This work was funded by NSF grants DMR-0605716 and DMR-1101189. Also, the Cornell NanoScale Science and Technology Center was used to grow and pattern the oxides. We thank them for their assistance. One of us FMG is grateful for the support of the Moti Lal Rustgi Professorship.

1. Before Bonding, Wafer Preparation
This step except for 1.8 is done in the Cornell Nanoscale Facility cleanroom.
<ol>
	<li>Grow the oxides in a standard thermal oxidation furnace using a wet oxide process for thick oxides and, to achieve better thickness control, a dry oxide process for very thin oxides. Check the thickness for uniformity over the full wafer with ellipsometry.</li>
	<li>Create a mask for the geometry you wish to etch.</li>
	<li>Spin photoresist on the wafers being etched.</li>
	<li>Expose, develop and bake a test wafer and examine with an appropriate microscope.</li>
	<li>If the test wafer is exposed as desired, etch the test wafer. The ratio of oxide thickness to lateral feature dimension will determine if a wet or dry etch is appropriate. Since the wet etches are isotropic they will not produce vertical walls in the oxide. In many cases this does not matter. If vertical walls are desired one can use reaction ion etching. If the etching is successful, proceed with the other wafers. Often, the hydrophobic/hydrophilic properties of Si and SiO2 can be used to see if the etching process has been successful.</li>
	<li>Remove the photoresist from the wafers. For most photoresists, this can be done initially with isopropyl alcohol and acetone. However, some small amount of resist will still remain on the wafers. This resist needs to be completely removed in order to achieve good bonding.</li>
	<li>Use a brief 20 min&#160;oxygen descumming process in a reactive ion etcher. This will remove whatever photoresist remains on the wafers. However, this will also add some oxide layers to the exposed silicon. This is typically 1-4 nm15.</li>
	<li>Drill the filling hole in the top wafer. This can be done with diamond tipped drill bits and smart-cut lubrication (see Materials&#160;for manufacturer details). Rinse off the smart-cut immediately after drilling with deionized water. Drilling can also be done using a diamond paste with 3-9 &#181;m grit for filling holes larger than ~0.124 cm in diameter. Smart-cut can again be used for lubrication. We use a small precision drill press at 1,000-2,000 rpm.</li>
</ol>
2. Bonding Preparation
<ol>
	<li>In order to bond wafers, cleanliness is paramount. There are a few steps that should be taken to clean the wafers. First, clean with RCA baths.
	<ol>
		<li>Rinse wafers in deionized (DI) water.</li>
		<li>Clean in &#34;RCA&#34; acid bath. RCA acid bath is H2O:H2O2:HCl with the ratios of 5:1:1. Place wafers in 80 &#176;C RCA acid for 15 min&#160;with the patterned sides facing up. This step will eliminate any metallic contamination.</li>
		<li>Remove wafers from the acid and rinse in DI water bath for 5 min.</li>
		<li>Clean in the &#34;RCA&#34; base next. RCA base is H2O:H2O2:NH4OH with the ratios of 10:2:1. Place wafers in 80 &#176;C RCA base for 15 min&#160;with the patterned sides facing up. This step will eliminate any organic contamination.</li>
		<li>Rinse wafers in DI water bath for ~15 min.</li>
	</ol>
	</li>
	<li>The wafers need to be removed from the DI water bath and remain clean in order for proper bonding to occur. This is done in two steps:
	<ol>
		<li>First, place the wafers with their patterned etched sides facing each other on a Teflon chuck in a clean microchamber as shown in Figure 3B. They are separated by ~1 mm Teflon tabs. Spray deionized water between the wafers while they spin slowly (~10-60 rpm) for ~2 min in order to remove any particle contamination. A film of water will be left between the wafers at this point. This prevents dust contamination prior to the next step.</li>
		<li>Cover the wafers with the clear acrylic lid and spin the wafers dry for ~30 min at 3,000 rpm. Use a 250 W infrared heat lamp to aid the drying process. The rapid spinning will entrain any particle contaminants with the ejection of the water film, as in Figure 3C.</li>
