Name: preparation of large-area vertical 2d crystal hetero-structures through the sulfurization of transition metal films for device fabrication
Uploaded: 2017-11-28T13:00:00
Description: Watch this Scientific Journal Video about Preparation of Large-area Vertical 2D Crystal Hetero-structures Through the Sulfurization of Transition Metal Films for Device Fabrication at JoVE.com

This work was supported in part by projects MOST 105-2221-E-001-011-MY3 and MOST 105-2622-8-002-001 funded by the Ministry of Science and Technology, Taiwan, and in part by the focused project funded by the Research Center for Applied Sciences, Academia Sinica, Taiwan.

1. Growth of Individual 2D material (MoS2 and WS2)
<ol>
	<li>Transition metal deposition using an RF sputtering system
	<ol>
		<li>A clean 2 x 2 cm2 sapphire substrate is placed on the sample holder with the polished side toward the targets of the sputtering system for the transition metal deposition. Sapphire substrates are chosen due to sapphire&#39;s chemical stability at high temperatures and atomic-flat surfaces.</li>
		<li>Pump down the sputtering chamber to 3 x 1...

<ol>
	<li>Moldt, T., 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=High-Yield+Production+and+Transfer+of+Graphene+Flakes+Obtained+by+Anodic+Bonding.">High-Yield Production and Transfer of Graphene Flakes Obtained by Anodic Bonding.</a> ACS Nano. 5, 7700-7706 (2011).</li><li>Choi, W., 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=High-Detectivity+Multilayer+MoS2+Phototransistors+with+Spectral+Response+from+Ultraviolet+to+Infrared.">High-Detectivity Multilayer MoS2 Phototransistors with Spectral Response from Ultraviolet to Infrared.</a> Adv. Mater. 24, 5832-5836 (2012).</li><li>Liu, H., Neal, A. T., Ye, P. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Channel+Length+Scaling+of+MoS2+MOSFETs.">Channel Length Scaling of MoS2 MOSFETs.</a> ACS Nano. 6, 8563-8569 (2012).</li><li>Wang, Q. H., Kalantar-Zadeh, K., Kis, A., Coleman, J. N., Strano, M. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electronics+and+optoelectronics+of+two-dimensional+transition+metal+dichalcogenides.">Electronics and optoelectronics of two-dimensional transition metal dichalcogenides.</a> Nat. Nanotechnol. 7, 699-712 (2012).</li><li>Radisavljevic, B., Radenovic, A., Brivio, J., Giacometti, V., Kis, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Single-layer+MoS2+transistors.">Single-layer MoS2 transistors.</a> Nat. Nanotechnol. 6, 147-150 (2011).</li><li>Lee, Y. H., 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=Synthesis+of+Large-Area+MoS2+Atomic+Layers+with+Chemical+Vapor+Deposition.">Synthesis of Large-Area MoS2 Atomic Layers with Chemical Vapor Deposition.</a> Adv. Mater. 24, 2320-2325 (2012).</li><li>Yu, Y., Li, C., Liu, Y., Su, L., Zhang, Y., Cao, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Controlled+Scalable+Synthesis+of+Uniform,+High-Quality+Monolayer+and+Few-layer+MoS2+Films.">Controlled Scalable Synthesis of Uniform, High-Quality Monolayer and Few-layer MoS2 Films.</a> Sci. Rep. 3, 1866 (2013).</li><li>Ling, X., 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=Role+of+the+Seeding+Promoter+in+MoS2+Growth+by+Chemical+Vapor+Deposition.">Role of the Seeding Promoter in MoS2 Growth by Chemical Vapor Deposition.</a> Nano Lett. 14, 464-472 (2014).</li><li>Lee, Y., 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=Synthesis+of+wafer-scale+uniform+molybdenum+disulfide+films+with+control+over+the+layer+number+using+a+gas+phase+sulfur+precursor.">Synthesis of wafer-scale uniform molybdenum disulfide films with control over the layer number using a gas phase sulfur precursor.</a> Nanoscale. 6, 2821-2826 (2014).</li><li>Lin, M. Y., Su, C. F., Lee, S. C., Lin, S. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Growth+Mechanisms+of+Graphene+Directly+on+Sapphire+Substrates+using+the+Chemical+Vapor+Deposition.">The Growth Mechanisms of Graphene Directly on Sapphire Substrates using the Chemical Vapor Deposition.</a> J. Appl. Phys. 115, 223510 (2014).