Name: preparation and high-temperature anti-adhesion behavior of a slippery surface on stainless steel
Uploaded: 2018-03-29T12:30:00
Description: Watch this Scientific Journal Video about Preparation and High-temperature Anti-adhesion Behavior of a Slippery Surface on Stainless Steel at JoVE.com

This work was supported by the National Natural Science Foundation of China (Grant No. 51290292) and was also supported by the Academic Excellence Foundation of BUAA for PhD students.

1. Photolithography on Stainless Steel
<ol>
	<li>Design the photomask using a mechanical drawing software and fabricate the design by submitting it to a photomask printer4.</li>
	<li>Wash the stainless steel (316 SS; lengthx width: 4 cm x 4 cm, thickness: 1 mm) by rinsing it in alkaline solutions (50 g/L NaOH and 40 g/L Na2CO3) at room temperature for 15 min to remove oil contaminants.</li>
	<li>Thoroughly clean the stainless steel by performing ultrasonic cleaning in an ul...

<ol>
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This manuscript details protocols for fabricating a slippery surface with high-temperature resistance. The slippery property of our prepared surface was demonstrated by observing the easy-sliding behavior of a water droplet. Then, the anti-wetting of the prepared slippery surface at different high temperatures was investigated by depositing a water droplet on the hot surface. The results show that the prepared slippery surface maintained its slippery property even when it was heated to above 300 &#176;C. We also determin...

Anti-adhesion surfaces at high temperatures for use with liquids and soft tissues have received considerable interest because of their extensive application potential in electrosurgical instruments, engines, pipelines etc.1,2,3,4. Bioinspired surfaces, particularly superhydrophobic surfaces, are considered the ideal choice because of their excellent anti-wetting abilities and self-cleaning properties5. In superhydrophobic surfaces, the anti-wetting ability should be ascribed to the locked air in the surface structure. However, the superhydrophobic state is unstable because it is in the Cassie-Baxter state6,7. Also, at high temperatures, the anti-wetting for liquid droplets can fail because of the wetting state transition from the Cassie-Baxter to the Wenzel state8. This wetting transition is induced by small liquid droplet wetting in the structures, which results in the failure to lock the air in place.
Recently, inspired by the slippery properties of the peritome of the pitcher plant, Nepenthes, Wong et al. reported a concept to construct slippery surfaces by infusing a lubricant into the surface structures9,10,11. Due to capillary force, the structures can firmly hold the lubricant in place, just as in the locked air pocket on superhydrophobic surfaces. Thus, the lubricant and surface structures can form a stable solid/liquid surface. When the lubricant has a preferential affinity for the surface structure, the liquid droplet on the composite surface can slide easily, with only a very low contact angle hysteresis (e.g., ~2&#176;)12. This lubricant layer also enables the surface to have remarkable anti-wetting capabilities13, demonstrating great potential for medical devices14,15. However, previous studies on slippery surfaces mainly focused on the preparation for application at room temperature or low temperatures. There are very few studies on the preparation of slippery surfaces with high-temperature resistance. For example, Zhang et al. showed that the rapid evaporation of lubricant rapidly causes the failure of the slippery property at even slightly high temperatures16.
Slippery surfaces with high-temperature resistance can widen the application potential; for example, they can be used as liquid barriers to decrease soft tissue adhesion to electrosurgical instrument tips. During the surgical operation, severe soft tissue adhesion occurs because of the high temperature of the electrosurgical instrument tips. The soft tissue can be charred, causing it to adhere to the instrument tip, which then tears the soft tissue around the tip17,18,19. The adhered soft tissue on the electrosurgical instrument tip negatively influences the operation and also may induce the failure of hemostasis19,20. These effects significantly harm people&#39;s health and economic interest. Therefore, solving the issue of soft tissue adhesion to electrosurgical instruments is very urgent. In fact, slippery surfaces offer an opportunity to solve this problem.
Here, we present a protocol to fabricate slippery surfaces available at high temperatures. Stainless steel was selected as the surface material because of its high-temperature resistance. The stainless steel was roughened by photolithography-assisted chemical etching. Then, the surface was functionalized with a biocompatible material, saline octadecyltrichlorosilane (OTS)21,22,23,24. A slippery surface was prepared by adding silicone oil. These materials enabled the slippery surface to achieve high-temperature resistance. The anti-wetting property at high temperatures and the anti-adhesion effects on soft tissue were investigated. The results show the potential of using slippery surfaces to solve the anti-adhesion problem at high temperatures.