	</ol>
	</li>
	<li>Before removing the lid over the wafers, remove the tabs separating the wafers by rotating the lid. This will bring the wafers into light local contact while still in the microclean chamber. Now the wafers may be safely removed from the microclean chamber on their carrier. The very small gap of approximately 1 &#181;m between the wafers will minimize dust contamination during this step. Also, do not pick up the wafers with tweezers at this point since this would initiate asymmetric bonding. Instead, transport the wafers with the use of the removable carrier onto the arbor press.</li>
</ol>
3. Wafer Bonding
<ol>
	<li>Press the two wafers together using an arbor press and a fairly rigid and smooth (Nerf) ball. The Nerf ball is used to apply pressure to the wafers from the middle outward. Pressure applied this way allows trapped air to be pushed out as the bonding wave spreads from the center out. Starting the bonding at the center minimizes the stresses which are built up as the wafers contour to each other. The wafers have a free-state flatness of about 1 &#181;m, while the gaps achieved in the bonding are uniform within a few nm. Thus, the wafers must distort from their free state in order to achieve this.
	<ol>
		<li>Check the bonding by looking for interference fringes using an infrared light source and detector with a 1 &#181;m high pass filter. Sample images are shown in Figures 4 and 5. Interference fringes (Newton rings) will appear if there is poor bonding. If bonding is good, one can proceed to step 3.3. If bonding is poor and there are nonuniformities, proceed as follows.</li>
		<li>Place the cell on an optical flat, cover with filter paper to protect and cushion the top wafer, and press the wafers together with wafer tongs. Push debonded &#34;bubbles&#34; to either the middle (where there is the filling hole) or to the edges. Be careful when applying force near the edges since the wafers may be slightly offset center to center. Pressure near the edges therefore may cause the top wafer to crack if it overhangs the bottom wafer.</li>
		<li>If the bonding irregularities persist or a dust particle is evident, split the wafers by wedging a razor blade between them. Repeat the process from the beginning (step 2.1.1). Up to this point, the bonding is reversible. The wafers can be rebonded at RT many times while trying to get acceptable bonding.</li>
	</ol>
	</li>
	<li>After obtaining acceptable RT bonding, one proceeds to anneal the wafers. Temperatures above 900 &#176;C need to be reached in order to be certain of proper annealing5,6.
	<ol>
		<li>Stage the cell onto a quartz vacuum chuck such that the filling hole is centered over the pumping hole in the chuck. The chuck is connected to a quartz pumping tube which is used to evacuate the cell prior and during the annealing process. This tube extends outside the furnace. Evacuating the cell causes a pressure of one atmosphere to be applied to the cell. This will help with the bonding. Pumping is also necessary to prevent pressure build up if the furnace temperature is ramped up too quickly. The time it takes to significantly lower the pressure in the cell will depend on the geometry within the cell.</li>
		<li>To avoid the growth of oxide on the outside of the cell, purge the furnace chamber with a nonreacting gas, typically 4He, so that no oxide is grown.</li>
		<li>To allow for strains to have time to relax, it is important to ramp temperatures from 250-1,200 &#176;C over the course of ~4 hr. After staying at 1,200 &#176;C for at least 4&#160;hr, turn off the furnace.</li>
		<li>Allow the system to cool to RT.</li>
	</ol>
	</li>
	<li>Analyze the cell once again using the infrared light source and detector as shown in Figure 6. If annealing went well, the cell will look as good as, or often better than, when initially put in the furnace. If there are unacceptable fringes indicating poor bonding, the entire process must be repeated from the beginning; however, this must be done with new wafers. Once annealed, the bond between wafers is permanent and there is no splitting possible.</li>
</ol>