</li><li>Wu, C. R., Chang, X. R., Chang, S. W., Chang, C. E., Wu, C. H., Lin, S. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multilayer+MoS2+prepared+by+one-time+and+repeated+chemical+vapor+depositions:+anomalous+Raman+shifts+and+transistors+with+high+ON/OFF+ratio.">Multilayer MoS2 prepared by one-time and repeated chemical vapor depositions: anomalous Raman shifts and transistors with high ON/OFF ratio.</a> J. Phys. D Appl. Phys. 48, 435101 (2015).</li><li>Li, M. Y., 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=Epitaxial+growth+of+a+monolayer+WSe2-MoS2+lateral+p-n+junction+with+an+atomically+sharp+interface.">Epitaxial growth of a monolayer WSe2-MoS2 lateral p-n junction with an atomically sharp interface.</a> Science. 349, 524-528 (2015).</li><li>Zhan, Y., Liu, Z., Najmaei, S., Ajayan, M. P., Lou, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Large-area+vapor-phase+growth+and+characterization+of+MoS2+atomic+layers+on+a+SiO2+substrate.">Large-area vapor-phase growth and characterization of MoS2 atomic layers on a SiO2 substrate.</a> Small. 8, 966 (2012).</li><li>Woods, J. 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=One-Step+Synthesis+of+MoS2/WS2+Layered+Heterostructures+and+Catalytic+Activity+of+Defective+Transition+Metal+Dichalcogenide+Films.">One-Step Synthesis of MoS2/WS2 Layered Heterostructures and Catalytic Activity of Defective Transition Metal Dichalcogenide Films.</a> ACS Nano. 10, 2004-2009 (2016).</li><li>Wu, C. R., Chang, X. R., Wu, C. H., Lin, S. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Growth+Mechanism+of+Transition+Metal+Dichalcogenides+using+Sulfurization+of+Pre-deposited+Transition+Metals+and+the+2D+Crystal+Hetero-structure+Establishment.">The Growth Mechanism of Transition Metal Dichalcogenides using Sulfurization of Pre-deposited Transition Metals and the 2D Crystal Hetero-structure Establishment.</a> Sci. Rep. 7, 42146 (2017).</li><li>Chen, K. C., Chu, T. W., Wu, C. R., Lee, S. C., Lin, S. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Layer+Number+Controllability+of+Transition-metal+Dichalcogenides+and+The+Establishment+of+Hetero-structures+using+Sulfurization+of+Thin+Transition+Metal+Films.">Layer Number Controllability of Transition-metal Dichalcogenides and The Establishment of Hetero-structures using Sulfurization of Thin Transition Metal Films.</a> J. of Phys. D: Appl. Phy. 50, 064001 (2017).</li><li>Wu, C. R., Chang, X. R., Chu, T. W., Chen, H. A., Wu, C. H., Lin, S. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Establishment+of+2D+Crystal+Heterostructures+by+Sulfurization+of+Sequential+Transition+Metal+Depositions:+Preparation,+Characterization,+and+Selective+Growth.">Establishment of 2D Crystal Heterostructures by Sulfurization of Sequential Transition Metal Depositions: Preparation, Characterization, and Selective Growth.</a> Nano Lett. 16, 7093-7097 (2016).</li><li>Lin, M. Y., 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=Toward+epitaxially+grown+two-dimensional+crystal+hetero-structures:+Single+and+double+MoS2/graphene+hetero-structures+by+chemical+vapor+depositions.">Toward epitaxially grown two-dimensional crystal hetero-structures: Single and double MoS2/graphene hetero-structures by chemical vapor depositions.</a> Appl. Phys. Lett. 105, 073501 (2014).</li><li>Lee, C., Yan, H., Brus, L. E., Heinz, T. F., Hone, J., Ryu, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Anomalous+Lattice+Vibrations+of+Single+and+Few-Layer+MoS2.">Anomalous Lattice Vibrations of Single and Few-Layer MoS2.</a> ACS Nano. 4, 2695-2700 (2010).</li><li>Chen, K. C., Chu, T. W., Wu, C. R., Lee, S. C., Lin, S. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atomic+Layer+Etchings+of+Transition+Metal+Dichalcogenides+with+Post+Healing+Procedures:+Equivalent+Selective+Etching+of+2D+Crystal+Hetero-structures.">Atomic Layer Etchings of Transition Metal Dichalcogenides with Post Healing Procedures: Equivalent Selective Etching of 2D Crystal Hetero-structures.</a> 2D Mater. 4, 034001 (2017).</li></ol>

