Name: aesthetically enhanced silica aerogel via incorporation of laser etching and dyes
Uploaded: 2021-03-12T13:00:00
Description: Watch this Scientific Journal Video about Aesthetically Enhanced Silica Aerogel Via Incorporation of Laser Etching and Dyes at JoVE.com

The authors would like to acknowledge the Union College Faculty Research Fund, Student Research Grant program, and the summer undergraduate research program for financial support of the project. The authors would also like to acknowledge Joana Santos for the design of the three-piece mold, Chris Avanessian for SEM imaging, Ronald Tocci for etching onto the curved aerogel surface, and Dr. Ioannis Michaloudis for inspiration and initial work on the etching project as well as for providing the Kouros image and cylindrical aerogel.

Safety glasses or goggles should be worn when preparing the aerogel precursor solutions, working with the hot press, and using the laser engraving system. Laboratory gloves should be worn when cleaning and preparing the mold, preparing the chemical reagent solution, pouring the solution into the mold in the hot press and handling the aerogel. Read Safety Data Sheets (SDS) for all chemicals, including solvents, prior to working with them.Tetramethyl orthosilicate (TMOS), methanol and concentrated ammonia, and solutions co...

<ol>
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M., Prasad, C., Hagerman, M. E., Carroll, M. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cobalt-alumina+sol+gels:+Effects+of+heat+treatment+on+structure+and+catalytic+ability.">Cobalt-alumina sol gels: Effects of heat treatment on structure and catalytic ability.</a> Journal of Non-Crystalline Solids. 453, 94-102 (2016).</li><li>Dunn, N. J. H., Carroll, M. K., Anderson, A. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+alumina+and+nickel-alumina+aerogels+prepared+via+rapid+supercritical+extraction.">Characterization of alumina and nickel-alumina aerogels prepared via rapid supercritical extraction.</a> Polymer Preprints. 52 (1), 250-251 (2011).</li><li>Tobin, Z. M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+and+characterization+of+copper-containing+alumina+and+silica+aerogels+for+catalytic+applications.">Preparation and characterization of copper-containing alumina and silica aerogels for catalytic applications.</a> Journal of Sol-gel Science and Technology. 84 (3), 432-445 (2017).</li><li>Tsou, P., Brownlee, D. E., Glesias, R., Grigoropoulos, C. P., Weschler, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cutting+silica+aerogel+for+particle+extraction.">Cutting silica aerogel for particle extraction.</a> Lunar and Planetary Science XXXVI. Part 19. , (2005).</li><li>Ishii, H. 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This protocol demonstrates how laser etching and the inclusion of dyes can be employed to prepare aesthetically pleasing aerogel materials.
Making large (10 cm x 11 cm x 1.5 cm) aerogel monoliths requires proper mold preparation through sanding, cleaning, and grease application to prevent the aerogel from sticking to the mold and major cracks from forming. The parts of the mold in direct contact with the precursor solution/soon to be formed aerogel are the most critical. Reducing the surface r...

Silica aerogel is a nanoporous, high surface area, acoustically insulating material with low thermal conductivity that can be used in a range of applications from collecting space dust to building insulation material1,2. When manufactured in monolithic form, silica aerogels are translucent and can be used to make highly insulating windows3,4,5.
Recently, we have demonstrated that it is possible to alter the appearance of a silica aerogel by etching onto or cutting through the surface using a laser engraving system6,7 without causing bulk structural damage to the aerogel. This could be useful for making aesthetic enhancements, printing inventory information and machining aerogel monoliths into various forms. Femtosecond lasers have been shown to work for crude &#34;micro-machining&#34; of aerogels8,9,10,11; however, the current protocol demonstrates the ability to alter the surface of aerogels with a simple laser engraving system. As a result, this protocol is broadly applicable to the artistic and technical communities.
It is also possible to incorporate dyes into the aerogel chemical precursor mixture and thereby make dye-doped aerogels with a range of hues. This method has been used to fabricate chemical sensors12,13, to enhance Cerenkov detection14, and for purely aesthetic reasons. Here, we demonstrate the use of dyes and laser etching to prepare aesthetically pleasing aerogels.
In the section that follows, we describe procedures for making large silica aerogel monoliths, altering the monolith preparation procedure to incorporate dyes, etching text, patterns and images onto the surface of an aerogel monolith, and cutting shapes from large dyed monoliths to be assembled into mosaics.

