This work was supported by the Natural Science and Engineering Research Council of Canada (Discovery Grant No. 122795-2010) and the program of the Canada Research Chair in Quantum Semiconductors (JJD). The help provided by Xiaohuan Xuang, Mohamed Walid Hassen and technical assistance of Sonia Blais of the Universit&#233; de Sherbrooke Centre de caract&#233;risation de mat&#233;riaux (CCM) in collecting XPS data are greatly appreciated. NL acknowledges the Merit Scholarship Program for Foreign Student, Fonds de recherche du Qu&#233;bec - Nature et technologies, for providing a graduate student scholarship.

1. Sample Preparation
<ol>
	<li>Use a diamode scribe to cleave an n-type (P-doped) one-side polished Si wafer (resistivity 3.1~4.8 &#937;.m) which is 3 inch in diameter, 380 &#181;m thick, into samples of 12 mm x 6 mm; clean the samples in OptiClear, acetone and isopropyl alcohol (5 min&#160;for every step).</li>
	<li>Etch samples in a ~0.9% HF solution for 1 &#160;min&#160;to etch away initial oxide; rinse in DI water and&#160;dry in high-purity (99.999%) nitrogen (N2).</li>
	<li>Store prepared samples in N2 bag to curb their &#160;oxidation in&#160;air.</li>
</ol>
2. Irradiate Samples by ArF (&#955;=193 nm) and KrF (&#955;=248 nm) Lasers.
<ol>
	<li>Place samples in a 0.74 mm tall chamber and then seal the chamber with a fused silica window that has high transmission in UV (&#8805;90%). Fill&#160;the chamber with H2O2/H2O solution in the range of 0.01-0.2 % or with degassed methanol using a microfluidic channel.</li>
	<li>Irradiate samples with homogenized ArF or KrF lasers at demagnification of 2.6 and 1.8, respectively. Irradiate&#160;only &#160;2&#160;sites on each sample by increasing laser pulses from 100 to 600 in step of 100 pulses &#160;through&#160;a circular mask (4 mm&#160;in&#160;diameter). Irradiate the samples in the same way with a &#8220;maple leaf&#8221;&#160;(9 mm x 7.2 mm) mask.</li>
	<li>Rinse samples in DI water, &#160;dry with N2 flush; place&#160;the samples in a sealed container, then quickly fill this container with N2, in order to avoid exposure to air prior to further experiments.</li>
</ol>
3. Immobilization of Bio-conjugated Nanospheres
<ol>
	<li>Dilute biotin-conjugated and fluorescein stained 40-nm-diameter nanospheres in a pH 7.4 phosphate buffered saline (PBS, 1X) solution to 1012 particles/ml&#160;at RT (~25 &#176;C). Immerse ArF or KrF laser irradiated samples for 2 &#160;hr&#160;in this solution at RT.</li>
	<li>Wash samples with PBS to eliminate physically bound fluorescein stained nanospheres on the surface.</li>
</ol>
4. Surface Characterization
<ol>
	<li>Contact angle (CA) measurement
	<ol>
		<li>Carry out static CA measurements with a goniometer in an environment of RT and ambient humidity.</li>
		<li>Employ high purity DI water (resistivity 17.95 M&#8486;&#183;cm) in a micro-syringe; generate similar volume (~5 &#181;l) drops on the sample surface by lowering the micro-syringe to a similar height for every measurement.</li>
		<li>Capture and save the water drops profile images by CCD camera with software. Measure independently 4 different sites with same irradiation conditions.</li>
		<li>Estimate and average&#160;the CA values in drop analysis module from ImageJ software; load the image and change it into grayscale; launch the plugin Dropsnake; place roughly a few knots on the drop contour (~10 knots) from left to right to initialize snake; accept the curve connecting these knots and evolve the curve by pressing snake button. Note: contact angles are displayed in the image and the table.</li>
	</ol>
	</li>
	<li>XPS measurement
	<ol>
		<li>Investigate surface chemical modification with a XPS spectrometer(1x10-9 Torr base pressure) outfitted with an Al K&#945; source working at 150 W:
		<ol>
			<li>Load the samples into the vacuum chamber.</li>
			<li>Acquire&#160;the surface survey data in constant energy modes of 50 eV pass energy from an area of 220 &#181;m x 220 &#181;m.</li>
			<li>Acquire high resolution scans data from the same analyzed area at 20 eV pass energy.</li>
		</ol>
		</li>
		<li>Process XPS spectra data with XPS spectra quantification software, as referenced25,26.</li>
	</ol>
	</li>
	<li>Fluorescence microscope imaging
	<ol>
		<li>Excite samples, which were irradiated through &#8220;maple leaf&#8221; mask and exposed to fluorescein stained nanospheres, using a blue light source (&#955;=450~490 nm).</li>
		<li>Observe fluorescent images, emitting at 515 nm, with a fluorescence inverted microscope in magnification of 4X.</li>
		<li>Characterize the surface morphology of these samples with AFM, as referenced27.</li>
	</ol>
	</li>
</ol>