Compared with conventional semiconductor materials such as Si and GaAs, the advantage of 2D materials for device applications lies in the possibility of device fabrication with very thin bodies down to several atomic layers. When the Si industry advances into the &#60;10 nm technology node, the high aspect ratio of Si fin FET will make the device architecture unsuitable for practical applications. Thus, 2D materials have emerged due to their potential to replace Si for electronic device applications.
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One of the most common approaches to obtain 2D crystal films is using mechanical exfoliation from bulk materials1,2,3,4,5. Although 2D crystal films with high crystalline quality can be easily obtained using this method, scalable 2D crystal films are not available through this approach, which is disadvantageous for practical applications. It has been demonstrated in previous publications that using chemical vapor deposition (CVD), large-area and uniform 2D crystal films can be prepared6,7,8,9. Direct growth of graphene on sapphire substrates and layer-number-controllable MoS2 films prepared by repeating the same growth cycle are also demonstrated using the CVD growth technique10,11. In one recent publication, in-plane WSe2/MoS2 hetero-structure flakes are also fabricated using the CVD growth technique12. Although the CVD growth technique is promising in providing scalable 2D crystal films, the major disadvantage of this growth technique is that different precursors have to be located for different 2D crystals. The growth conditions also vary between different 2D crystals. In this case, the growth procedures will become more complicated when demand grows for 2D crystal hetero-structures.
Compared with the CVD growth technique, the sulfurization of pre-deposited transition metal films has provided a similar but much simpler growth approach for TMDs13,14. Since the growth procedure involves only metal deposition and the following sulfurization procedure, it is possible to grow different TMDs through the same growth procedures. On the other hand, the layer number controllability of the 2D crystals may also be achieved by changing the pre-deposited transition metal thicknesses. In this case, growth optimization and layer number control down to a single layer are required for different TMDs. Understanding growth mechanisms is also very important for the establishment of complicated TMD hetero-structures using this method.
In this paper, MoS2 and WS2 films are prepared under similar growth procedures of the metal deposition followed by the sulfurization procedure. With the results obtained from the sulfurization of Mo films under sulfur sufficient and deficient conditions, two growth mechanisms are observed during the sulfurization procedure15. Under the sulfur sufficient condition, a uniform and layer-number-controllable MoS2 film can be obtained after the sulfurization procedure. When the sample is sulfurized under the sulfur deficient condition, the background sulfur is not sufficient to form a complete MoS2 film such that the Mo oxide segregation and coalescence will be the dominant mechanism at the early growth stage. A sample with Mo oxide clusters covered by few layers of MoS2 will be obtained after the sulfurization procedure15. Through sequential metal deposition and following sulfurization procedures, WS2/MoS2 vertical hetero-structures with layer number controllability down to a single layer can be prepared15,16. Using this technique, a sample is obtained on a single sapphire substrate with four regions: (I) blank sapphire substrate, (II) standalone MoS2, (III) WS2/MoS2 hetero-structure, and (IV) standalone WS217. The results demonstrate that the growth technique is advantageous for the establishment of vertical 2D crystal hetero-structure and is capable of selective growth. The enhanced device performances of 2D crystal hetero-structures will mark the first step toward practical applications for 2D crystals.