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>2000 grit sandpaper</td>
			<td>Various</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>50W Laser Engraver</td>
			<td>Epilog Laser</td>
			<td></td>
			<td>Any laser cutter is suitable</td>
		</tr>
		<tr>
			<td>Acetone</td>
			<td>Fisher Scientific www.fishersci.com</td>
			<td>A18-20</td>
			<td>Certified ACS Reagent Grade&#160;</td>
		</tr>
		<tr>
			<td>Ammonium Hydroxide (aqueous ammonia)</td>
			<td>Fisher Scientific www.fishersci.com</td>
			<td>A669S212</td>
			<td>Certified ACS Plus, about 14.8N, 28.0-20.0 w/w%</td>
		</tr>
		<tr>
			<td>Beakers</td>
			<td>Purchased from Fisher Scientific</td>
			<td></td>
			<td>Any glass beaker is suitable.</td>
		</tr>
		<tr>
			<td>Deionized Water</td>
			<td>On tap in house</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Digital balance</td>
			<td>OHaus Explorer Pro</td>
			<td></td>
			<td>Any digital balance is suitable.</td>
		</tr>
		<tr>
			<td>Disposable cleaning wipes</td>
			<td>Fisher Scientific www.fishersci.com</td>
			<td>06-666</td>
			<td>KimWipe</td>
		</tr>
		<tr>
			<td>Drawing Software</td>
			<td>CorelDraw Graphics Suite</td>
			<td></td>
			<td>CorelDraw</td>
		</tr>
		<tr>
			<td>Flexible Graphite Sheet</td>
			<td>Phelps Industrial Products</td>
			<td>7500.062.3</td>
			<td>1/16&#34; thick</td>
		</tr>
		<tr>
			<td>Fluorescein</td>
			<td>Sigma Aldrich www.sigmaaldrich.com</td>
			<td>F2456</td>
			<td>Dye content ~95%</td>
		</tr>
		<tr>
			<td>Foam paint brush&#160;</td>
			<td>Various&#160;</td>
			<td></td>
			<td>1-2 cm size</td>
		</tr>
		<tr>
			<td>High Vacuum Grease</td>
			<td>Dow Corning</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Hydraulic Hot Press</td>
			<td>Tetrahedron www.tetrahedronassociates.com</td>
			<td>MTP-14</td>
			<td>Any hot press with temperature and force control will work. Needs maximum temperature of ~550 F and maximum force of 24 tons.</td>
		</tr>
		<tr>
			<td>Laser Engraver</td>
			<td>Epilogue Laser</td>
			<td>Helix - 24</td>
			<td>50 W</td>
		</tr>
		<tr>
			<td>Methanol (MeOH)</td>
			<td>Fisher Scientific www.fishersci.com</td>
			<td>A412-20</td>
			<td>Certified ACS Reagent Grade, &#8805;99.8%</td>
		</tr>
		<tr>
			<td>Mold</td>
			<td>Fabricated in House</td>
			<td></td>
			<td>Fabricate from cold-rolled steel or stainless steel.</td>
		</tr>
		<tr>
			<td>Paraffin Film</td>
			<td>Fisher Scientific www.fishersci.com</td>
			<td>S37441</td>
			<td>Parafilm M Laboratory Film</td>
		</tr>
		<tr>
			<td>Rhodamine-6G 
			Rhodamine-6g 
			FlouresceinRhodamine-6g</td>
			<td>Sigma Aldrich www.sigmaaldrich.com</td>
			<td>20,132-4</td>
			<td>Dye content ~95%</td>
		</tr>
		<tr>
			<td>Rhodamine-B 
			Rhodamine-6g 
			FlouresceinRhodamine-6g</td>
			<td>Sigma Aldrich www.sigmaaldrich.com</td>
			<td>R-953</td>
			<td>Dye content ~80%</td>
		</tr>
		<tr>
			<td>Soap to clean mold</td>
			<td>Various</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Stainless Steel Foil</td>
			<td>Various</td>
			<td></td>
			<td>.0005&#34; thick, 304 Stainless Steel</td>
		</tr>
		<tr>
			<td>Tetramethylorthosilicate (TMOS)</td>
			<td>Sigma Aldrich www.sigmaaldrich.com</td>
			<td>218472-500G</td>
			<td>98% purity, CAS 681-84-5</td>
		</tr>
		<tr>
			<td>Ultrasonic Cleaner</td>
			<td>FisherScientific FS6</td>
			<td>153356</td>
			<td>Any sonicator is suitable.</td>
		</tr>
		<tr>
			<td>Vacuum Exhaust system</td>
			<td>Purex</td>
			<td>800i</td>
			<td>Any exhaust system is suitable.</td>
		</tr>
		<tr>
			<td>Variable micropipettor, 100-1000 &#181;L</td>
			<td>Manufactured by Eppendorf, purchased from Fisher Scientific www.fishersci.com</td>
			<td>S304665</td>
			<td>Any 100-1000 &#181;L pipettor is suitable.</td>
		</tr>
	</tbody>
</table>

aesthetically enhanced silica aerogel via incorporation of laser etching and dyes

