Name: advanced experimental methods for low-temperature magnetotransport measurement of novel materials
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Description: Watch this Scientific Journal Video about Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials at JoVE.com

This work is supported by the National Institute of Standards and Technology of the United States Department of Commerce.

1. Preparation of Substrate
<ol>
	<li>Obtain 4 inch silicon (Si) wafer composed of heavily-doped p-doped Si covered by approximately 300 nm of SiO2. This substrate structure will allow the substrate to serve as a back gate.</li>
	<li>Using drafting/design software, design a 1 cm &#215; 1 cm pattern with evenly spaced features, such as enumerated crosses, in the x and y direction to use as positional locators on the substrate for transferred sample flakes and alignment marks for electron beam lithography (<st...

<ol>
	<li>Doty, F. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Properties+of+CdZnTe+crystals+grown+by+a+high+pressure+Bridgman+method.">Properties of CdZnTe crystals grown by a high pressure Bridgman method.</a> Journal of Vacuum Science &amp; Technology B. 10 (4), 1418-1422 (1992).</li><li>Ikesue, A., Kinoshita, T., Kamata, K., Yoshida, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fabrication+and+optical+properties+of+high-performance+polycrystalline+Nd-YAG+Ceramics+for+Solid-State+Lasers.">Fabrication and optical properties of high-performance polycrystalline Nd-YAG Ceramics for Solid-State Lasers.</a> Journal of the American Ceramic Society. 78 (4), 1033-1040 (1995).</li><li>Elwell, D., Scheel, H. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Crystal Growth From High-Temperature Solutions. , (2011).</li><li>Doty, F. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Properties+of+CdZnTe+crystals+grown+by+a+high+pressure+Bridgman+method.">Properties of CdZnTe crystals grown by a high pressure Bridgman method.</a> Journal of Vacuum Science &amp; Technology B. 10 (4), 1418-1422 (1992).</li><li>Ikesue, A., Kinoshita, T., Kamata, K., Yoshida, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fabrication+and+optical+properties+of+high-performance+polycrystalline+Nd-YAG+Ceramics+for+Solid-State+Lasers.">Fabrication and optical properties of high-performance polycrystalline Nd-YAG Ceramics for Solid-State Lasers.</a> Journal of the American Ceramic Society. 78 (4), 1033-1040 (1995).</li><li>Elwell, D., Scheel, H. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Crystal Growth From High-Temperature Solutions. , (2011).</li><li>Therese, G. H. A., Kamath, P. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+Synthesis+of+Metal+Oxides+and+Hydroxides.">Electrochemical Synthesis of Metal Oxides and Hydroxides.</a> Chemistry of Materials. 12, 1195-1294 (2000).</li><li>Capper, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bulk+Crystal+Growth+-+Methods+and+Materials.">Bulk Crystal Growth - Methods and Materials.</a> Handbook of Electronic and Photonic Materials. , 231-254 (2007).</li><li>Seiler, D. G., Becker, W. M., Roth, L. 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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=Two-dimensional+gas+of+massless+Dirac+fermions+in+graphene.">Two-dimensional gas of massless Dirac fermions in graphene.</a> Nature. 438, 197-200 (2005).</li><li>Wang, L., 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-Dimensional+Electrical+Contact+to+a+Two-Dimensional+Metal.">One-Dimensional Electrical Contact to a Two-Dimensional Metal.</a> Science. 342, 614-617 (2013).</li><li>Giessibl, F. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Advances+in+Atomic+Force+Microscopy.">Advances in Atomic Force Microscopy.</a> Reviews of Modern Physics. 75, 949-983 (2003).</li><li>Smith, K. C. A., Oatley, C. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Scanning+Electron+Microscope+and+its+Fields+of+Applications.">The Scanning Electron Microscope and its Fields of Applications.</a> British Journal of Applied Physics. 6, 391-399 (1955).</li><li>Geim, A. K., Grigorieva, I. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Van+der+Waals+heterostructures.">Van der Waals heterostructures.</a> Nature. 499, 419-425 (2013).</li></ol>

After acquisition of high quality bulk samples, characterized to ensure appropriate composition and structure, samples are patterned into the geometry depicted by exfoliating flakes of sample onto 1 cm &#215; 1 cm pieces of substrate. Substrates composed of heavily p-doped Si covered by approximately 300 nm of SiO2 are preferred as they increase the experimental parameter space by allowing the application of a back gate. Samples must be sufficiently thin &#8212; fewer than 10 nm&#160;&#8212; to produce a suffi...