<table>
	<tbody>
		<tr>
			<td>RF sputtering system</td>
			<td>Kao Duen Technology</td>
			<td>N/A</td>
			<td></td>
		</tr>
		<tr>
			<td>Furnace for sulfurization</td>
			<td>Creating Nano Technologies</td>
			<td>N/A</td>
			<td></td>
		</tr>
		<tr>
			<td>Polymethyl methacrylate (PMMA)</td>
			<td>Microchem</td>
			<td>8110788</td>
			<td>Flammable</td>
		</tr>
		<tr>
			<td>KOH, &#62; 85%</td>
			<td>Sigma-Aldrich</td>
			<td>30603</td>
			<td></td>
		</tr>
		<tr>
			<td>Acetone, 99.5%</td>
			<td>Echo Chemical</td>
			<td>CMOS110</td>
			<td></td>
		</tr>
		<tr>
			<td>Sulfur (S), 99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>13803</td>
			<td></td>
		</tr>
		<tr>
			<td>Molybdenum (Mo), 99.95%</td>
			<td>Summit-Tech</td>
			<td>N/A</td>
			<td></td>
		</tr>
		<tr>
			<td>Tungsten (W), 99.95%</td>
			<td>Summit-Tech</td>
			<td>N/A</td>
			<td></td>
		</tr>
		<tr>
			<td>C-plane Sapphire substrate</td>
			<td>Summit-Tech</td>
			<td>X171999</td>
			<td>(0001) &#177; 0.2 &#176; one side polished</td>
		</tr>
		<tr>
			<td>300 nm SiO2/Si substrate</td>
			<td>Summit-Tech</td>
			<td>2YCDDM</td>
			<td>P-type Si substrate, resistivity: 1-10 &#937; &#183; cm.</td>
		</tr>
		<tr>
			<td>Sample holder (sputtering system)</td>
			<td>Kao Duen Technology</td>
			<td>N/A</td>
			<td>Ceramic material</td>
		</tr>
		<tr>
			<td>Mechanical pump (sputtering system)</td>
			<td>Ulvac</td>
			<td>D-330DK</td>
			<td></td>
		</tr>
		<tr>
			<td>Diffusion pump (sputtering system)</td>
			<td>Ulvac</td>
			<td>ULK-06A</td>
			<td></td>
		</tr>
		<tr>
			<td>Mass flow controller</td>
			<td>Brooks</td>
			<td>5850E</td>
			<td>The maximum Argon flow is 400 mL/min</td>
		</tr>
		<tr>
			<td>Manual wheel Angle poppet valve</td>
			<td>King Lai</td>
			<td>N/A</td>
			<td>Vacuum range from 2500 ~1 &#215; 10-8 torr</td>
		</tr>
		<tr>
			<td>Raman measurement system</td>
			<td>Horiba</td>
			<td>Jobin Yvon LabRAM HR800</td>
			<td></td>
		</tr>
		<tr>
			<td>Transmission electron microscopy</td>
			<td>Fei</td>
			<td>Tecnai G2 F20</td>
			<td></td>
		</tr>
		<tr>
			<td>Petri dish</td>
			<td>Kwo Yi</td>
			<td>N/A</td>
			<td></td>
		</tr>
		<tr>
			<td>Tweezer</td>
			<td>Venus</td>
			<td>2A</td>
			<td></td>
		</tr>
		<tr>
			<td>Digital dry cabinet</td>
			<td>Jwo Ruey Technical</td>
			<td>DRY-60</td>
			<td></td>
		</tr>
		<tr>
			<td>Dual-channel system sourcemeter</td>
			<td>Keithley</td>
			<td>2636B</td>
			<td></td>
		</tr>
	</tbody>
</table>

preparation of large-area vertical 2d crystal hetero-structures through the sulfurization of transition metal films for device fabrication

We have demonstrated that through the sulfurization of transition metal films such as molybdenum (Mo) and tungsten (W), large-area and uniform transition metal dichalcogenides (TMDs) MoS2 and WS2 can be prepared on sapphire substrates. By controlling the metal film thicknesses, good layer number controllability, down to a single layer of TMDs, can be obtained using this growth technique. Based on the results obtained from the Mo film sulfurized under the sulfur deficient condition, there are two mechanisms of (a) planar MoS2 growth and (b) Mo oxide segregation observed during the sulfurization procedure. When the background sulfur is sufficient, planar TMD growth is the dominant growth mechanism, which will result in a uniform MoS2 film after the sulfurization procedure. If the background sulfur is deficient, Mo oxide segregation will be the dominant growth mechanism at the initial stage of the sulfurization procedure. In this case, the sample with Mo oxide clusters covered with few-layer MoS2 will be obtained. After sequential Mo deposition/sulfurization and W deposition/sulfurization procedures, vertical WS2/MoS2 hetero-structures are established using this growth technique. Raman peaks corresponding to WS2 and MoS2, respectively, and the identical layer number of the hetero-structure with the summation of individual 2D materials have confirmed the successful establishment of the vertical 2D crystal hetero-structure. After transferring the WS2/MoS2 film onto a SiO2/Si substrate with pre-patterned source/drain electrodes, a bottom-gate transistor is fabricated. Compared with the transistor with only MoS2 channels, the higher drain currents of the device with the WS2/MoS2 hetero-structure have exhibited that with the introduction of 2D crystal hetero-structures, superior device performance can be obtained. The results have revealed the potential of this growth technique for the practical application of 2D crystals.

The Raman spectrum and the cross-sectional HRTEM images of individual MoS2 and WS2 fabricated using the sulfurization of pre-deposited transition metals are shown in Figure 1a-b17, respectively. Two characteristic Raman peaks are observed for both MoS2 and WS2, which correspond to in-plane <img alt="Equation 1" src="/files/ftp_upload/56494/56494eq1.jpg" /> and out-of-plane A<...

Watch this Scientific Journal Video about Preparation of Large-area Vertical 2D Crystal Hetero-structures Through the Sulfurization of Transition Metal Films for Device Fabrication at JoVE.com

Preparation of Large-area Vertical 2D Crystal Hetero-structures Through the Sulfurization of Transition Metal Films for Device Fabrication

Through the sulfurization of pre-deposited transition metals, large-area and vertical 2D crystal hetero-structures can be fabricated. The film transferring and device fabrication procedures are also demonstrated in this report.