<ol>
	<li>Gasparini, F. M., Kimball, M. O., Mooney, K. P., Diaz-Avila, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Finite-size+scaling+of+He-4+at+the+superfluid+transition.">Finite-size scaling of He-4 at the superfluid transition.</a> Rev. Mod. Phys. 80, 1009-1059 (2008).</li><li>Mehta, S., Kimball, M. O., Gasparini, F. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Superfluid+transition+of+He-4+for+two-dimensional+crossover,+heat+capacity,+and+finite-size+scaling.">Superfluid transition of He-4 for two-dimensional crossover, heat capacity, and finite-size scaling.</a> J. Low Temp. Phys. 114, 467-521 (1999).</li><li>Reppy, J. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Superfluid-Helium+in+Porous-Media.">Superfluid-Helium in Porous-Media.</a> J. Low Temp. Phys. 87, 205-245 (1992).</li><li>Mehta, S., 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=Silicon+wafers+at+sub-mu+m+separation+for+confined+He-4+experiments.">Silicon wafers at sub-mu m separation for confined He-4 experiments.</a> Czech. J. Phys. 46, 133-134 (1996).</li><li>Tong, Q. Y., Cha, G. H., Gafiteanu, R., Gosele, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Low-Temperature Wafer Direct Bonding. J. Microelectromech. S. 3, 29-35 (1994).</li><li>Tong, Q. Y., Gosele, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Semiconductor+Wafer+Bonding+-+Recent+Developments.">Semiconductor Wafer Bonding - Recent Developments.</a> Mater. Chem. Phys. 37, 101-127 (1994).</li><li>Gosele, U., Tong, Q. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Semiconductor+wafer+bonding.">Semiconductor wafer bonding.</a> Annu. Rev. Mater. Sci. 28, 215-241 (1998).</li><li>Rhee, I., Petrou, A., Bishop, D. J., Gasparini, F. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bonding+Si-Wafers+at+Uniform+Separation.">Bonding Si-Wafers at Uniform Separation.</a> Physica B. 165, 123-124 (1990).</li><li>Rhee, I., Gasparini, F. M., Petrou, A., Bishop, D. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Si+Wafers+Uniformly+Spaced+-+Bonding+and+Diagnostics.">Si Wafers Uniformly Spaced - Bonding and Diagnostics.</a> Rev. Sci. Instrum. 61, 1528-1536 (1990).</li><li>Perron, J. K., Kimball, M. O., Mooney, K. P., Gasparini, F. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Critical+behavior+of+coupled+4He+regions+near+the+superfluid+transition.">Critical behavior of coupled 4He regions near the superfluid transition.</a> Phys. Rev. B. 87, (2013).</li><li>Perron, J., Gasparini, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Specific+Heat+and+Superfluid+Density+of+4He+near+T+&#955;+of+a+33.6+nm+Film+Formed+Between+Si.">Specific Heat and Superfluid Density of 4He near T &#955; of a 33.6 nm Film Formed Between Si.</a> , 1-10 (2012).</li><li>Perron, J. K., Gasparini, F. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Critical+Point+Coupling+and+Proximity+Effects+in+He-4+at+the+Superfluid+Transition.+.">Critical Point Coupling and Proximity Effects in He-4 at the Superfluid Transition. .</a> Phys. Rev. Lett.. 109, (2012).</li><li>Gasparini, F. M., Kimball, M. O., Mehta, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Adiabatic+fountain+resonance+for+He-4+and+He-3-He-4+mixtures.">Adiabatic fountain resonance for He-4 and He-3-He-4 mixtures.</a> J. Low Temp. Phys. 125, 215-238 (2001).</li><li>Corruccini, R. J., Gniewek, J. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermal+expansion+of+technical+solids+at+low+temperatures;+a+compilation+from+the+literature.">Thermal expansion of technical solids at low temperatures; a compilation from the literature.</a> U.S. Dept. of Commerce, National Bureau of Standards. , (1961).</li><li>Kahn, H., Deeb, C., Chasiotis, I., Heuer, A. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Anodic+oxidation+during+MEMS+processing+of+silicon+and+polysilicon:+Native+oxides+can+be+thicker+than+you+think.">Anodic oxidation during MEMS processing of silicon and polysilicon: Native oxides can be thicker than you think.</a> J. Microelectromech. S. 14, 914-923 (2005).</li><li>Tong, Q. Y., Gosele, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thickness+Considerations+in+Direct+Silicon-Wafer+Bonding.">Thickness Considerations in Direct Silicon-Wafer Bonding.</a> J. Electrochem. Soc. 142, 3975-3979 (1995).</li><li>Corbino, O. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Azioni+Elettromagnetiche+Doyute+Agli+Ioni+dei+Metalli+Deviati+Dalla+Traiettoria+Normale+per+Effetto+di+un+Campo.">Azioni Elettromagnetiche Doyute Agli Ioni dei Metalli Deviati Dalla Traiettoria Normale per Effetto di un Campo.</a> Nuovo Cim. 1, 397-420 (1911).</li><li>Diaz-Avila, M., Kimball, M. O., Gasparini, F. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Behavior+of+He-4+near+T-lambda+in+films+of+infinite+and+finite+lateral+extent.">Behavior of He-4 near T-lambda in films of infinite and finite lateral extent.</a> J. Low Temp. Phys. 134, 613-618 (2004).</li><li>Dimov, S., 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=Anodically+bonded+submicron+microfluidic+chambers.">Anodically bonded submicron microfluidic chambers.</a> Rev. Sci. Instrum. 81, (2010).</li><li>Duh, A., 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=Microfluidic+and+Nanofluidic+Cavities+for+Quantum+Fluids+Experiments.">Microfluidic and Nanofluidic Cavities for Quantum Fluids Experiments.</a> J. Low Temp. Phys. 168, 31-39 (2012).</li></ol>