The authors have nothing to disclose.

We have proposed a protocol of UV laser irradiation of Si wafer in a microfluidic chamber filled with low concentration of H2O2 solution to induce a superhydrophilic Si surface, which is mainly due to the generation of Si-OH. UV laser photolysis of H2O2 was supposed to form negatively charged OH- radicals. Also, UV laser photoelectric effect leads to the formation of a positively charged surface37. Therefore, the interaction of these negative OH-</sup...

The remarkable electronic and chemical properties as well as its high mechanical strength have made silicon (Si) an ideal choice for microelectronic devices and biomedical chips1. Selective area control of the Si surface has received significant attention for applications involving microfluidic and lab-on-chip devices2,3.This is often obtained either by nano-scale modification of the surface roughness or by chemical treatment of the surface4. The surface roughening or patterning to produce disordered or ordered surface structures on the Si surface include photolithography5, ion beam lithography6 and laser techniques7. Compared with these methods,&#160;laser surface texturing process is reported to be less complicated with the potential to produce microstructures with high spatial resolution8. However, as Si has an elevated texturing threshold, requiring irradiation with pulse fluence to induce surface texturing in excess of its ablation threshold (~500 mJ/cm2)9, texturing of Si surface has frequently been assisted by employing reactive gas atmospheres, such as that of a high pressure SF6 environment4,7,8. Consequently, to modify wettability of the Si surface, numerous works have focused on chemical treatment by depositing organic10 and inorganic films2, or using plasma or electron beam surface treatment11,12. It is recognized that hydrophilicity of Si originating from the existence of singular and associated OH groups on its surface could be achieved by boiling it in a H2O2 solution at 100 &#176;C for several minutes13. However, the hydrophobic Si surface states, most of which are due to the presence of Si-H or Si-O-CH3 groups, could be achieved by wet chemical handling involving etching with&#160;HF acid solution or coating with photoresist13-15. To achieve selective area control of wettability of Si, complex patterning steps are usually required, including treatment in chemical solutions16. The high chemical reactivity of UV laser radiation has also been used to selective area process organic film coated solid substrates and modify their wettability17. However, a limited amount of data is available on laser-assisted modification of Si wettability by irradiation of samples immersed in different chemical solutions.
In our previous research, UV laser irradiation of III-V semiconductors in air18-20 and NH321 was successfully used to alter the surface chemical composition of GaAs, InGaAs and InP. We established that UV laser irradiation of III-V semiconductors&#160;in deionized (DI) water decreases surface oxides and carbides, while the water adsorbed on semiconductor surface increases22. A strongly hydrophobic Si surface (CA~103&#176;) was obtained by ArF laser irradiation of Si samples in methanol in our recent work 23. As indicated by X-ray photoelectron spectroscopy (XPS), this is&#160;primarily&#160;due to the&#160;ability&#160;of the ArF laser to photodissociate CH3OH. We have also used KrF and ArF lasers to irradiate Si (001) in a 0.01% of H2O2 in DI water. This allowed us to achieve selective area formation of superhydrophilic surface of Si (001) characterized by the CA of near 15&#176;. The XPS results suggest that this is due to generation of Si-OH bonds on the irradiated surface24.
A detailed description of this new technique using KrF and ArF lasers for selective area in situ modification of the hydrophilic/hydrophobic surface of Si surface in low concentration of H2O2/H2O and methanol solutions is demonstrated in this article. The details provided here should be sufficient to allow similar experiments to be performed by interested researchers.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>fluorescein stained nanospheres</td>
			<td>Invitrogen</td>
			<td>F8795</td>
			<td></td>
		</tr>
		<tr>
			<td>OptiClear</td>
			<td>National Diagnostics</td>
			<td>OE-101</td>
			<td></td>
		</tr>
		<tr>
			<td>ArF laser (&#955;=193 nm)</td>
			<td>Lumonics</td>
			<td>pulse master 800</td>
			<td></td>
		</tr>
		<tr>
			<td>KrF laser (&#955;=248 nm)</td>
			<td>Lumonics</td>
			<td>pulse master 800</td>
			<td></td>
		</tr>
		<tr>
			<td>XPS</td>
			<td>Kratos Analytical</td>
			<td>AXIS Ultra DLD</td>
			<td></td>
		</tr>
		<tr>
			<td>Fluorescence microscope</td>
			<td>Olympus</td>
			<td>IX71</td>
			<td></td>
		</tr>
		<tr>
			<td>XPS quantitification software</td>
			<td>CasaXPS</td>
			<td>2.3.15</td>
			<td></td>
		</tr>
	</tbody>
</table>