<table width="614">
	<tbody>
		<tr height="48" style="height:36.0pt">
			<td class="xl17" height="48" style="width:128pt;height:36.0pt" width="171">Stainless steel</td>
			<td class="xl17" style="width:113pt" width="150">Hongtu Corporation</td>
			<td class="xl20" style="width:95pt" width="126">316</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="47" style="height:35.25pt">
			<td class="xl17" height="47" style="width:128pt;height:35.25pt" width="171">Octadecyltrichlorosilane</td>
			<td class="xl17" style="width:113pt" width="150">Huaxia Reagent</td>
			<td class="xl17" style="width:95pt" width="126">112-04-9</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="91" style="height:68.25pt">
			<td class="xl17" height="91" style="width:128pt;height:68.25pt" width="171">Photoresist</td>
			<td class="xl17" style="width:113pt" width="150">Kempur Microelectronic Corporation</td>
			<td class="xl16">317S</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="55" style="height:41.25pt">
			<td class="xl17" height="55" style="width:128pt;height:41.25pt" width="171">Silicone oil</td>
			<td class="xl17" style="width:113pt" width="150">Beijing Chemical Works</td>
			<td class="xl17" style="width:95pt" width="126">350 cst</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="52" style="height:39.0pt">
			<td class="xl16" height="52" style="height:39.0pt">Anhydrous toluene</td>
			<td class="xl17" style="width:113pt" width="150">Beijing Chemical Works</td>
			<td class="xl17" style="width:95pt" width="126">108-88-3</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="56" style="height:42.0pt">
			<td class="xl17" height="56" style="width:128pt;height:42.0pt" width="171">Phosphoric acid (H3PO4)</td>
			<td class="xl17" style="width:113pt" width="150">Tianjin Chemical Corporation</td>
			<td class="xl17" style="width:95pt" width="126">7664-38-2</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="63" style="height:47.25pt">
			<td class="xl17" height="63" style="width:128pt;height:47.25pt" width="171">Hydrochloric acid (HCl)</td>
			<td class="xl17" style="width:113pt" width="150">Tianjin Chemical Corporation</td>
			<td class="xl16">7647-01-0</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="56" style="height:42.0pt">
			<td class="xl16" height="56" style="height:42.0pt">Ferric chloride (FeCl3)</td>
			<td class="xl17" style="width:113pt" width="150">Tianjin Chemical Corporation</td>
			<td class="xl16">7705-08-0</td>
			<td class="xl17" style="width:125pt" width="167">Use as received</td>
		</tr>
		<tr height="54" style="height:40.5pt">
			<td class="xl17" height="54" style="width:128pt;height:40.5pt" width="171">Optical upright microscope</td>
			<td class="xl16">Olympus</td>
			<td class="xl16">BX51</td>
			<td class="xl16"></td>
		</tr>
		<tr height="46" style="height:34.5pt">
			<td class="xl17" height="46" style="width:128pt;height:34.5pt" width="171">Optical stereo microscope</td>
			<td class="xl16">Olympus</td>
			<td class="xl16">SZX16</td>
			<td class="xl16"></td>
		</tr>
		<tr height="50" style="height:37.5pt">
			<td class="xl16" height="50" style="height:37.5pt">High speed camera</td>
			<td class="xl16">Olympus</td>
			<td class="xl16">i-SPEED LT</td>
			<td class="xl16"></td>
		</tr>
		<tr height="52" style="height:39.0pt">
			<td class="xl17" height="52" style="width:128pt;height:39.0pt" width="171">Ultrasonic cleaner</td>
			<td class="xl19" style="width:113pt" width="150">KUNSHAN ULTRASONIC INSTRUMENTS CO. LTD</td>
			<td class="xl16">KQ-500E</td>
			<td></td>
		</tr>
		<tr height="49" style="height:36.75pt">
			<td class="xl17" height="49" style="width:128pt;height:36.75pt" width="171">Dynamometer</td>
			<td class="xl19" style="width:113pt" width="150">Yueqing Handapi Instruments Co. Ltd</td>
			<td class="xl16">HP-5</td>
			<td></td>
		</tr>
		<tr height="64" style="height:48.0pt">
			<td class="xl17" height="64" style="width:128pt;height:48.0pt" width="171">Manipulator</td>
			<td class="xl17" style="width:113pt" width="150">Yueqing Handapi Instruments Co. Ltd</td>
			<td class="xl16">HLD</td>
			<td></td>
		</tr>
		<tr height="62" style="height:46.5pt">
			<td class="xl17" height="62" style="width:128pt;height:46.5pt" width="171">Hot plate</td>
			<td class="xl17" style="width:113pt" width="150">Shenzhen Jingyihuang Corporation</td>
			<td class="xl16">DRB-1</td>
			<td></td>
		</tr>
	</tbody>
</table>