We have nothing to disclose.

The development of suitable silicon lithography in combination with direct wafer bonding has allowed us to make vacuum tight enclosures with highly uniform small dimensions over all the full area of a 5 cm diameter silicon wafer. These enclosures have allowed us to study the behavior of liquid 4He in the neighborhood of its phase transitions from a normal liquid to a superfluid. These studies have verified predictions of finite-size scaling, as well as pointed out failures which remain to be explored. The work...

When clean silicon wafers are brought into intimate contact at RT, they are attracted to each other via van der Waals forces and form weak local bonds. This bonding can be made much stronger by annealing at higher temperatures5,6. Bonding can be done successfully with surfaces of either SiO2 to Si or SiO2 to SiO2. Bonding of Si wafers are most commonly used for silicon on insulator devices, silicon-based sensors and actuators, and optical devices7. The work described here takes wafer direct bonding in a different direction by using it to achieve well-defined uniformly-spaced enclosures over the entire wafer area8,9. Having a well-defined geometry where fluid can be introduced allows measurements to be performed in order to determine the effect of the confinement on the properties of the fluid. Hydrodynamic flows can be studied where the small dimension can be controlled from tens of nanometers to several micrometers.
SiO2 can be grown on Si wafers using a wet or dry thermal oxide process in a furnace. The SiO2 can then be patterned and etched as desired using lithographic techniques. Patterns which have been used in our work include a pattern of widely spaced support posts which results upon bonding in a planar or film geometry (see Figure 1). We have also patterned channels for one-dimensional characteristics, and arrays of boxes, either of (1 &#181;m)3 or (2 &#181;m)3 dimension1 (see Figure 2). When designing a confinement with boxes, typically 10-60 million on a wafer, there needs to be a way to fill all of the individual boxes. A separate patterning of the top wafer with a design that stands off the two wafers by 30 nm or more allows for this. Or, equivalently, shallow channels can be designed on the top wafer so that all the boxes are linked. The thickness of the oxide grown on the top wafer is different from that on the bottom wafer. This adds another degree of flexibility and complexity to the design. Being able to pattern both wafers allows for a larger variety of confinement geometries to be realized.
The size of the geometric features in these bonded wafers, or cells, can vary. Cells with planar films as small as 30 nm have been made successfully10,11. At thicknesses below this, overbonding can take place whereby the wafers bend around the support posts thus &#34;sealing&#34; the cell. Recently, a series of measurements on liquid 4He have been performed with an array of (2 &#181;m)3 boxes with varying separation distance between them10,12. Features much larger in depth than 2 &#181;m are not very practical due to the increasing length of time required to grow the oxide. However, measurements have been made with an oxide as thick as 3.9 &#181;m9. The limits on the smallness of the lateral dimension arise from the limits of the lithography capabilities. The limit for the largeness of the lateral dimension is determined by the size of the wafer. We have successfully created planar cells where the lateral dimension spanned almost the entire wafer diameter, but one could just as easily imagine patterning several smaller structures on the order of tens of nanometers in width. However such structures would require e-beam lithography. We have not done this at this time.
In all of our work the bonded wafers formed a vacuum tight enclosure. This is achieved by retaining in the patterned oxide a solid ring of SiO2 of 3-4 mm in width at the perimeter of the wafer, see Figure 1. This, upon bonding, forms a tight seal. This design could be easily modified if one were interested in hydrodynamic studies which require an input and an output.
The bursting pressure of the bonded cells has also been tested. We found that with 375 &#181;m thick wafers, pressure up to approximately nine atmospheres could be applied. However, we have not studied how this could be improved by bonding over larger oxide areas or, perhaps, for thicker wafers.
The procedure for interfacing the silicon cells to a filling line and the techniques for measuring the properties of the confined helium at low temperature is given in &#160;Mehta et al.2 and Gasparini et al.13&#160;We note that changes in linear dimension for silicon are only 0.02% upon cooling the cells14. This is negligible for the patterns formed at RT.

