lower glass transition temperature (Tg) poly(oxyethylene) acrylate (POEA). The conduction mechanism has been discussed and it has been demonstrated the relationship between polymer segmental motion and ionic conductivity indeed has a Vogel-Tammann-Fulcher (VTF) dependence. Batteries containing commercially available LP30 organic (LiPF6 in ethylene carbonate (EC):dimethyl carbonate (DMC) at a 1:1 ratio) and GCE were cycled at ambient temperature. It was found that at ambient temperature, the batteries containing GCE showed a greater overpotential when compared to LP30 electrolyte. However at temperatures greater than 60 &deg;C, the GCE cell exhibited much lower overpotential due to fast polymer electrolyte conductivity and nearly the full theoretical specific capacity of 170 mAh/g was accessed.

Lithium ion batteries employ flammable and volatile organic electrolytes that are suitable for ambient temperature applications. A safer alternative to organic electrolytes are solid polymer batteries. Solid polymer batteries operate safely at high temperatures (&gt;120 &deg;C), thus making them applicable to high temperature applications such as deep oil drilling and hybrid electric vehicles. This paper will discuss (a) the polymer synthesis, (b) the polymer conduction mechanism, and (c) provide temperature cycling for both solid polymer and organic electrolytes.

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 ...

Fabrication, Operation and Flow Visualization in Surface-acoustic-wave-driven Acoustic-counterflow Microfluidics

Surface acoustic waves (SAWs) can be used to drive liquids in portable microfluidic chips via the acoustic counterflow phenomenon. In this video we present the fabrication protocol for a multilayered SAW acoustic counterflow device. The device is fabricated starting from a lithium niobate (LN) substrate onto which two interdigital transducers (IDTs) and appropriate markers are patterned. A polydimethylsiloxane (PDMS) channel cast on an SU8 master mold is finally bonded on the patterned substrate. Following the fabrication procedure, we show the techniques that allow the characterization and operation of the acoustic counterflow device in order to pump fluids through the PDMS channel grid. We finally present the procedure to visualize liquid flow in the channels. The protocol is used to show on-chip fluid pumping under different flow regimes such as laminar flow and more complicated dynamics characterized by vortices and particle accumulation domains.

In this video we first describe fabrication and operation procedures of a surface acoustic wave (SAW) acoustic counterflow device. We then demonstrate an experimental setup that allows for both qualitative flow visualization and quantitative analysis of complex flows within the SAW pumping device.

Surface acoustic waves (SAWs) can be used to drive liquids in portable microfluidic chips via the acoustic counterflow phenomenon. In this video we ...

Fabrication of Uniform Nanoscale Cavities via Silicon Direct Wafer Bonding

Measurements of the heat capacity and superfluid fraction of confined 4He have been performed near the lambda transition using lithographically patterned and bonded silicon wafers. Unlike confinements in porous materials often used for these types of experiments3, bonded wafers provide predesigned uniform spaces for confinement. The geometry of each cell is well known, which removes a large source of ambiguity in the interpretation of data.
Exceptionally flat, 5 cm diameter, 375 &#181;m thick Si wafers with about 1 &#181;m variation over the entire wafer can be obtained commercially (from Semiconductor Processing Company, for example). Thermal oxide is grown on the wafers to define the confinement dimension in the z-direction. A pattern is then etched in the oxide using lithographic techniques so as to create a desired enclosure upon bonding. A hole is drilled in one of the wafers (the top) to allow for the introduction of the liquid to be measured. The wafers are cleaned2 in RCA solutions and then put in a microclean chamber where they are rinsed with deionized water4. The wafers are bonded at RT and then annealed at ~1,100 &#176;C. This forms a strong and permanent bond. This process can be used to make uniform enclosures for measuring thermal and hydrodynamic properties of confined liquids from the nanometer to the micrometer scale.

A method for permanently bonding two silicon wafers so as to realize a uniform enclosure is described. This includes wafer preparation, cleaning, RT bonding, and annealing processes. The resulting bonded wafers (cells) have uniformity of enclosure ~1%1,2. The resulting geometry allows for measurements of confined liquids and gasses.

Measurements of the heat capacity and superfluid fraction of confined 4He have been performed near the lambda transition using lithographically patterned ...

Patterning via Optical Saturable Transitions - Fabrication and Characterization

This protocol describes the fabrication and characterization of nanostructures using a novel nanolithographic technique called Patterning via Optical Saturable Transitions (POST). In this technique the chemical properties of organic photochromic molecules that undergo single-photon reactions are exploited, enabling rapid top-down nanopatterning over large areas at low light intensities, thereby, allowing for the circumvention of the far-field diffraction barrier.4 Simple, cost-effective, high throughput and resolution alternatives to nanopatterning are being explored, such as, two-photon polymerization5,6, beam pen lithography (BPL)7, scanning electron beam lithography (SEBL), and focused ion beam (FIB) patterning. However, multi-photon approaches require high light intensities, which limit their potential for high throughput and offer low image contrast. Although, electron and ion beam lithographic processes offer increased resolution, the serial nature of the process is limited to slow writing speeds, which also prevents patterning of features over large areas. Beam-pen lithography is an approach towards parallel near-field optical lithography. However, the gap between the source of the beam and the surface of the photoresist needs to be controlled extremely precisely for good pattern uniformity and this is very challenging to accomplish for large arrays of beams. Patterning via Optical Saturable Transitions (POST) is an alternative optical nanopatterning technique for patterning sub-wavelength features1-3. Since this technique uses single photons instead of electrons, it is extremely fast and does not require high light intensities1-3, opening the door to massive parallelization.

