The research leading to these results has received funding from the European Union Seventh Framework Program under grant agreement n&#176;604391 Graphene Flagship. C.B. acknowledges the German Research Foundation, DFG, under grant BA 4856/2-1.

1. Liquid Exfoliation &#8212; Preparation of Suitable Stock Dispersions
<ol>
	<li>Mount a metal cup underneath a sonotrode in an ice bath.</li>
	<li>Immerse 1.6 g of the TMD powder in 80 mL aqueous solution of sodium cholate (SC) surfactant (sodium cholate concentration, CSC= 6 g L-1) in the metal cup.</li>
	<li>Move the sonic tip to the bottom of the metal cup and then up by ~ 1 cm. Wrap aluminum foil around the sonic probe to avoid spillage.</li>
	<li>Sonicate the mixture under ice-cooling by probe sonication to avoid heating using a solid flathead tip (750 W processor) for 1 h at 60% amplitude (pulse of 6 s on and 2 s off).</li>
	<li>Centrifuge the dispersion at a centrifugation speed of 2,660 x g for 1.5 h. Discard the supernatant containing impurities and collect the sediment in 80 mL fresh surfactant solution (CSC= 2 g L-1). 
	NOTE: Use maximum filling heights in the centrifuge tubes of maximum 10 cm. Otherwise, increase the centrifugation time.</li>
	<li>Subject the dispersion to a second, longer sonication using the solid flathead tip for 5 h at 60% amplitude (pulse of 6 s on and 2 s off) under ice-cooling. Replace the ice bath every 2 h while pausing the sonication.</li>
</ol>
2. Nanosheet Size Selection by Liquid Cascade Centrifugation
NOTE: To select nanosheets by size, liquid cascade centrifugation with sequentially increasing centrifugal acceleration is applied (Figure 1). The following procedure is recommended as standard size selection of the cascade in the case of TMDs. For other materials, centrifugation speeds may need to be adjusted.
<ol>
	<li>Remove unexfoliated powder by centrifugation at 240 x g (1.5 krpm), 2 h. Discard the sediment.</li>
	<li>Centrifuge the supernatant at a higher centrifugal acceleration: 425 x g (2 krpm), 2 h. Collect the sediment in fresh surfactant at reduced volume (3-8 mL).</li>
	<li>Centrifuge the supernatant at even higher centrifugal acceleration: 950 x g (3 krpm), 2 h. Collect the sediment in fresh surfactant at reduced volume (3-8 mL).</li>
	<li>Repeat this procedure with the following centrifugal accelerations: 1,700 x g (4 krpm), 2,650 x g (5 krpm), 3,500 x g (6 krpm), 5,500 x g (7.5 krpm), and 9,750 x g (10 krpm).</li>
</ol>
3. Determination of Nanosheets Size and Thickness by Statistical Microscopy
NOTE: If spectroscopic metrics are already available, section 3 can be skipped or reduced, i.e., not carried out for every sample.
<ol>
	<li>Length: Transmission electron microscopy (TEM)
	<ol>
		<li>Deposition
		<ol>
			<li>Dilute the high concentration dispersions with water (to reduce the surfactant concentration) so that they are of light in color. Drop cast onto a grid (for example holey carbon, 400 mesh) placed on a filter membrane to wick away excess solvent.</li>
		</ol>
		</li>
		<li>Imaging
		<ol>
			<li>Record multiple images on different positions on the grid. Adjust the field of view depending on nanosheet size. For a comprehensive TEM imaging tutorial, see reference 18.</li>
		</ol>
		</li>
		<li>Statistical length analysis performed using ImageJ
		<ol>
			<li>Open the ImageJ software, select the relevant TEM image via the &#34;file&#34; menu and &#34;open&#34; the image. The image will open in a new window.</li>
			<li>Click the &#34;analyze&#34; tab. Select &#34;set scale&#34; from the drop down menu. A new window will open. Click &#34;remove scale&#34;, tick &#34;global&#34; and click &#34;ok&#34;.</li>
			<li>Select the &#34;line&#34; tool. Draw a line profile along the length of the scale bar of the TEM image.</li>
			<li>Click &#34;analyze&#34;. Select &#34;set scale&#34; from the drop down menu. Enter the length of the scale bar in nm into the &#34;known distance&#34; box and click &#34;ok&#34;. 
			NOTE: The distance of the line drawn on the scale bar is displayed in pixels.</li>
			<li>Select the &#34;line&#34; tool and measure the nanosheet length by drawing a line profile of the longest axis of the nanosheet.</li>
			<li>Press &#34;control+M&#34; to measure. A new box labelled &#34;results&#34; opens with the nanosheet length displayed in the &#34;length&#34; column.</li>
			<li>Repeat step 3.1.3.6 for all individually deposited nanosheets (not aggregated ones) in the image.</li>
			<li>When opening a new image, repeat steps 3.1.3.3- 3.1.3.7. Count the length of 150 nanosheets. 