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			<td height="20" style="height:20px;width:215px;">SmartCut</td>
			<td style="width:192px;">North American Tool</td>
			<td style="width:104px;">FL 130</td>
			<td style="width:600px;">Not much is needed per cell. Smaller sizes are available.</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Silicon Wafers</td>
			<td>Semiconductor Processing Co</td>
			<td></td>
			<td>There are many suppliers. Pay attention to thickness and thickness variation when ordering.</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Deionized Water</td>
			<td></td>
			<td></td>
			<td>General Availability</td>
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			<td height="20" style="height:20px;">Peroxide</td>
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			<td height="20" style="height:20px;">Diamond Paste</td>
			<td>Beuler Metadi II</td>
			<td>e.g. 406533032</td>
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			<td height="20" style="height:20px;">Diamond Drills</td>
			<td>Starlite</td>
			<td>e.g. 115010</td>
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			<td height="20" style="height:20px;">Pyrex Dishes</td>
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			<td height="20" style="height:20px;">Quartz tubes for flushing furnace</td>
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			<td height="20" style="height:20px;">Rubber vacuum hose</td>
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</table>

fabrication of uniform nanoscale cavities via silicon direct wafer bonding

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

Properly bonded wafers will have no unbonded regions. Attempting to split the wafers after annealing will cause the cell to break into pieces due to the strength of the bond. Infrared images of properly bonded wafer are shown in Figures 5 and 6. Often annealing improves the uniformity of the cell, especially if local unbonded regions are due to lack of flatness in the wafers. In Figure&#160;5 the light spots and border are bonded areas. The center bright spot is the hole...

Watch this Scientific Journal Video about Fabrication of Uniform Nanoscale Cavities via Silicon Direct Wafer Bonding at JoVE.com

Fabrication of Uniform Nanoscale Cavities via Silicon Direct Wafer Bonding

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

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

fabrication-uniform-nanoscale-cavities-via-silicon-direct-wafer

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Engineering

7.2K vistas.  The State University of New York at Buffalo. Se describe un método para unir permanentemente dos obleas de silicio con el fin de realizar un recinto uniforme. Esto incluye la preparación de obleas, la limpieza, la unión RT y los procesos de recocido. Las obleas (células) enlazadas resultantes tienen uniformidad de recinto ~1%1,2. La geometría resultante permite mediciones de líquidos y gases confinados.

Video: Fabrication of Uniform Nanoscale Cavities via Silicon Direct Wafer Bonding

Fabrication And Characterization Of Photonic Crystal Slow Light Waveguides And Cavities