preparation and high-temperature anti-adhesion behavior of a slippery surface on stainless steel

Anti-adhesion surfaces with high-temperature resistance have a wide application potential in electrosurgical instruments, engines, and pipelines. A typical anti-wetting superhydrophobic surface easily fails when exposed to a high-temperature liquid. Recently, Nepenthes-inspired slippery surfaces demonstrated a new way to solve the adhesion problem. A lubricant layer on the slippery surface can act as a barrier between the repelled materials and the surface structure. However, the slippery surfaces in previous studies rarely showed high-temperature resistance. Here, we describe a protocol for the preparation of slippery surfaces with high-temperature resistance. A photolithography-assisted method was used to fabricate pillar structures on stainless steel. By functionalizing the surface with saline, a slippery surface was prepared by adding silicone oil. The prepared slippery surface maintained the anti-wetting property for water, even when the surface was heated to 300 &#176;C. Also, the slippery surface exhibited great anti-adhesion effects on soft tissues at high temperatures. This type of slippery surface on stainless steel has applications in medical devices, mechanical equipment, etc.

The slippery surface was prepared by adding silicone oil to OTS-coated, chemically etched stainless steel. Due to their similar chemical properties, the surface was completely wetted by silicone oil. The wetting process is shown in Figure 1a. The red dotted line marks the wetting line. After the wetting, a visible oil layer could be distinguished from the dry surface. The slippery property of the prepared slippery surface was investigated by depositing a wate...

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Preparation and High-temperature Anti-adhesion Behavior of a Slippery Surface on Stainless Steel

Slippery surfaces provide a new way to solve the adhesion problem. This protocol describes how to fabricate slippery surfaces at high temperatures. The results demonstrate that the slippery surfaces showed anti-wetting for liquids and a remarkable anti-adhesion effect on soft tissues at high temperatures.

Anti-adhesion surfaces with high-temperature resistance have a wide application potential in electrosurgical instruments, engines, and pipelines. A ...