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.

These representative results have been presented in our previous published work23,24. Figure 1 shows the CA vs. N (number of pulses) on sites irradiated by KrF laser at 250 mJ/cm2 in DI H2O for different concentrations of H2O2/H2O solutions (e.g., 0.01, 0.02, 0.05 and 0.2%).&#160;The CA decreases with increasing pulse number for all the H2O2 solutions. The minimum CA (~15&#176;) for the 0.02 and 0.01% H2...

Watch this Scientific Journal Video about Selective Area Modification of Silicon Surface Wettability by Pulsed UV Laser Irradiation in Liquid Environment at JoVE.com

Selective Area Modification of Silicon Surface Wettability by Pulsed UV Laser Irradiation in Liquid Environment

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 ...

selective-area-modification-silicon-surface-wettability-pulsed-uv

Research

JoVE Journal

Engineering

8.2K 조회수.  Université de Sherbrooke.  우리는 HF의 시츄 변경이 2 O 2 / H 2 O 용액 (0.01 % -0.5 %) 또는 메탄올 용액 H로 채워진 미세 유체 챔버에서 샘플을 조사함으로써 친수성 또는 소수성 상태의 Si (001) 표면 처리에서의 공정보고 상대적으로 낮은 펄스 UV 플루 언스의 레이저 펄스를 사용. 

비디오: Selective Area Modification of Silicon Surface Wettability by Pulsed UV Laser Irradiation in Liquid Environment

Characterization of Surface Modifications by White Light Interferometry: Applications in Ion Sputtering, Laser Ablation, and Tribology Experiments