Slow light has been one of the hot topics in the photonics community in the past decade, generating great interest both from a fundamental point of view and for its considerable potential for practical applications. Slow light photonic crystal waveguides, in particular, have played a major part and have been successfully employed for delaying optical signals1-4 and the enhancement of both linear5-7 and nonlinear devices.8-11
Photonic crystal cavities achieve similar effects to that of slow light waveguides, but over a reduced band-width. These cavities offer high Q-factor/volume ratio, for the realization of optically12 and electrically13 pumped ultra-low threshold lasers and the enhancement of nonlinear effects.14-16 Furthermore, passive filters17 and modulators18-19 have been demonstrated, exhibiting ultra-narrow line-width, high free-spectral range and record values of low energy consumption.
To attain these exciting results, a robust repeatable fabrication protocol must be developed. In this paper we take an in-depth look at our fabrication protocol which employs electron-beam lithography for the definition of photonic crystal patterns and uses wet and dry etching techniques. Our optimised fabrication recipe results in photonic crystals that do not suffer from vertical asymmetry and exhibit very good edge-wall roughness. We discuss the results of varying the etching parameters and the detrimental effects that they can have on a device, leading to a diagnostic route that can be taken to identify and eliminate similar issues.
The key to evaluating slow light waveguides is the passive characterization of transmission and group index spectra. Various methods have been reported, most notably resolving the Fabry-Perot fringes of the transmission spectrum20-21 and interferometric techniques.22-25 Here, we describe a direct, broadband measurement technique combining spectral interferometry with Fourier transform analysis.26 Our method stands out for its simplicity and power, as we can characterise a bare photonic crystal with access waveguides, without need for on-chip interference components, and the setup only consists of a Mach-Zehnder interferometer, with no need for moving parts and delay scans.
When characterising photonic crystal cavities, techniques involving internal sources21 or external waveguides directly coupled to the cavity27 impact on the performance of the cavity itself, thereby distorting the measurement. Here, we describe a novel and non-intrusive technique that makes use of a cross-polarised probe beam and is known as resonant scattering (RS), where the probe is coupled out-of plane into the cavity through an objective. The technique was first demonstrated by McCutcheon et al.28 and further developed by Galli et al.29

Use of photonic crystal slow light waveguides and cavities has been widely adopted by the photonics community in many differing applications. Therefore fabrication and characterization of these devices are of great interest. This paper outlines our fabrication technique and two optical characterization methods, namely: interferometric (waveguides) and resonant scattering (cavities).

Slow light has been one of the hot topics in the photonics community in the past decade, generating great interest both from a fundamental point of view ...

Concurrent Quantitative Conductivity and Mechanical Properties Measurements of Organic Photovoltaic Materials using AFM

Organic photovoltaic (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale inhomogeneity of OPV materials affects performance of photovoltaic devices. Thus, understanding of spatial variations in composition as well as electrical properties of OPV materials is of paramount importance for moving PV technology forward.1,2 In this paper, we describe a protocol for quantitative measurements of electrical and mechanical properties of OPV materials with sub-100 nm resolution. Currently, materials properties measurements performed using commercially available AFM-based techniques (PeakForce, conductive AFM) generally provide only qualitative information. The values for resistance as well as Young's modulus measured using our method on the prototypical ITO/PEDOT:PSS/P3HT:PC61BM system correspond well with literature data. The P3HT:PC61BM blend separates onto PC61BM-rich and P3HT-rich domains. Mechanical properties of PC61BM-rich and P3HT-rich domains are different, which allows for domain attribution on the surface of the film. Importantly, combining mechanical and electrical data allows for correlation of the domain structure on the surface of the film with electrical properties variation measured through the thickness of the film.

Organic photovoltaic (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale inhomogeneity of OPV materials affects performance of photovoltaic devices. In this paper, we describe a protocol for quantitative measurements of electrical and mechanical properties of OPV materials with sub-100 nm resolution.

Organic photovoltaic  (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale  inhomogeneity of OPV materials affects performance ...

Patterning via Optical Saturable Transitions - Fabrication and Characterization

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

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

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

Thermal Measurement Techniques in Analytical Microfluidic Devices

Thermal measurement techniques have been used for many applications such as thermal characterization of materials and chemical reaction detection. Micromachining techniques allow reduction of the thermal mass of fabricated structures and introduce the possibility to perform high sensitivity thermal measurements in the micro-scale and nano-scale devices. Combining thermal measurement techniques with microfluidic devices allows performing different analytical measurements with low sample consumption and reduced measurement time by integrating the miniaturized system on a single chip. The procedures of thermal measurement techniques for particle detection, material characterization, and chemical detection are introduced in this paper.

Here, we present three protocols for thermal measurements in microfluidic devices.

Thermal measurement techniques have been used for many applications such as thermal characterization of materials and chemical reaction detection. ...