We report that the diffraction limit of conventional optical lithography can be overcome by exploiting the transitions of organic photochromic derivatives induced by their photoisomerization at low light intensities.1-3 This paper outlines our fabrication technique and two locking mechanisms, namely: dissolution of one photoisomer and electrochemical oxidation.

This protocol describes the fabrication and characterization of nanostructures using a novel nanolithographic technique called Patterning via Optical ...

Characterization of Full Set Material Constants and Their Temperature Dependence for Piezoelectric Materials Using Resonant Ultrasound Spectroscopy

During the operation of high power electromechanical devices, a temperature rise is unavoidable due to mechanical and electrical losses, causing the degradation of device performance. In order to evaluate such degradations using computer simulations, full matrix material properties at elevated temperatures are needed as inputs. It is extremely difficult to measure such data for ferroelectric materials due to their strong anisotropic nature and property variation among samples of different geometries. Because the degree of depolarization is boundary condition dependent, data obtained by the IEEE (Institute of Electrical and Electronics Engineers) impedance resonance technique, which requires several samples with drastically different geometries, usually lack self-consistency. The resonant ultrasound spectroscopy (RUS) technique allows the full set material constants to be measured using only one sample, which can eliminate errors caused by sample to sample variation. A detailed RUS procedure is demonstrated here using a lead zirconate titanate (PZT-4) piezoceramic sample. In the example, the complete set of material constants was measured from room temperature to 120 &#176;C. Measured free dielectric constants <img alt="Equation 1" src="/files/ftp_upload/53461/image001.jpg" /> and&#160;<img alt="Equation 2" src="/files/ftp_upload/53461/image002.jpg" /> were compared with calculated ones based on the measured full set data, and piezoelectric constants d15 and d33 were also calculated using different formulas. Excellent agreement was found in the entire range of temperatures, which confirmed the self-consistency of the data set obtained by the RUS.

This protocol describes the procedure of measuring the temperature dependence of the full set material constants of piezoelectric materials using resonant ultrasound spectroscopy (RUS).

During the operation of high power electromechanical devices, a temperature rise is unavoidable due to mechanical and electrical losses, causing the ...

Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution for future high-speed reentry missions. But despite the advancements made since Apollo, heat flux prediction remains an imperfect science and engineers resort to safety factors to determine the TPS thickness. This goes at the expense of embarked payload, hampering, for example, sample return missions. 
Ground testing in plasma wind-tunnels is currently the only affordable possibility for both material qualification and validation of material response codes. The subsonic 1.2MW Inductively Coupled Plasmatron facility at the von Karman Institute for Fluid Dynamics is able to reproduce a wide range of reentry environments. This protocol describes a procedure for the study of the gas/surface interaction on ablative materials in high enthalpy flows and presents sample results of a non-pyrolyzing, ablating carbon fiber precursor. With this publication, the authors envisage the definition of a standard procedure, facilitating comparison with other laboratories and contributing to ongoing efforts to improve heat shield reliability and reduce design uncertainties.
The described core techniques are non-intrusive methods to track the material recession with a high-speed camera along with the chemistry in the reactive boundary layer, probed by emission spectroscopy. Although optical emission spectroscopy is limited to line-of-sight measurements and is further constrained to electronically excited atoms and molecules, its simplicity and broad applicability still make it the technique of choice for analysis of the reactive boundary layer. Recession of the ablating sample further requires that the distance of the measurement location with respect to the surface is known at all times during the experiment. Calibration of the optical system of the applied three spectrometers allowed quantitative comparison. At the fiber scale, results from a post-test microscopy analysis are presented.

Development of new ablative materials and their numerical modeling requires extensive experimental investigation. This protocol describes procedures for material response characterization in plasma flows with the core techniques being non-intrusive methods to track the material recession along with the chemistry in the reactive boundary layer by emission spectroscopy.

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution ...

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

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

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

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

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

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 ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of lithium-ion (Li-ion) batteries. However, a number of setbacks prevent their integration into commercial devices. The main limiting factor is due to nanoscale phenomena occurring at the electrode/electrolyte interfaces, ultimately leading to degradation of battery operation. These key problems are highly challenging to observe and characterize as these batteries contain multiple buried interfaces. One approach for direct observation of interfacial phenomena in thin film batteries is through the fabrication of electrochemically active nanobatteries by a focused ion beam (FIB). As such, a reliable technique to fabricate nanobatteries was developed and demonstrated in recent work. Herein, a detailed protocol with a step-by-step process is presented to enable the reproduction of this nanobattery fabrication process. In particular, this technique was applied to a thin film battery consisting of LiCoO2/LiPON/a-Si, and has further been previously demonstrated by in situ cycling within a transmission electron microscope.

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...