A procedure for aesthetically enhancing silica aerogel monoliths by laser etching and incorporation of dyes is described in this manuscript. Using a rapid supercritical extraction method, large silica aerogel monolith (10 cm x 11 cm x 1.5 cm) can be fabricated in about 10 h. Dyes incorporated into the precursor mixture result in yellow-, pink- and orange-tinged aerogels. Text, patterns, and images can be etched onto the surface (or surfaces) of the aerogel monolith without damaging the bulk structure. The laser engraver can be used to cut shapes from the aerogel and form colorful mosaics.

This protocol can be employed to prepare a wide variety of aesthetically pleasing aerogel monoliths for applications including, but not limited to, art and sustainable building design. Inclusion in the precursor mixture of the small amounts of dye employed here is only observed to impact the color of the resulting aerogel monolith; changes in other optical or structural properties are not observed.
Figure 8<...

Watch this Scientific Journal Video about Aesthetically Enhanced Silica Aerogel Via Incorporation of Laser Etching and Dyes at JoVE.com

Aesthetically Enhanced Silica Aerogel Via Incorporation of Laser Etching and Dyes

This protocol describes a method for etching text, patterns, and images onto the surface of silica aerogel monoliths in native and dyed form and assembling the aerogels into mosaic designs.

A procedure for aesthetically enhancing silica aerogel monoliths by laser etching and incorporation of dyes is described in this manuscript. Using a rapid ...