Prescribed 3-D Direct Writing of Suspended Micron/Sub-micron Scale Fiber Structures via a Robotic Dispensing System

A 3-axis dispensing system is utilized to control the initiating and terminating fiber positions and trajectory via the dispensing software. The polymer fiber length and orientation is defined by the spatial positioning of the dispensing system 3-axis stages. The fiber diameter is defined by the prescribed dispense time of the dispensing system valve, the feed rate (the speed at which the stage traverses from an initiating to a terminating position), the gauge diameter of the dispensing tip, the viscosity and surface tension of the polymer solution, and the programmed drawing length. The stage feed rate affects the polymer solution&#8217;s evaporation rate and capillary breakup of the filaments. The dispensing system consists of a pneumatic valve controller, a droplet-dispensing valve and a dispensing tip. Characterization of the direct write process to determine the optimum combination of factors leads to repeatedly acquiring the desired range of fiber diameters. The advantage of this robotic dispensing system is the ease of obtaining a precise range of micron/sub-micron fibers onto a desired, programmed location via automated process control. Here, the discussed self-assembled micron/sub-micron scale 3D structures have been employed to fabricate suspended structures to create micron/sub-micron fluidic devices and bioengineered scaffolds.

Here, we present a protocol to fabricate freely-suspended, micron/sub-micron scale polymer fibers and &#8220;web-like&#8221; structures generated via automated direct writing procedure by means of a 3-axis dispensing system.

A 3-axis dispensing system is utilized to control the initiating and terminating fiber positions and trajectory via the dispensing software. The polymer ...

Solvent Bonding for Fabrication of PMMA and COP Microfluidic Devices

Thermoplastic microfluidic devices offer many advantages over those made from silicone elastomers, but bonding procedures must be developed for each thermoplastic of interest. Solvent bonding is a simple and versatile method that can be used to fabricate devices from a variety of plastics. An appropriate solvent is added between two device layers to be bonded, and heat and pressure are applied to the device to facilitate the bonding. By using an appropriate combination of solvent, plastic, heat, and pressure, the device can be sealed with a high quality bond, characterized as having high bond coverage, bond strength, optical clarity, durability over time, and low deformation or damage to microfeature geometry. We describe the procedure for bonding devices made from two popular thermoplastics, poly(methyl-methacrylate) (PMMA), and cyclo-olefin polymer (COP), as well as a variety of methods to characterize the quality of the resulting bonds, and strategies to troubleshoot low quality bonds. These methods can be used to develop new solvent bonding protocols for other plastic-solvent systems.

Solvent bonding is a simple and versatile method for fabricating thermoplastic microfluidic devices with high quality bonds. We describe a protocol to achieve strong, optically clear bonds in PMMA and COP microfluidic devices that preserve microfeature details, by a judicious combination of pressure, temperature, an appropriate solvent, and device geometry.

Thermoplastic microfluidic devices offer many advantages over those made from silicone elastomers, but bonding procedures must be developed for each ...

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and forging. Adoption of this technique is proceeding despite disagreement concerning the underlying mechanism responsible for EAD. The experimental procedure described herein enables a more explicit study compared to previous EAD research by removing thermal effects, which are responsible for disagreement in interpreting previous EAD results. Furthermore, as the procedure described here enables EAD observation in situ and in real time in a transmission electron microscope (TEM), it is superior to existing post-mortem methods that observe EAD effects post-test. Test samples consist of a single crystal copper (SCC) foil having a free-standing tensile test section of nanoscale thickness, fabricated using a combination of laser and ion beam milling. The SCC is mounted to an etched silicon base that provides mechanical support and electrical isolation while serving as a heat sink. Using this geometry, even at high current density (~3,500 A/mm2), the test section experiences a negligible temperature increase (&#60;0.02 &#176;C), thus eliminating Joule heating effects. Monitoring material deformation and identifying the corresponding changes to microstructures, e.g. dislocations, are accomplished by acquiring and analyzing a series of TEM images. Our sample preparation and in situ experiment procedures are robust and versatile as they can be readily utilized to test materials with different microstructures, e.g., single and polycrystalline copper.

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

Isolating electrical and thermal effects on electrically assisted deformation (EAD) is very difficult using macroscopic samples. Metallic sample micro- and nanostructures together with a custom test procedure have been developed to evaluate the impact of applied current on the formation without joule heating and evolution of dislocations on these samples.

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and ...