The overall goal of this experiment is to describe how to fabricate slippery surfaces with high-temperature resistance and to investigate the anti-adhesion effect of the as-prepared surfaces at high temperatures. This method can help answer key questions in the biomedicine field. Such as, soft tissue adhesion problem on the electrosurgical instruments.The main advantage of this technique is that the prepared slip surfaces can achieve excellent adhesion at high temperatures. Demonstrating the procedure will be Liu Guang, a graduate student from my laboratory. To begin this procedure, design and fabricate the photomask as outlined in the text protocol.Next, wash the stainless steel plate in alkaline solutions at room temperature for 15 minutes. Using an ultrasonic cleaning machine, thoroughly clean the plate at working frequency of 40 kilohertz in an ultrasonic power of 500 watts. Then rinse it sequentially with deionized water and hexane, acetone, and ethanol for 10 minutes each.Place the washed plate on a hotplate set to 150 degrees Celsius. Cover the stainless steel with a sheet of aluminum foil and leave it on the hotplate for 30 minutes to dry. After this, transfer the steel to a spin cutter placing it in the center.Using a dropper, deposit about 1 milliliter of positive photoresist on the plate starting from the center and moving toward the edge until the entire plate is covered. Next start the spin cutter spinning at 700 rpm for six seconds and then increase to 1500 rpm for 15 seconds to evenly spread the photoresist. Then release the vacuum valve.Using a pair of tweezers, remove the coated steel from the spin cutter. Keep the steel on a hotplate at 120 degrees Celsius for two minutes to bake the photoresist. Next transfer the stainless steel to the vacuum valve of the photomatography machine.Set the exposure time to 25 seconds and turn the photomatography machine on. After this remove the steel. Submerge it in developer solution for one minute to remove the photoresist without exposing it to UV light.Then remove the plate from the developer solution and wash it with deionized water. Dry the washed plate under nitrogen gas. Next place the dried steel on a hotplate.Bake it at 120 degrees Celsius for two minutes. Using an upright microscope with a magnification of 100 times, inspect the obtained photoresist texture on the stainless steel. To begin, prepare 200 milliliters of chemical etching solution in a 500 milliliter beaker.Then add the stainless steel. Leave the plate in the solution for 10 minutes. Using tweezers, remove the chemically etched steel.Wash with deionized water for one minute. Dry using nitrogen gas. Use an ultrasonic cleaning machine to clean the steel in acetone for five minutes to remove the photoresist texture.Next dry the etched plate with the nitrogen gas. Use a steady stream of deionized water to clean the chemically etched stainless steel. Dry with nitrogen gas.Using a hotplate, heat the steel to 100 degrees Celsius for 30 minutes to completely dry the surface. Next transfer the steel to an RF plasma machine. Use an RF power of 100 watts, a system pressure of 100 millibar, and flow rate of 20 SSCM to hydroxylate the steel with an O2 plasma treatment for 10 minutes.After this prepare one milliliter OTS solution in anhydrous toluene. Transfer the etched steel in the OTS solution. Seal the beaker and let it rest for four hours at room temperature.Then remove the steel from the solution and clean it with anhydrous toluene. Using an ultrasonic cleaning machine, clean the plate for 10 minutes. Dry it with nitrogen gas.To begin use a dropper to deposit approximately 10 milliliters of silicone oil onto the OTS coated chemically etched stainless steel. Next use an optical stereomicroscope to observe the wetting process of the silicone on the steel surface. Place the steel plate in a vertical position for one hour to remove any excess oil.Then deposit a four microliter droplet of water on the slippery silicon surface. Load the steel into an optical microscope and tilt it to about two degrees. At a low magnification, observe the water droplet to confirm that it can easily move on the slippery surface.Using tweezers, transfer the steel onto a hotplate. Set the temperature to analyze the anti-wetting behaviors at different high temperatures as outlined in the text protocol. Fix a high-speed camera to a tripod and direct it toward the steel.After adjusting the focus, use a microsyringe to deposit 10 microliters of water on the slippery surface and record the movement of the water droplet at a frame rate of 500 hertz. Stop recording when the droplet slides off the steel slippery surface. Then analyze the slippery surface's anti-adhesion effects on soft tissue as outlined in the test protocol.In this study, a slippery surface is prepared by adding silicone oil to OTS coated chemically etched stainless steel. After the wetting processing is complete, a visible oil layer can be distinguished from the dry surface. The slippery property is then investigated depositing a droplet of water on the prepared surface when it is oriented at an angle of two degrees.The yellow dotted line marks the point of contact and the water droplet is seen to float and slide along the surface. Next the anti-wetting behaviors are investigated at various high temperatures. At 200 degrees Celsius, the water droplet is initially seen to firmly contact the surface but that contact decreases over time.At 6200 milliseconds, the droplet begins to slide off the surface. At 250 degrees Celsius, the initial contact area of the droplet is seen to be significantly smaller. At this temperature, the droplet begins sliding off the surface after only 800 milliseconds.However, at 300 degrees Celsius the droplet is immediately unstable on contact and slides off the surface rapidly after only 250 milliseconds. Then the anti-adhesion effect of the slippery surface on soft tissue is evaluated my measuring the adhesion force. The adhesion force is seen to be 0.80 plus or minus 0.18 newtons on the smooth stainless steel and 0.04 plus or minus 0.02 newtons on the slippery surface.Thus, there was an order of magnitude difference in the adhesion force between the slippery surface and the smooth stainless steel surface. Once mastered, this technique can be done in 12 hours if it is performed properly. This method can provide insight into designing and fabricating electrosurgical instruments with slippery surfaces for effective adhesion effect.It can also be applied to other systems such as lubrication of controls and adhesion of agents. While attempting this procedure, it's important to remember to avoid touching the hotplate when it is at high temperatures. After its development, this technique paved the way for researchers in the field of biomedical engineering to solve soft tissue adhesion problems in electrosurgical instruments.After watching this video, you should have a good understanding of how to fabricate a slippery surface with high temperature resistance.