This protocol presents the first visual methodology for etching and cutting plain and dyed Aerogel using a laser engraving system. The main advantage of this technique is its simplicity as it allows Aerogel monoliths of any shape, size, or color to be etched. Video presentation allows demonstration of the practical considerations of the protocol, including placement of the Aerogel and alignment of the laser cutter.To prepare a mold for Aerogel monolith fabrication, select a three-part steel mold consisting of a top, middle, and bottom part with outer dimensions of 15.24 by 14 centimeters in a 10 by 11 centimeter cavity in the center. The top part of the mold should have seven 0.08 centimeter vent holes on each side. Use diluted soap and a rough textured sponge to scrub the top, middle, and bottom parts of the mold and dry all of the clean parts of the mold with a paper towel.After drying, use individual disposable acetone-dipped cleaning wipes to wipe the mold until the cleaning wipe remains clean. Next, use 2, 000 grit sandpaper to lightly sand all of the surfaces until the mold is smooth to the touch and any residue from previous uses has been removed, paying extra attention to the inside of the middle mold where the Aerogel is formed. Clear the vent holes on the top mold part with compressed air and manually apply approximately 2.4 milliliters of high vacuum grease in a thick, even one to two millimeter layer over the entire top connecting surface of the bottom mold and approximately one milliliter of grease in a thick, even one to two millimeter layer to the outer half of the bottom connecting surface of the top mold.Apply approximately 0.5 milliliters of high vacuum grease in an even less than 0.5 millimeter layer to the inside surfaces of the top and bottom molds and use a disposable cleaning wipe to wipe away excess grease until the surface feels smooth and no stickiness from the grease remains. Manually apply 0.5 milliliters of high vacuum grease in an even less than 0.5 millimeter layer of grease to the inside surface of the middle mold. To prepare the etching pattern file, open a new document in an appropriate drawing application and add the desired text or image of any size and line width directly to the document, then save the file.To etch an Aerogel monolith, first turn on the laser engraver, vacuum exhaust system, and attached computer. Measure the size of the Aerogel monolith surface that will be etched and open the etching pattern file. Set the document's dimension size to correspond to the measured Aerogel monolith size and open the lid of the laser engraver.Use a gloved hand to place the Aerogel onto the laser engraver platform and align the Aerogel on the top left corner with the Aerogel touching the top and left rulers. Flip the V-shape magnet manual focus gauge attached to the laser upside down and press Focus on the laser engraver. Protect the Aerogel monolith with a disposable cleaning wipe and use the up arrow on the laser engraver control panel to move the laser engraver platform until the bottom part of the manual focus gauge just touches the Aerogel.Remove the wipe and return the gauge to its original position. Close the laser engraver lid and click File and Print in the drawing program. Select the laser engraver as the print location and open the preferences window to set the printer properties.Select the raster mode inside a DPI of 600, a speed of 100%and a power of 55%Confirm that the piece size matches the measured Aerogel monolith size and click Apply and Print. On the front panel of the laser engraver, click Job and select the corresponding filename. Click Go.When the laser engraver finishes, click Focus and use the down arrow on the laser engraver front control panel to lower the base.Use a gloved hand to gently transfer the Aerogel from the laser engraver platform to its container and click Trash to purge the job from the engraver. To cut an Aerogel monolith, turn on the laser engraver, vacuum exhaust system, and attached computer and measure the size of the Aerogel monolith surface to be cut. For general cutting, open a new document in the drawing program and enter the dimensions for the document size to correlate with the measured Aerogel monolith size.Use the hairline width drawing tool to create the pattern that will be cut and position the pattern to match the desired cut location on the Aerogel. Clean a 0.0127 millimeter thick sheet of stainless steel foil large enough to cover the base of the Aerogel monolith with acetone and place the foil onto the laser engraver platform. Align the Aerogel and stainless steel foil in the top left corner with the Aerogel touching the top and left rulers and adjust the gauge position as demonstrated.Click File and Print in the drawing program and select the laser engraver as the print location and open the preferences window to set the printer properties. Select the vector mode and set the DPI to 600, the speed to 3%the power to 90%and the frequency of 1, 000 Hertz. Confirm that the piece size matches the measured Aerogel size.The depth of the cut will vary with the laser speed. Click Job and Go to initiate the cutting as demonstrated. After collecting the sample, use a foam brush to gently remove any small pieces of ablated Aerogel left on the face of the monolith that was in contact with the laser.For this Aerogel mosaic approach, the same pattern was cut into three different dyed Aerogel monoliths and the pieces were reassembled into a mosaic pattern. It is possible to etch designs on smaller monolithic pieces as demonstrated to obtain visually interesting arrangements under natural and ultraviolet light conditions even on smaller pieces. As illustrated, native Aerogels can be etched with patterns of various density with photographs printed onto the front surface of a planar Aerogel, onto a curved surface, and onto fluorescent dyed Aerogels.In this scanning electron microscope image of an etched silica Aerogel, the interface between the etched lines and the almost smooth unetched nanoporous Aerogel can be observed. Etching causes the ablation and melting of the surface material into filament-like structures as observed in this image showing the effect of a single laser pulse of the Aerogel. Careful preparation, including contrast adjustment of the images to be etched, is critical to achieving high-quality results.Further refinement of the laser etching method could provide an alternative to micro-machining of the silica Aerogels. Aesthetic Aerogel monoliths could find application in a wide variety of areas, including artwork and sustainable buildings.

Research

JoVE Journal

Engineering

Fabrication of Silica Ultra High Quality Factor Microresonators

Whispering gallery resonant cavities confine light in circular orbits at their periphery.1-2 The photon storage lifetime in the cavity, quantified by the ...

Spatial Separation of Molecular Conformers and Clusters

Gas-phase molecular physics and physical chemistry experiments commonly use supersonic expansions through pulsed valves for the production of cold ...

Scalable Nanohelices for Predictive Studies and Enhanced 3D Visualization

Spring-like materials are ubiquitous in nature and of interest in nanotechnology for energy harvesting, hydrogen storage, and biological sensing ...

Characterizing Far-infrared Laser Emissions and the Measurement of Their Frequencies

The generation and subsequent measurement of far-infrared radiation has found numerous applications in high-resolution spectroscopy, radio astronomy, and ...

Compact Lens-less Digital Holographic Microscope for MEMS Inspection and Characterization

A micro-electro-mechanical-system (MEMS) is a widely used component in many industries, including energy, biotechnology, medical, communications, and ...

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 ...

Laser-induced Forward Transfer of Ag Nanopaste

Over the past decade, there has been much development of non-lithographic methods1-3 for printing metallic inks or other functional materials. Many of ...

Electrochemical Etching and Characterization of Sharp Field Emission Points for Electron Impact Ionization

A new variation of the drop-off method for fabricating field emission points by electrochemically etching tungsten rods in a NaOH solution is described. ...