We have demonstrated that through the sulfurization of transition metal films such as molybdenum (Mo) and tungsten (W), large-area and uniform transition ...

The overall goal of this growth technique is to establish complex vertical 2D crystal heterostructures, with good control over the number of 2D layers, using similar growth procedures for each material. The main advantage of this simple technique is that it uses similar growth procedures for different 2D materials and it has good layer number controllability. This technique can help investigate practical applications of vertical 2D material heterostructures as it can produce larger vertical 2D crystal heterostructures with enhanced transitor properties compared to single material structures.To begin the procedure, mount a clean C-plane two centimeter by two centimeter sapphire substrate on the sample stage of an RF sputtering system, with the polished side facing the molybdenum target. Pump down the sample chamber to three times 10 to the negative six tores. Inject argon gas into the system at 40 milliliters per minute and ensure that the chamber pressure is stable at five times 10 to the negative two tores.Ignite the plasma, and set the power output to 40 watts. Reduce the chamber pressure to five times 10 to the negative three tores. Then, manually open the molybdenum target shutter and deposit the metal for 30 seconds.Ensure that the power output remains constant throughout deposition. When sputtering has finished, place the substrate in a quart sample holder with the metal film facing up. Set the substrate in the center of the heating zone of a calibrated tube furnace.Place 1.5 grams of sulfur powder in a alumina heating boat. Place the boat two centimeters upstream of the heating zone so that the sulfur temperature will be 120 degrees Celsius when the substrate reaches 800 degrees Celsius. Close and pump down the furnace to five times 10 to the negative three tores.Then, flow argon gas through the furnace at 130 milliliters per minute. Ensure that the furnace pressure stabilizes at 0.7 tores. Ramp the furnace from room temperature to 800 degrees Celsius at 20 degrees Celsius per minute.Hold the furnace at 800 degrees Celsius until the sulfur has fully evaporated. Then, turn off the furnace heat and allow the substrate to cool to room temperature under a flow of argon. Next, mount the substrate in the RF sputtering system with the molybdenum disulfide film facing the tungsten target.Sputter tungsten on the substrate for 30 seconds using the same settings as for molybdenum. Place the tungsten-coated substrate in the center of the furnace heating zone and one gram of sulfur powder two centimeters upstream of the heating zone. Sulfurize the tungsten film using the same parameters as for the molybdenum film.To begin the thin film transfer, spin coat three drops of polymethyl methacrylate on a prepared transition metal dichalcogenide film for 10 seconds each at 500 and 800 rotations per minute. Cure the PMMA at 120 degrees Celsius for five minutes. Then, place the PMMA-coated substrate in a Petri dish filled with deionized water.Use tweezers with round, flat tips to carefully peel one corner of the PMMA with the attached TMD film from the substrate. Transfer the substrate to a one molar aqueous potassium hydroxide solution heated to 100 degrees Celsius. Slowly and carefully peel the entire PMMA TMD film from the substrate using tweezers.Scoop up the PMMA TMD film from the potassium hydroxide solution with another clean sapphire substrate with the polished side facing the film. Transfer the film to a beaker of deionized water. Transfer the film to fresh deionized water three more times in the same way, to ensure that residual potassium hydroxide is completely removed.Next, obtain a 300 nanometer thick P type silicon dioxide on silicon substrate patterned with titanium or gold electrodes. Immerse the patterned substrate in the final beaker of deionized water and carefully attach the TMD film to the substrate. Bake the substrate with the attached film at 100 degrees Celsius for three minutes to evaporate the water.Cover the substrate surface with PMMA to ensure that the film is firmly attached to the substrate. Dry the substrate in an electronic drying cabinet for eight hours. Then, remove the PMMA layer and use photolithography and reactive ion etching to fabricate a TMD heterostructure transistor.The molybdenum sulfurization mechanism was examined with HRTEM. Under sulfur rich conditions, the sulfur rapidly replaced the oxygen of molybdenum oxides, eventually forming a uniform film with a controllable number of layers. Molybdenum oxide segregation and coalescence was the dominant early growth mechanism in sulfur deficient conditions.Raman spectroscopy of individual molybdenum disulfide and tungsten disulfide films each showed two characteristic peaks. HRTEM showed five molybdenum disulfide layers and four tungsten disulfide layers. Sequential metal deposition resulted in a tungsten disulfide molybdenum disulfide vertical heterostructure.Both sets of characteristic peaks were apparent in the Ramen spectrum. The formation of a vertical TMD heterostructure was supported by repeated atomic etching of individual tungsten disulfide layers until only molybdenum disulfide remained. A transistor fabricated with a tungsten disulfide molybdenum disulfide single heterostructure showed a substantially greater drain current when compared to a transistor fabricated with only molybdenum disulfide.The single heterostructure transistor had a higher field effect mobility value, which could have been the result of electron injection from tungsten disulfide to molybdenum disulfide and from channels with higher electron concentrations under thermal equilibrium. After watching this video, you should have a good understanding of how to use a equipment and procedures shown to easily establish vertical 2D material heterostructures for different device applications. When using this protocol, you should only need to optimize the sputtering powers, the position times and separation temperatures for your equipment to obtain high quality 2D materials and heterostructures.