In materials science and engineering it is often necessary to obtain quantitative measurements of surface topography with micrometer lateral resolution. From the measured surface, 3D topographic maps can be subsequently analyzed using a variety of software packages to extract the information that is needed.
In this article we describe how white light interferometry, and optical profilometry (OP) in general, combined with generic surface analysis software, can be used for materials science and engineering tasks. In this article, a number of applications of white light interferometry for investigation of surface modifications in mass spectrometry, and wear phenomena in tribology and lubrication are demonstrated. We characterize the products of the interaction of semiconductors and metals with energetic ions (sputtering), and laser irradiation (ablation), as well as ex situ measurements of wear of tribological test specimens.
Specifically, we will discuss:
<ol class="lroman">
	<li>Aspects of traditional ion sputtering-based mass spectrometry such as sputtering rates/yields measurements on Si and Cu and subsequent time-to-depth conversion.</li>
	<li>Results of quantitative characterization of the interaction of femtosecond laser irradiation with a semiconductor surface. These results are important for applications such as ablation mass spectrometry, where the quantities of evaporated material can be studied and controlled via pulse duration and energy per pulse. Thus, by determining the crater geometry one can define depth and lateral resolution versus experimental setup conditions.</li>
	<li>Measurements of surface roughness parameters in two dimensions, and quantitative measurements of the surface wear that occur as a result of friction and wear tests.</li>
</ol>
Some inherent drawbacks, possible artifacts, and uncertainty assessments of the white light interferometry approach will be discussed and explained.

White light microscope interferometry is an optical, noncontact and quick method for measuring the topography of surfaces. It is shown how the method can be applied toward mechanical wear analysis, where wear scars on tribological test samples are analyzed; and in materials science to determine ion beam sputtering or laser ablation volumes and depths.

In materials science and engineering it is often necessary to obtain quantitative measurements of surface topography with micrometer lateral resolution. ...

Fabrication of Nano-engineered Transparent Conducting Oxides by Pulsed Laser Deposition

Nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas allows the deposition of metal oxides with tunable morphology, structure, density and stoichiometry by a proper control of the plasma plume expansion dynamics. Such versatility can be exploited to produce nanostructured films from compact and dense to nanoporous characterized by a hierarchical assembly of nano-sized clusters. In particular we describe the detailed methodology to fabricate two types of Al-doped ZnO (AZO) films as transparent electrodes in photovoltaic devices: 1) at low O2 pressure, compact films with electrical conductivity and optical transparency close to the state of the art transparent conducting oxides (TCO) can be deposited at room temperature, to be compatible with thermally sensitive materials such as polymers used in organic photovoltaics (OPVs); 2) highly light scattering hierarchical structures resembling a forest of nano-trees are produced at higher pressures. Such structures show high Haze factor (&gt;80%) and may be exploited to enhance the light trapping capability. The method here described for AZO films can be applied to other metal oxides relevant for technological applications such as TiO2, Al2O3, WO3 and Ag4O4.

We describe the experimental method to deposit nanostructured oxide thin films by nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas. By using this method Al-doped ZnO (AZO) films, from compact to hierarchically structured as nano-tree forests, can be deposited.

Nanosecond Pulsed  Laser Deposition (PLD) in the presence of a background gas allows the deposition  of metal oxides with tunable morphology, structure, ...

Visualization of High Speed Liquid Jet Impaction on a Moving Surface

Two apparatuses for examining liquid jet impingement on a high-speed moving surface are described: an air cannon device (for examining surface speeds between 0 and 25 m/sec) and a spinning disk device (for examining surface speeds between 15 and 100 m/sec). The air cannon linear traverse is a pneumatic energy-powered system that is designed to accelerate a metal rail surface mounted on top of a wooden projectile. A pressurized cylinder fitted with a solenoid valve rapidly releases pressurized air into the barrel, forcing the projectile down the cannon barrel. The projectile travels beneath a spray nozzle, which impinges a liquid jet onto its metal upper surface, and the projectile then hits a stopping mechanism. A camera records the jet impingement, and a pressure transducer records the spray nozzle backpressure. The spinning disk set-up consists of a steel disk that reaches speeds of 500 to 3,000 rpm via a variable frequency drive (VFD) motor. A spray system similar to that of the air cannon generates a liquid jet that impinges onto the spinning disc, and cameras placed at several optical access points record the jet impingement. Video recordings of jet impingement processes are recorded and examined to determine whether the outcome of impingement is splash, splatter, or deposition. The apparatuses are the first that involve the high speed impingement of low-Reynolds-number liquid jets on high speed moving surfaces. In addition to its rail industry applications, the described technique may be used for technical and industrial purposes such as steelmaking and may be relevant to high-speed 3D printing.