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Mechanical Expansion of Steel Tubing as a Solution to Leaky Wellbores

Wellbore cement, a procedural component of wellbore completion operations, primarily provides zonal isolation and mechanical support of the metal pipe (casing), and protects metal components from corrosive fluids. These are essential for uncompromised wellbore integrity. Cements can undergo multiple forms of failure, such as debonding at the cement/rock and cement/metal interfaces, fracturing, and defects within the cement matrix. Failures and defects within the cement will ultimately lead to fluid migration, resulting in inter-zonal fluid migration and premature well abandonment. Currently, there are over 1.8 million operating wells worldwide and over one third of these wells have leak related problems defined as Sustained Casing Pressure (SCP)1. 
The focus of this research was to develop an experimental setup at bench-scale to explore the effect of mechanical manipulation of wellbore casing-cement composite samples as a potential technology for the remediation of gas leaks. 
The experimental methodology utilized in this study enabled formation of an impermeable seal at the pipe/cement interface in a simulated wellbore system. Successful nitrogen gas flow-through measurements demonstrated that an existing microannulus was sealed at laboratory experimental conditions and fluid flow prevented by mechanical manipulation of the metal/cement composite sample. Furthermore, this methodology can be applied not only for the remediation of leaky wellbores, but also in plugging and abandonment procedures as well as wellbore completions technology, and potentially preventing negative impacts of wellbores on subsurface and surface environments.

This article reports on a laboratory scale investigation of an existing field procedure and its adaptation for sealing of leaky wellbores. It consists of mechanical expansion of metal pipe, which results in an improved metal/cement bond, ultimate sealing of hydraulic pathways and prevention of gas leaks caused by the presence of a microannular channel.

Wellbore cement, a procedural component of wellbore completion operations, primarily provides zonal isolation and mechanical support of the metal pipe ...

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 ...

The Evolution of Silica Nanoparticle-polyester Coatings on Surfaces Exposed to Sunlight

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, building and food industries, amongst others. Polyester and coatings containing both polyester and silica nanoparticles (SiO2NPs) have been widely used to protect steel substrata from corrosion. In this study, we utilized X-ray photoelectron spectroscopy, attenuated total reflection infrared micro-spectroscopy, water contact angle measurements, optical profiling and atomic force microscopy to provide an insight into how exposure to sunlight can cause changes in the micro- and nanoscale integrity of the coatings. No significant change in surface micro-topography was detected using optical profilometry, however, statistically significant nanoscale changes to the surface were detected using atomic force microscopy. Analysis of the X-ray photoelectron spectroscopy and attenuated total reflection infrared micro-spectroscopy data revealed that degradation of the ester groups had occurred through exposure to ultraviolet light to form COO&#903;, -H2C&#903;, -O&#903;, -CO&#903; radicals. During the degradation process, CO and CO2 were also produced.

Two types of surfaces, polyester-coated steel and polyester coated with a layer of silica nanoparticles, were studied. Both surfaces were exposed to sunlight, which was found to cause substantial changes in the chemistry and nanoscale topography of the surface.

Corrosion of metallic surfaces is prevalent in the environment and is of great concern in many areas, including the military, transport, aviation, ...

Applying X-ray Imaging Crystal Spectroscopy for Use as a High Temperature Plasma Diagnostic

X-ray spectra provide a wealth of information on high temperature plasmas; for example electron temperature and density can be inferred from line intensity ratios. By using a Johann spectrometer viewing the plasma, it is possible to construct profiles of plasma parameters such as density, temperature, and velocity with good spatial and time resolution. However, benchmarking atomic code modeling of X-ray spectra obtained from well-diagnosed laboratory plasmas is important to justify use of such spectra to determine plasma parameters when other independent diagnostics are not available. This manuscript presents the operation of the High Resolution X-ray Crystal Imaging Spectrometer with Spatial Resolution (HIREXSR), a high wavelength resolution spatially imaging X-ray spectrometer used to view hydrogen- and helium-like ions of medium atomic number elements in a tokamak plasma. In addition, this manuscript covers a laser blow-off system that can introduce such ions to the plasma with precise timing to allow for perturbative studies of transport in the plasma.