The pursuit of materials platforms for advanced electronics technology demands methods for high-throughput materials synthesis and subsequent characterization. Novel materials of interest in this pursuit may be produced in bulk by direct reaction synthesis1,2, electrochemical growth3,4, and other methods5 in a more rapid fashion than more involved single crystal thin film deposition techniques such as molecular beam epitaxy or chemical vapor deposition. The conventional method to measure the transport properties of bulk crystal samples is to cleave a rectangular prism-shaped fragment with dimensions of approximately 1 mm x 1 mm x 6 mm and attach wire leads to the sample in a Hall bar configuration6.
Certain materials pose a challenge wherein the traditional bulk Hall bar device fabrication method is insufficient to produce a measureable device for sample transport measurement. This can be because the crystals produced are too small to attach lead wires to, even under a powerful optical microscope, because the desired sample thickness is on the order of one to only a few monolayers, or because one aims to measure a stack of layered two-dimensional materials with near- or sub-nanometer thickness. The first category consists of, for example nanowires and certain preparations of molybdenum oxide bronzes7. The second category consists of single to very-few layers of two-dimensional materials such as graphene8, TMDs (MoS2, WTe2, etc.), and topological insulators (Bi2Se3, BixSb1-xTe3, etc.). The third category consists of heterostructures prepared by stacking individual layers of two-dimensional materials by manual assembly via layer transfer, most notably a trilayer stack of hBN-graphene-hBN9.
Exploratory research of novel electronic materials demands adequate methods for producing devices on difficult-to-measure samples. Often, the first batch of a new material synthesized by direct reaction or electrochemical growth yields very small single crystals with dimensions on the size order of microns. Such samples have historically proven enormously difficult to attach metal contacts to, necessitating improvement of sample growth parameters to achieve larger crystals for easier transport device fabrication, presenting an obstacle in the high-throughput research of novel materials. In order to enable rapid characterization of materials, a method of device fabrication for very small samples has been devised to permit the characterization of novel materials as soon as a preliminary batch has been produced. A slight variation of this methodology is applicable to producing devices using exfoliated samples of two-dimensional materials such as graphene, hBN, and TMDs, as well as multilayer heterostructures of such materials. Devices are adhered and wire-bonded to a package for insertion into a commercial superconducting magnet, dry helium close-cycle cryostat magnetotransport system. Transport measurements are taken at temperatures down to 0.300 K and magnetic fields up to 12 T.