			NOTE: All nanosheet length data is compiled in the &#34;results&#34; window and can be copied into other programs for further processing.</li>
		</ol>
		</li>
	</ol>
	</li>
	<li>Thickness: Atomic force microscopy (AFM)
	<ol>
		<li>Dilute the dispersion so that are almost transparent to the human eye (corresponding to extinction intensity of ideally ~0.2 per 1 cm pathlength at 400 nm). In the case of surfactant dispersions, dilute with water not surfactant.</li>
		<li>Drop-cast on pre-heated wafers. For water-based dispersion, heat the wafer to ~170 &#176;C on a hot plate and deposit 10 &#181;L per 0.5 x 0.5 cm2 wafer.</li>
		<li>Rinse the wafers thoroughly with a minimum of 5 mL of water and 3 mL of 2-propanol to remove residual surfactant and other impurities.</li>
		<li>Scan and save multiple images across the sample with the AFM in tapping mode. For small nanosheets use a resolution of 512 lines per image and image sizes of maximum 2 x 2 &#181;m2. For samples containing larger nanosheets, increase the field of view to up to 8 x 8 &#181;m2. Use scan rates as appropriate (typically 0.4-0.7 Hz). Alternatively, scan larger areas at higher resolution.</li>
		<li>Thickness measurement using Gwyddion Software
		<ol>
			<li>Open the software and select the relevant AFM image via &#34;file&#34; and &#34;open&#34;. The image will open in a new window.</li>
			<li>Correct the background using the &#34;level data by mean plane subtraction&#34; &#34;align rows&#34; and &#34;correct horizontal scars&#34; in the &#34;Data Process&#34; section of the home menu. Apply the corrections, change the image color for better contrast by right-clicking on the legend and set z-plane to zero.</li>
			<li>Zoom in the region of choice (if convenient). Click on the &#34;crop&#34; tool in the home menu. Drag the cursor over the image to mark the region of choice. Press &#34;apply&#34;. Check the &#34;create new channel&#34; to open the selected region in a new window.</li>
			<li>Select &#34;extract profiles&#34; from the tools menu. A new window opens.</li>
			<li>Draw a line across the nanosheet. Write down the thickness in a table. In the case of non-homogeneously thick nanosheets, average the thickness across the nanosheet. Take extreme care to measure only individually deposited and non-aggregated nanosheets.</li>
			<li>Repeat 3.2.5.3-3.2.5.5 for all nanosheets on the image.</li>
			<li>Repeat 3.2.5.1-3.2.5.6 for all images recorded. Count minimum 150 nanosheets.</li>
		</ol>
		</li>
	</ol>
	</li>
	<li>Conversion of AFM thickness to layer number 
	NOTE: Apparent AFM heights from liquid exfoliated nanomaterials are usually overestimated due to the presence of residual solvent. In addition, accurate height measurements of inhomogeneous samples (such as nanomaterials deposited on substrates) using AFM are generally challenging due to contributions from effects such as capillary forces and adhesion which depend on the material and measurement parameters.19,20 To overcome these problems and to convert the apparent measured AFM thickness to the number of layers, a procedure termed step height analysis was developed as described in the following.12,13,16,21. Steps 3.3.1-3.3.4 can be skipped if the step height is known.
	<ol>
		<li>Open, correct and crop the AFM image as described in 3.2 to select a nanosheet with clearly discernible terraces.</li>
		<li>Measure the height across the nanosheet using the &#34;extract&#34; profile tool. 
		NOTE: Suitable profiles show discrete steps as the one in Figure 2B inset.
		<ol>
			<li>Record the height of these steps (i.e., the height difference from one terrace to the next on the nanosheet).</li>
		</ol>
		</li>
		<li>Count at least 70 of these steps.</li>
		<li>Plot the step height in ascending order (Figure 2C). 
		NOTE: Observe that for TMDs the apparent step height is always a multiple of ~1.9 nm.</li>
		<li>Divide the apparent AFM thickness (measured as described in section 3.2) by 1.9 nm to obtain the layer number. 
		NOTE: Other materials have other step height conversion factors requiring a different calibration.</li>
	</ol>
	</li>
</ol>
4. Determination of MoS2 and WS2 Size and Thickness Based on Extinction Spectra
<ol>
	<li>Spectra acquisition
	<ol>
		<li>Dilute the high concentration samples with the respective medium (here aqueous sodium cholate, 2 g L-1) to yield extinctions below 2 across the entire spectral range.</li>
		<li>Set the increments for the spectral acquisition to 0.5 nm in the instrument settings or use scan speed slow or medium.</li>
		<li>Choose the settings &#34;subtract baseline&#34; in the instrument settings. Place the cuvette containing the aqueous sodium cholate solution in the sample compartment of the spectrometer and run the measurement.</li>
		<li>Remove the cuvette with the sodium cholate solution from the spectrometer and empty it. Fill in the sample, place the sample in the sample compartment of the spectrometer and run a scan of the sample.</li>
	</ol>
	</li>
	<li>Length determination from intensity ratios
	<ol>
		<li>Option 1: Read-off the intensity at the A-exciton, ExtA (~660 nm for MoS2 and 620 nm for WS2) and the local minimum Extmin (345 nm for MoS2 and 295 nm for WS2). Divide the intensity at the A-exciton by the intensity at the local minimum to obtain the intensity ratio ExtA/Extmin.</li>
		<li>Determine the mean nanosheet length, &#60;L&#62; by using equation 1. 