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Engineering

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 ...

Fabrication of Low Temperature Carbon Nanotube Vertical Interconnects Compatible with Semiconductor Technology

We demonstrate a method for the low temperature growth (350 &#176;C) of vertically-aligned carbon nanotubes (CNT) bundles on electrically conductive thin-films. Due to the low growth temperature, the process allows integration with modern low-&#954; dielectrics and some flexible substrates. The process is compatible with standard semiconductor fabrication, and a method for the fabrication of electrical 4-point probe test structures for vertical interconnect test structures is presented. Using scanning electron microscopy the morphology of the CNT bundles is investigated, which demonstrates vertical alignment of the CNT and can be used to tune the CNT growth time. With Raman spectroscopy the crystallinity of the CNT is investigated. It was found that the CNT have many defects, due to the low growth temperature. The electrical current-voltage measurements of the test vertical interconnects displays a linear response, indicating good ohmic contact was achieved between the CNT bundle and the top and bottom metal electrodes. The obtained resistivities of the CNT bundle are among the average values in the literature, while a record-low CNT growth temperature was used.

A method for the growth of low temperature vertically-aligned carbon nanotubes, and the subsequent fabrication of vertical interconnect electrical test structures using semiconductor fabrication is presented.

We demonstrate a method for the low temperature growth (350 &#176;C) of vertically-aligned carbon nanotubes (CNT) bundles on electrically conductive ...

Preparation of Liquid-exfoliated Transition Metal Dichalcogenide Nanosheets with Controlled Size and Thickness: A State of the Art Protocol

We summarize recent advances in the production of liquid-exfoliated transition metal dichalcogenide (TMD) nanosheets with controlled size and thickness. Layered crystals of molybdenum disulphide (MoS2) and tungsten disulphide (WS2) are exfoliated in aqueous surfactant solution by sonication. This yields highly polydisperse mixtures containing nanosheets with broad size and thickness distributions. However, for most purposes, specific sizes (in terms of both lateral dimension and thickness) are required. For example, large and thin nanosheets are desired for (opto) electronic applications, while laterally small nanosheets are interesting for catalytic applications. Therefore, post-exfoliation size selection is an important step that we address here. We provide a detailed protocol on the efficient size selection in large quantities by liquid cascade centrifugation and the size and thickness quantification by statistical microscopic analysis (atomic force microscopy and transmission electron microscopy). The comparison of MoS2 and WS2 shows that both materials are size-selected in a similar way by the same procedure. Importantly, the dispersions of size-selected nanosheets show systematic changes in their optical extinction spectra with size due to edge and confinement effects. We show how these optical changes are related quantitatively to the nanosheets dimensions and describe how mean nanosheets length and layer number can be extracted reliably from the extinction spectra. The exfoliation and size selection protocol can be applied to a broad range of layered crystals as we have previously demonstrated for graphene, gallium sulphide (GaS) and black phosphorus.

A protocol for the liquid exfoliation of layered materials to nanosheets, their size selection and size measurement by microscopic and spectroscopic techniques is presented.

We summarize recent advances in the production of liquid-exfoliated transition metal dichalcogenide (TMD) nanosheets with controlled size and thickness. ...

Fabrication of 1-D Photonic Crystal Cavity on a Nanofiber Using Femtosecond Laser-induced Ablation

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using femtosecond laser-induced ablation. We show that thousands of periodic nano-craters are fabricated on an optical nanofiber by irradiating with just a single femtosecond laser pulse. For a typical sample, periodic nano-craters with a period of 350 nm and with diameter gradually varying from 50 - 250 nm over a length of 1 mm are fabricated on a nanofiber with diameter around 450 - 550 nm. A key aspect of such a nanofabrication is that the nanofiber itself acts as a cylindrical lens and focuses the femtosecond laser beam on its shadow surface. Moreover, the single-shot fabrication makes it immune to mechanical instabilities and other fabrication imperfections. Such periodic nano-craters on nanofiber, act as a 1-D PhC and enable strong and broadband reflection while maintaining the high transmission out of the stopband. We also present a method to control the profile of the nano-crater array to fabricate apodized and defect-induced PhC cavities on the nanofiber. The strong confinement of the field, both transverse and longitudinal, in the nanofiber-based PhC cavities and the efficient integration to the fiber networks, may open new possibilities for nanophotonic applications and quantum information science.