X-ray spectra provide a wealth of information on high temperature plasmas. This manuscript presents the operation of a high wavelength resolution spatially imaging X-ray spectrometer used to view hydrogen- and helium-like ions of medium atomic number elements in a tokamak plasma.

X-ray spectra provide a wealth of information on high temperature plasmas; for example electron temperature and density can be inferred from line ...

Adsorption Device Based on a Langatate Crystal Microbalance for High Temperature High Pressure Gas Adsorption in Zeolite H-ZSM-5

We present a high-temperature and high-pressure gas adsorption measurement device based on a high-frequency oscillating microbalance (5 MHz langatate crystal microbalance, LCM) and its use for gas adsorption measurements in zeolite H-ZSM-5. Prior to the adsorption measurements, zeolite H-ZSM-5 crystals were synthesized on the gold electrode in the center of the LCM, without covering the connection points of the gold electrodes to the oscillator, by the steam-assisted crystallization (SAC) method, so that the zeolite crystals remain attached to the oscillating microbalance while keeping good electroconductivity of the LCM during the adsorption measurements. Compared to a conventional quartz crystal microbalance (QCM) which is limited to temperatures below 80 &#176;C, the LCM can realize the adsorption measurements in principle at temperatures as high as 200-300 &#176;C (i.e., at or close to the reaction temperature of the target application of one-stage DME synthesis from the synthesis gas), owing to the absence of crystalline-phase transitions up to its melting point (1,470 &#176;C). The system was applied to investigate the adsorption of CO2, H2O, methanol and dimethyl ether (DME), each in the gas phase, on zeolite H-ZSM-5 in the temperature and pressure range of 50-150 &#176;C and 0-18 bar, respectively. The results showed that the adsorption isotherms of these gases in H-ZSM-5 can be well fitted by Langmuir-type adsorption isotherms. Furthermore, the determined adsorption parameters, i.e., adsorption capacities, adsorption enthalpies, and adsorption entropies, compare well to literature data. In this work, the results for CO2 are shown as an example.

A protocol for high-temperature and high-pressure gas adsorption measurements on zeolite H-ZSM-5 using an adsorption measurement device based on a langatate crystal microbalance is presented. Prior to the adsorption measurements, the synthesis of zeolite H-ZSM-5 on the langatate crystal microbalance sensor by the steam-assisted crystallization (SAC) method is demonstrated.

We present a high-temperature and high-pressure gas adsorption measurement device based on a high-frequency oscillating microbalance (5 MHz langatate ...

Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion batteries for use in devices operating at elevated temperatures require thermally stable and non-flammable electrolytes. Ionic liquids (ILs), which are non-flammable, non-volatile, thermally stable molten salts, are an ideal replacement for flammable and low boiling point organic solvent electrolytes currently used today. We herein describe the procedures to: 1) synthesize mono- and di-phosphonium ionic liquids paired with chloride or bis(trifluoromethane)sulfonimide (TFSI) anions; 2) measure the thermal properties and stability of these ionic liquids by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA); 3) measure the electrochemical properties of the ionic liquids by cyclic voltammetry (CV); 4) prepare electrolytes containing lithium bis(trifluoromethane)sulfonamide; 5) measure the conductivity of the electrolytes as a function of temperature; 6) assemble a coin cell battery with two of the electrolytes along with a Li metal anode and LiCoO2 cathode; and 7) evaluate battery performance at 100 &#176;C. We additionally describe the challenges in execution as well as the insights gained from performing these experiments.

Here, we describe protocols to prepare phosphonium-based ionic liquid and lithium bis(trifluoromethane)sulfonimide salt electrolytes, and assemble a non-flammable and high temperature functioning lithium-ion coin cell battery.

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion ...