Two experimental devices for examining liquid jet impingement on a high-speed moving surface are described: an air cannon device and a spinning disk device. The apparatuses are used to determine optimal approaches to the application of liquid friction modifier (LFM) onto rail tracks for top-of-rail friction control.

Two apparatuses for examining liquid jet impingement on a high-speed moving surface are described: an air cannon device (for examining surface speeds ...

Integration of Light Trapping Silver Nanostructures in Hydrogenated Microcrystalline Silicon Solar Cells by Transfer Printing

One of the potential applications of metal nanostructures is light trapping in solar cells, where unique optical properties of nanosized metals, commonly known as plasmonic effects, play an important role. Research in this field has, however, been impeded owing to the difficulty of fabricating devices containing the desired functional metal nanostructures. In order to provide a viable strategy to this issue, we herein show a transfer printing-based approach that allows the quick and low-cost integration of designed metal nanostructures with a variety of device architectures, including solar cells. Nanopillar poly(dimethylsiloxane) (PDMS) stamps were fabricated from a commercially available nanohole plastic film as a master mold. On this nanopatterned PDMS stamps, Ag films were deposited, which were then transfer-printed onto block copolymer (binding layer)-coated hydrogenated microcrystalline Si (&#181;c-Si:H) surface to afford ordered Ag nanodisk structures. It was confirmed that the resulting Ag nanodisk-incorporated &#181;c-Si:H solar cells show higher performances compared to a cell without the transfer-printed Ag nanodisks, thanks to plasmonic light trapping effect derived from the Ag nanodisks. Because of the simplicity and versatility, further device application would also be feasible thorough this approach.

A viable transfer printing-based methodology to introduce plasmonic metal nanostructures in solar cells is described. Using nanopillar poly(dimethylsiloxane) stamps, an Ag-based ordered nanodisk array was integrated with standard hydrogenated microcrystalline Si solar cells, which led to improved device performances due to plasmonic light trapping.

One of the potential applications of metal nanostructures is light trapping in solar cells, where unique optical properties of nanosized metals, commonly ...

Automation of Mode Locking in a Nonlinear Polarization Rotation Fiber Laser through Output Polarization Measurements

When a laser is mode-locked, it emits a train of ultra-short pulses at a repetition rate determined by the laser cavity length. This article outlines a new and inexpensive procedure to force mode locking in a pre-adjusted nonlinear polarization rotation fiber laser. This procedure is based on the detection of a sudden change in the output polarization state when mode locking occurs. This change is used to command the alignment of the intra-cavity polarization controller in order to find mode-locking conditions. More specifically, the value of the first Stokes parameter varies when the angle of the polarization controller is swept and, moreover, it undergoes an abrupt variation when the laser enters the mode-locked state. Monitoring this abrupt variation provides a practical easy-to-detect signal that can be used to command the alignment of the polarization controller and drive the laser towards mode locking. This monitoring is achieved by feeding a small portion of the signal to a polarization analyzer measuring the first Stokes parameter. A sudden change in the read out of this parameter from the analyzer will occur when the laser enters the mode-locked state. At this moment, the required angle of the polarization controller is kept fixed. The alignment is completed. This procedure provides an alternate way to existing automating procedures that use equipment such as an optical spectrum analyzer, an RF spectrum analyzer, a photodiode connected to an electronic pulse-counter or a nonlinear detecting scheme based on two-photon absorption or second harmonic generation. It is suitable for lasers mode locked by nonlinear polarization rotation. It is relatively easy to implement, it requires inexpensive means, especially at a wavelength of 1550 nm, and it lowers the production and operation costs incurred in comparison to the above-mentioned techniques.