We present a protocol for fabricating 1-D photonic crystal cavities on subwavelength diameter silica fibers (optical nanofibers) using femtosecond laser-induced ablation.

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using ...

Orientational Transition in a Liquid Crystal Triggered by the Thermodynamic Growth of Interfacial Wetting Sheets

In liquid crystal (LC) physical chemistry, molecules near the surface play a great role in controlling bulk orientation. Thus far, mainly to achieve desired molecular orientation states in LC displays, the "static" surface property of LCs, so-called surface anchoring, has been intensively studied. As a rule of thumb, once the initial orientation of LCs is "locked" by specific surface treatments, such as rubbing or treatment with a specific alignment layer, it hardly changes with temperature. Here, we present a system exhibiting an orientational transition upon temperature variation, which conflicts with the consensus. Right on the transition, the bulk LC molecules experience the orientational rotation, with 90&#176; between the planar (P) orientation at high temperatures and the vertical (V) orientation at low temperatures in the first-order transitional manner. We have tracked thermodynamic surface anchoring behavior by means of polarizing optical microscopy (POM), dielectric spectroscopy (DS), high-resolution differential scanning calorimetry (HR-DSC), and grazing incidence X-ray diffraction (GI-XRD) and reached a plausible physical explanation: that the transition is triggered by a growth of surface wetting sheets, which impose the V orientation locally against the P orientation in the bulk. This landscape would provide a general link explaining how the equilibrium bulk orientation is affected by surface-localized orientation in many LC systems. In our characterization, POM and DS are advantageous by offering information on the spatial distribution of the orientation of LC molecules. HR-DSC gives information about the precise thermodynamic information on transitions, which cannot be addressed by conventional DSC instruments due to limited resolution. GI-XRD provides information on surface-specific molecular orientation and short-range orderings. The goal of this paper is to present a protocol for preparing a sample that exhibits the transition and to demonstrate how the thermodynamic structural variation, both in the bulk and on surfaces, can be analyzed through the abovementioned methods.

Here, we present a protocol to trigger an orientational transition of a liquid crystal in response to temperature. Methodologies are described for preparing a sample in order to observe the transition and the detailed transitional evolution.

In liquid crystal (LC) physical chemistry, molecules near the surface play a great role in controlling bulk orientation. Thus far, mainly to achieve ...

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

A strategy based on doped liquid crystalline networks is described to create mechanical self-sustained oscillations of plastic films under continuous light irradiation. The photo-excitation of dopants that can quickly dissipate light into heat, coupled with anisotropic thermal expansion and self-shadowing of the film, gives rise to the self-sustained deformation. The oscillations observed are influenced by the dimensions and the modulus of the film, and by the directionality and intensity of the light. The system developed offers applications in energy conversion and harvesting for soft-robotics and automated systems.
The general method described here consists of creating free-standing liquid crystalline films and characterizing the mechanical and thermal effects observed. The molecular alignment is achieved using alignment layers (rubbed polyimide), commonly used in the display manufacturing industry. To obtain actuators with large deformation, the mesogens are aligned and polymerized in a splay/bend configuration, i.e., with the director of the liquid crystals (LCs) going gradually from planar to homeotropic through the film thickness. Upon irradiation, the mechanical and thermal oscillations obtained are monitored with a high-speed camera. The results are further quantified by image analysis using an image processing program.

The goal of the protocol is to create liquid crystalline polymer films that can mechanically oscillate under continuous light irradiation. We describe in great detail the conception of free-standing films, from the liquid crystal alignment method to the photo-actuation. The experimental protocol applied to prepare this material is broadly applicable.

A strategy based on doped liquid crystalline networks is described to create mechanical self-sustained oscillations of plastic films under continuous ...