Fabrication of Magnetic Nanostructures on Silicon Nitride Membranes for Magnetic Vortex Studies Using Transmission Microscopy Techniques

Electron and x-ray magnetic microscopies allow for high-resolution magnetic imaging down to tens of nanometers. However, the samples need to be prepared on transparent membranes which are very fragile and difficult to manipulate. We present processes for the fabrication of samples with magnetic micro- and nanostructures with spin configurations forming magnetic vortices suitable for Lorentz transmission electron microscopy and magnetic transmission x-ray microscopy studies. The samples are prepared on silicon nitride membranes and the fabrication consists of a spin coating, UV and electron-beam lithography, the chemical development of the resist, and the evaporation of the magnetic material followed by a lift-off process forming the final magnetic structures. The samples for the Lorentz transmission electron microscopy consist of magnetic nanodiscs prepared in a single lithography step. The samples for the magnetic x-ray transmission microscopy are used for time-resolved magnetization dynamic experiments, and magnetic nanodiscs are placed on a waveguide which is used for the generation of repeatable magnetic field pulses by passing an electric current through the waveguide. The waveguide is created in an extra lithography step.

A protocol for the fabrication of magnetic micro- and nanostructures with spin configurations forming magnetic vortices suitable for transmission electron microscopy (TEM) and magnetic transmission x-ray microscopy (MTXM) studies is presented.

Electron and x-ray magnetic microscopies allow for high-resolution magnetic imaging down to tens of nanometers. However, the samples need to be prepared ...

Fabrication of Three-Dimensional Graphene-Based Polyhedrons via Origami-Like Self-Folding

The assembly of two-dimensional (2D) graphene into three-dimensional (3D) polyhedral structures while preserving the graphene's excellent inherent properties has been of great interest for the development of novel device applications. Here, fabrication of 3D, microscale, hollow polyhedrons (cubes) consisting of a few layers of 2D graphene or graphene oxide sheets via an origami-like self-folding process is described. This method involves the use of polymer frames and hinges, and aluminum oxide/chromium protection layers that reduce tensile, spatial, and surface tension stresses on the graphene-based membranes when the 2D nets are transformed into 3D cubes. The process offers control of the size and shape of the structures as well as parallel production. In addition, this approach allows the creation of surface modifications by metal patterning on each face of the 3D cubes. Raman spectroscopy studies show the method allows the preservation of the intrinsic properties of the graphene-based membranes, demonstrating the robustness of our method.

Fabrication of Three-Dimensional Graphene-Based Polyhedrons via Origami-Like Self-Folding

Here, we present a protocol for fabrication of 3D graphene-based polyhedrons via origami-like self-folding.

The assembly of two-dimensional (2D) graphene into three-dimensional (3D) polyhedral structures while preserving the graphene's excellent inherent ...

Fabrication of Robust Nanoscale Contact between a Silver Nanowire Electrode and CdS Buffer Layer in Cu(In,Ga)Se2 Thin-film Solar Cells

Silver nanowire transparent electrodes have been employed as window layers for Cu(In,Ga)Se2 thin-film solar cells. Bare silver nanowire electrodes normally result in very poor cell performance. Embedding or sandwiching silver nanowires using moderately conductive transparent materials, such as indium tin oxide or zinc oxide, can improve cell performance. However, the solution-processed matrix layers can cause a significant number of interfacial defects between transparent electrodes and the CdS buffer, which can eventually result in low cell performance. This manuscript describes how to fabricate robust electrical contact between a silver nanowire electrode and the underlying CdS buffer layer in a Cu(In,Ga)Se2 solar cell, enabling high cell performance using matrix-free silver nanowire transparent electrodes. The matrix-free silver nanowire electrode fabricated by our method proves that the charge-carrier collection capability of silver nanowire electrode-based cells is as good as that of standard cells with sputtered ZnO:Al/i-ZnO as long as the silver nanowires and CdS have high-quality electrical contact. The high-quality electrical contact was achieved by depositing an additional CdS layer as thin as 10 nm onto the silver nanowire surface.

Fabrication of Robust Nanoscale Contact between a Silver Nanowire Electrode and CdS Buffer Layer in CuIn,GaSe2 Thin-film Solar Cells

In this protocol, we describe the detailed experimental procedure for the fabrication of a robust nanoscale contact between a silver nanowire network and CdS buffer layer in a CIGS thin-film solar cell.