<table border="0" cellpadding="0" cellspacing="0" width="840">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">Cryogenic Limited 12T CFMS</td>
			<td style="width:89px;">Cryogen Limited</td>
			<td style="width:135px;">CFM-12T-H3- IVTI-25</td>
			<td style="width:417px;">Magnetotransport system customized with modulated field magnet (step 4)</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">7270 DSP Lock-in amplifier</td>
			<td style="width:89px;">Signal Recovery</td>
			<td style="width:135px;">7270</td>
			<td style="width:417px;">lock-in amplifier for source/drain and voltage measurements (step 4)</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">GS200 DC Voltage/Current Source</td>
			<td style="width:89px;">Yokogawa</td>
			<td style="width:135px;">GS200</td>
			<td style="width:417px;">Voltage source for gate voltage application (step 4)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:200px;">2636B System Sourcemeter</td>
			<td style="width:89px;">Keithley</td>
			<td style="width:135px;">2636B</td>
			<td style="width:417px;">Sourcemeter for source/drain and voltage measurements</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">DWL 2000 Laser Pattern Generator</td>
			<td style="width:89px;">Heidelberg Instruments</td>
			<td style="width:135px;">DWL 2000</td>
			<td style="width:417px;">Generate chrome mask for lithography of substrate location/alignment feature pattern (step 1.3)</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">Suss MicroTec MA6/BA6 Contact Aligner</td>
			<td style="width:89px;">Suss</td>
			<td style="width:135px;">MA6</td>
			<td style="width:417px;">Used for the lithography of substrate location/alignment feature pattern (step 1.4.12)</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">JEOL Direct Write Electron Beam Lithography System</td>
			<td style="width:89px;">JEOL</td>
			<td style="width:135px;">JBX 6300-FS&#160;</td>
			<td style="width:417px;">Perform high-resolution lithography of devices</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">Discovery 550 Sputtering System</td>
			<td style="width:89px;">Denton Vacuum</td>
			<td style="width:135px;">Discovery 550</td>
			<td style="width:417px;">Perform SiO2 sputtering (step 2.5)</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">Infinity 22 Electron Beam Evaporator</td>
			<td style="width:89px;">Denton Vacuum</td>
			<td style="width:135px;">Infinty 22</td>
			<td style="width:417px;">Perform Cr/Au deposition (steps 1.5 and 3.7)</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">Unaxis 790 Reactive Ion Etcher</td>
			<td style="width:89px;">Unaxis</td>
			<td style="width:135px;">Unaxis 790</td>
			<td style="width:417px;">Etch sample into Hall bar structure (step 3.4)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:200px;">Name</td>
			<td style="width:89px;">Company</td>
			<td style="width:135px;">Catalog Number</td>
			<td style="width:417px;">Comments</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">PMMA 495 A4</td>
			<td style="width:89px;">MicroChem</td>
			<td style="width:135px;">PMMA 495 A4</td>
			<td style="width:417px;">Polymer coating/electron beam mask for lithography (step 3.5.1)</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">PMMA 950 A4</td>
			<td style="width:89px;">MicroChem</td>
			<td style="width:135px;">PMMA 950 A4</td>
			<td style="width:417px;">Polymer coating/electron beam mask for sample dicing and lithography (steps 1.7.3, 3.3.1, and 3.5.2)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:200px;">S1813 positive photoresist</td>
			<td style="width:89px;">MicroChem</td>
			<td style="width:135px;">S1813 G2</td>
			<td style="width:417px;">Positive photoresist (step 1.4.8)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:200px;">LOR resist</td>
			<td style="width:89px;">MicroChem</td>
			<td style="width:135px;">LOR 3A</td>
			<td style="width:417px;">Lift off resist (step 1.4.3)</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">1:3 MIBK:IPA PMMA developer</td>
			<td style="width:89px;">MicroChem</td>
			<td style="width:135px;">1:3 MIBK:IPA</td>
			<td style="width:417px;">PMMA developer</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">MF-321 Developer</td>
			<td style="width:89px;">MicroChem</td>
			<td style="width:135px;">MF-321</td>
			<td style="width:417px;">Novolac positive photoresist-compatible developer solution (step 1.4.15)</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">Diglycidiyl ether-terminated polydimethylsiloxane</td>
			<td style="width:89px;">Sigma Aldrich</td>
			<td style="width:135px;">SA 480282</td>
			<td style="width:417px;">For layered material stacking (step 2.6.1)</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:200px;">Polypropylene carbonate</td>
			<td style="width:89px;">Sigma Aldrich</td>
			<td style="width:135px;">SA 389021</td>
			<td style="width:417px;">For layered material stacking (step 2.6.2)</td>
		</tr>
	</tbody>
</table>

advanced experimental methods for low-temperature magnetotransport measurement of novel materials

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film synthesis) for the purpose of exploratory materials research. Certain materials pose a challenge wherein the traditional bulk Hall bar device fabrication method is insufficient to produce a measureable device for sample transport measurement, principally because the single crystal size is too small to attach wire leads to the sample in a Hall bar configuration. This can be, for example, because the first batch of a new material synthesized yields very small single crystals or because flakes of samples of one to very few monolayers are desired. In order to enable rapid characterization of materials that may be carried out in parallel with improvements to their growth methodology, a method of device fabrication for very small samples has been devised to permit the characterization of novel materials as soon as a preliminary batch has been produced. A slight variation of this methodology is applicable to producing devices using exfoliated samples of two-dimensional materials such as graphene, hexagonal boron nitride (hBN), and transition metal dichalcogenides (TMDs), as well as multilayer heterostructures of such materials. Here we present detailed protocols for the experimental device fabrication of fragments and flakes of novel materials with micron-sized dimensions onto substrate and subsequent measurement in a commercial superconducting magnet, dry helium close-cycle cryostat magnetotransport system at temperatures down to 0.300 K and magnetic fields up to 12 T.

Figure 3 shows a typical Hall bar device patterned for the purpose of a low temperature magnetotransport experiment. The optical image in the upper figure shows a successfully-fabricated Graphene/hBN Hall bar; the lower image shows the device schematic with the Landauer-B&#252;ttiker edge states that arise from the Landau levels (LLs), a transport mechanism that can be used to calculate the values of the quantized Hall resistances, the experimental investigation of which ...

Watch this Scientific Journal Video about Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials at JoVE.com

Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials

We describe the methodology of mechanical exfoliation and deposition of flakes of novel materials with micron-sized dimensions onto substrate, fabrication of experimental device structures for transport experimentation, and the magnetotransport measurement in a dry helium close-cycle cryostat at temperatures down to 0.300 K and magnetic fields up to 12 T.

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film ...

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