Fabrication of Ultra-thin Color Films with Highly Absorbing Media Using Oblique Angle Deposition

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present an advanced method for fabricating ultra-thin color films with improved characteristics. The proposed process addresses several fabrication issues, including large area processing. Specifically, the protocol describes a process for fabricating ultra-thin color films using an electron beam evaporator for oblique angle deposition of germanium (Ge) and gold (Au) on silicon (Si) substrates.&#160; Film porosity produced by the oblique angle deposition induces color changes in the ultra-thin film. The degree of color change depends on factors such as deposition angle and film thickness. Fabricated samples of the ultra-thin color films showed improved color tunability and color purity. In addition, the measured reflectance of the fabricated samples was converted into chromatic values and analyzed in terms of color. Our ultra-thin film fabricating method is expected to be used for various ultra-thin film applications such as flexible color electrodes, thin film solar cells, and optical filters. Also, the process developed here for analyzing the color of the fabricated samples is broadly useful for studying various color structures.

We present a detailed method for fabricating ultra-thin color films with improved characteristics for optical coatings. The oblique angle deposition technique using an electron beam evaporator allows improved color tunability and purity. Fabricated films of Ge and Au on Si substrates were analyzed by reflectance measurements and color information conversion.

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present ...

Atmospheric Pressure Fabrication of Large-Sized Single-Layer Rectangular SnSe Flakes

Tin selenide (SnSe) belongs to the family of layered metal chalcogenide materials with a buckled structure like phosphorene, and has shown potential for applications in two-dimensional nanoelectronics devices. Although many methods to synthesize SnSe nanocrystals have been developed, a simple way to fabricate large-sized single-layer SnSe flakes remains a great challenge. Herein, we show the experimental method to directly grow large-sized single-layer rectangular SnSe flakes on commonly used SiO2/Si insulating substrates using a straightforward two-step fabrication method in an atmospheric pressure quartz tube furnace system. The single-layer rectangular SnSe flakes with an average thickness of ~6.8 &#197; and lateral dimensions of about 30 &#181;m &#215; 50 &#181;m were fabricated by a combination of vapor transport deposition technique and nitrogen etching route. We characterized the morphology, microstructure, and electrical properties of the rectangular SnSe flakes and obtained excellent crystallinity and good electronic properties. This article about the two-step fabrication method can help researchers grow other similar two-dimensional, large-sized, single-layer materials using an atmospheric pressure system.

A protocol is presented demonstrating a two-step fabrication technique to grow large-sized single-layer rectangular shaped SnSe flakes on low-cost SiO2/Si dielectrics wafers in an atmospheric pressure quartz tube furnace system.

Tin selenide (SnSe) belongs to the family of layered metal chalcogenide materials with a buckled structure like phosphorene, and has shown potential for ...

Fabrication of Superhydrophobic Metal Surfaces for Anti-Icing Applications

Several ways to produce superhydrophobic metal surfaces are presented in this work. Aluminum was chosen as the metal substrate due to its wide use in industry. The wettability of the produced surface was analyzed by bouncing drop experiments and the topography was analyzed by confocal microscopy. In addition, we show various methodologies to measure its durability and anti-icing properties. Superhydrophobic surfaces hold a special texture that must be preserved to keep their water-repellency. To fabricate durable surfaces, we followed two strategies to incorporate a resistant texture. The first strategy is a direct incorporation of roughness to the metal substrate by acid etching. After this surface texturization, the surface energy was decreased by silanization or fluoropolymer deposition. The second strategy is the growth of a ceria layer (after surface texturization) that should enhance the surface hardness and corrosion resistance. The surface energy was decreased with a stearic acid film.
The durability of the superhydrophobic surfaces was examined by a particle impact test, mechanical wear by lateral abrasion, and UV-ozone resistance. The anti-icing properties were explored by studying the ability to repeal subcooled water, freezing delay, and ice adhesion.

We illustrate several methodologies to produce superhydrophobic metal surfaces and to explore their durability and anti-icing properties.

Several ways to produce superhydrophobic metal surfaces are presented in this work. Aluminum was chosen as the metal substrate due to its wide use in ...

Fused Filament Fabrication (FFF) of Metal-Ceramic Components

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with diverse customization options and favorable production methods is increasing continuously. With fused filament fabrication (FFF), it is possible to produce large and complex components quickly with high material efficiency. In FFF, a continuous thermoplastic filament is melted in a heated nozzle and deposited below. The computer-controlled print head is moved in order to build up the desired shape layer by layer. Investigations regarding printing of metals or ceramics are increasing more and more in research and industry. This study focuses on additive manufacturing (AM) with a multi-material approach to combine a metal (stainless steel) with a technical ceramic (zirconia: ZrO2). Combining these materials offers a broad variety of applications due to their different electrical and mechanical properties. The paper shows the main issues in preparation of the material and feedstock, device development, and printing of these composites.

Fused Filament Fabrication FFF of Metal-Ceramic Components

This study shows multi-material additive manufacturing (AM) using fused filament fabrication (FFF) of stainless steel and zirconia.

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with ...