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 Aligned Steel Fiber Reinforced Cementitious Composite and Its Flexural Behavior

The aim of this work is to present an approach, inspired by the way in which a compass needle maintains a consistent orientation under the action of the Earth&#39;s magnetic field, for manufacturing a cementitious composite reinforced with aligned steel fibers. Aligned steel fiber reinforced cementitious composites (ASFRC) were prepared by applying a uniform electromagnetic field to fresh mortar containing short steel fibers, whereby the short steel fibers were driven to rotate in alignment with the magnetic field. The degree of alignment of steel fibers in hardened ASFRC was assessed both by counting steel fibers in fractured cross-sections and by X-ray computed tomography analysis. The results from the two methods show that the steel fibers in ASFRC were highly aligned while the steel fibers in non-magnetically treated composites were randomly distributed. The aligned steel fibers had a much higher reinforcing efficiency, and the composites, therefore, exhibited significantly enhanced flexural strength and toughness. The ASFRC is thus superior to SFRC in that it can withstand greater tensile stress and more effectively resist cracking.

This protocol describes an approach for manufacturing aligned steel fiber reinforced cementitious composite by applying a uniform electromagnetic field. Aligned steel fiber reinforced cementitious composite exhibits superior mechanical properties to ordinary fiber reinforced concrete.

The aim of this work is to present an approach, inspired by the way in which a compass needle maintains a consistent orientation under the action of the ...

Radio Frequency Magnetron Sputtering of GdBa2Cu3O7&#8722;&#948;/ La0.67Sr0.33MnO3 Quasi-bilayer Films on SrTiO3 (STO) Single-crystal Substrates

Here, we demonstrate a method of coating ferromagnetic La0.67Sr0.33MnO3 (LSMO) nanoparticles on (001) SrTiO3 (STO) single-crystal substrates by radio frequency (RF) magnetron sputtering. LSMO nanoparticles were deposited with diameters from 10 to 20 nm and heights between 20 and 50 nm. At the same time, (Gd) Ba2Cu3O7&#8722;&#948; ((Gd) BCO) films were fabricated on both undecorated and LSMO nanoparticle decorated STO substrates using RF magnetron sputtering. This report also describes the properties of GdBa2Cu3O7&#8722;&#948;/ La0.67Sr0.33MnO3 quasi-bilayer films structures (e.g., crystalline phase, morphology, chemical composition); magnetization, magneto-transport, and superconducting transport properties were also evaluated.

Radio Frequency Magnetron Sputtering of GdBa2Cu3O7ÃƒÂ¢Ã‹â€ &#039;ÃƒÅ½ ´/ La0.67Sr0.33MnO3 Quasi-bilayer Films on SrTiO3 STO Single-crystal Substrates

Here, we present a protocol to grow LSMO nanoparticles and (Gd) BCO films on (001) SrTiO3 (STO) single-crystal substrates by radio frequency (RF)-sputtering.

Here, we demonstrate a method of coating ferromagnetic La0.67Sr0.33MnO3 (LSMO) nanoparticles on (001) SrTiO3 (STO) single-crystal substrates by radio ...

Generating Lap Joints Via Friction Stir Spot Welding on DP780 Steel

Friction stir spot welding (FSSW), a derivative of friction stir welding (FSW), is a solid-state welding technique that was developed in 1991. An industry application was found in the automotive industry in 2003 for the aluminum alloy that was used in the rear doors of automobiles. Friction stir spot welding is mostly used in Al alloys to create lap joints. The benefits of friction stir spot welding include a nearly 80% melting temperature that lowers the thermal deformation welds without splashing compared to resistance spot welding. Friction stir spot welding includes 3 steps: plunging, stirring, and retraction. In the present study, other materials including high strength steel are also used in the friction stir welding method to create joints. DP780, whose traditional welding process involves the use of resistance spot welding, is one of several high strength steel materials used in the automotive industry. In this paper, DP780 was used for friction stir spot welding, and its microstructure and microhardness were measured. The microstructure data showed that there was a fusion zone with fine grain and a heat effect zone with island martensite. The microhardness results indicated that the center zone exhibited a greater degree of hardness compared with the base metal. All data indicated that the friction stir spot welding used in dual phase steel 780 can create a good lap joint. In the future, friction stir spot welding can be used in high-strength steel welding applied in industrial manufacturing processes.

Here, we present a friction stir spot welding (FSSW) protocol on dual phase 780 steel. A tool pin with high-speed rotation generates heat from friction to soften the material, and then, the pin plunges into 2 sheet joints to create the lap joint.

Friction stir spot welding (FSSW), a derivative of friction stir welding (FSW), is a solid-state welding technique that was developed in 1991. An industry ...