A protocol to detect and automate mode locking in a pre-adjusted nonlinear polarization rotation fiber laser is presented. The detection of a sudden change in the output polarization state when mode locking occurs is used to command the alignment of an intra-cavity polarization controller in order to find mode-locking conditions.

When a laser is mode-locked, it emits a train of ultra-short pulses at a repetition rate determined by the laser cavity length. This article outlines a ...

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 ...

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m2&#183;g-1. An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia YSZ Scaffolds by In Situ Carbon Templating Xerogels

A protocol for fabricating porous, nanostructured yttria-stabilized-zirconia (YSZ) scaffolds at temperatures between 1,000 &#176;C and 1,400 &#176;C is presented.

We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) ...

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

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 ...

Quantitative Analysis of Vacuum Induction Melting by Laser-induced Breakdown Spectroscopy

Vacuum induction melting is a popular method for refining high purity metal and alloys. Traditionally, standard process control in metallurgy involves several steps, include drawing samples, cooling, cutting, transport to the laboratory, and analysis. The whole analysis process requires more than 30 minutes, which hinders on-line process control. Laser-induced breakdown spectroscopy is an excellent on-line analysis method that can satisfy the requirements of vacuum induction melting because it is fast and noncontact and does not require sample preparation. The experimental facility uses a lamp-pumped Q-switched laser to ablate melted liquid steel with an output energy of 80 mJ, a frequency of 5 Hz, a FWHM pulse width of 20 ns, and a working wavelength of 1,064 nm. A multi-channel linear charge coupled device (CCD) spectrometer is used to measure the emission spectrum in real time, with a spectral range from 190 to 600 nm and a resolution of 0.06 nm at a wavelength of 200 nm. The protocol includes several steps: standard alloy sample preparation and an ingredient test, smelting of standard samples and determination of the laser breakdown spectrum, and construction of the elements concentration quantitative analysis curve of each element. To realize the concentration analysis of unknown samples, the spectrum of a sample also needs to be measured and disposed with the same process. The composition of all main elements in the melted alloy can be quantitatively analyzed with an internal standard method. The calibration curve shows that the limit of detection of most metal elements ranges from 20-250 ppm. The concentration of elements, such as Ti, Mo, Nb, V, and Cu, can be lower than 100 ppm, and the concentrations of Cr, Al, Co, Fe, Mn, C, and Si range from 100-200 ppm. The R2 of some calibration curves can exceed 0.94.

During vacuum induction melting, laser-induced breakdown spectroscopy is used to perform real-time quantitative analysis of the main-ingredient elements of a molten alloy.

Vacuum induction melting is a popular method for refining high purity metal and alloys. Traditionally, standard process control in metallurgy involves ...

Impacts of Free-falling Spheres on a Deep Liquid Pool with Altered Fluid and Impactor Surface Conditions

Vertical impacts of spheres on clean water have been the subject of numerous water entry investigations characterizing cavity formation, splash crown ascension and Worthington jet stability. Here, we establish experimental protocols for examining splash dynamics when smooth free-falling spheres of varying wettability, mass, and diameter impact the free surface of a deep liquid pool modified by thin penetrable fabrics and liquid surfactants. Water entry investigations provide accessible, easily assembled and executed experiments for studying complex fluid mechanics. We present herein a tunable protocol for characterizing splash height, flow separation metrics, and impactor kinematics, and representative results which might be acquired if reproducing our approach. The methods are applicable when characteristic splash dimensions remain below approximately 0.5 m. However, this protocol may be adapted for greater impactor release heights and impact velocities, which augurs well for translating results to naval and industry applications.

This protocol demonstrates the basic experimental configuration for water entry experiments with free-falling spheres. Methods for the alteration of liquid surface with penetrable fabrics, the preparation of chemically non-wetting spheres, and steps for splash visualization and data extraction are discussed.

Vertical impacts of spheres on clean water have been the subject of numerous water entry investigations characterizing cavity formation, splash crown ...