		<img alt="Equation 1" src="/files/ftp_upload/54806/54806equation1.jpg" /> (Eq. 1) 
		where ExtA/Extmin is the intensity ratio of the extinction at the A-exciton (ExtA) and the local minimum (Extmin). 
		NOTE: The equation holds for both MoS2 and WS2. However, its accuracy is limited especially for small nanosheets.</li>
		<li>Option 2: Determine the intensity ratio of the local maximum in the UV region of the spectrum, ExtMax-HE (270 nm for MoS2 and 235 nm for WS2) and the local minimum, Extmin (345 nm for MoS2 and 295 nm for WS2)</li>
		<li>Determine the mean nanosheet length, &#60;L&#62; by using equation 2. 
		<img alt="Equation 2" src="/files/ftp_upload/54806/54806equation2.jpg" /> (Eq. 2) 
		With Extmax-HE denoting the intensity at the local maximum at high energy (270 nm for MoS2 and 235 nm for WS2) and Extmin the extinction intensity at the local minimum (345 nm for MoS2 and 295 nm for WS2). 
		NOTE: Option 2 gives a more accurate measure of the lateral size. However, the high energy region may not be accessible in all solvents/surfactant.</li>
	</ol>
	</li>
	<li>Concentration
	<ol>
		<li>Record the extinction intensity relative to 1 cm pathlength at 345 nm for MoS2 and 235 nm for WS2, respectively. 
		NOTE: Divide the recorded measured extinction by the pathlength of the cuvette.</li>
		<li>Divide this intensity by the extinction coefficients of 68 Lg-1cm-1 at 345 nm for MoS2 and 47 Lg-1cm-1 at 235 nm for WS2 to obtain the nanosheet concentration in gL-1.</li>
	</ol>
	</li>
	<li>Thickness determination from A-exciton position
	<ol>
		<li>Calculate the second derivative of the spectrum.
		<ol>
			<li>Using the data analysis and graphing software (e.g., OriginPro), select the column containing the extinction intensity. Click on the &#34;analysis&#34; tab, select &#34;mathematics&#34; from the drop down menu and &#34;differentiate&#34;, &#34;open dialog&#34;. A new window will open. Set the derivative order to 2 and press ok.</li>
		</ol>
		</li>
		<li>Smooth the second derivative by Adjacent Averaging (~ 10-20 points per window in A-exciton region).
		<ol>
			<li>For example, using the data analysis and graphing software, plot the second derivative spectrum.
			<ol>
				<li>With the graphic window active, click on &#34;analysis&#34; and choose &#34;signal processing&#34;, then &#34;smooth&#34; then &#34;open dialog&#34; from the drop down menu. A new window will open.</li>
				<li>Choose &#34;Adjacent Averaging&#34; as smoothing method and set the points to 20.</li>
				<li>Plot the resultant smoothed spectrum which is displayed as new columns. If the noise is still high, repeat the smoothing. 
				NOTE: Usually, spectral smoothing is required to reduce the noise unless high integration times during the measurement are used. The appropriate smoothing is an important part of the data analysis and the appropriate smoothing method depends on the desired outcome. This particular smoothing method is only ideal to determine the mean peak position.13</li>
			</ol>
			</li>
		</ol>
		</li>
		<li>Read-off the peak position from the second derivative. This is the wavelength of the A-exciton, &#955;A. Alternatively, carry out the steps described in 4.4.4-4.4.7.</li>
		<li>Convert the x-axis from wavelength to energy using the relation: 
		E(eV) = 4.135E-6 * 2.997E8 / &#955;(nm)</li>
		<li>Fit the second derivative to the second derivative of a Lorentzian. 
		NOTE: A Lorentzian can be written as 
		<img alt="Equation 3" src="/files/ftp_upload/54806/54806equation3.jpg" /> (Eq. 3) 
		Where h is the height, E&#39;0 is the center and w is the FWHM. Differentiating twice with respect to E gives 
		<img alt="Equation 4" src="/files/ftp_upload/54806/54806equation4.jpg" /> (Eq. 4)
		<ol>
			<li>In the data analysis and graphing software, choose &#34;tools&#34; from the main menu and select &#34;fitting function builder&#34;. A new window will open.</li>
			<li>Select &#34;create a new function&#34;, click next.</li>
			<li>Leave the default settings, give the function a name and click next.</li>
			<li>Set &#34;h,E,w&#34; as parameters, click next.</li>
			<li>Enter &#34;(-8*h/w^2)*(1-3*(2*(E-x)/w)^2)/(1+(2*(E-x)/w)^2)^3&#34; as function body, click finish.</li>
			<li>Plot only the A-exciton region of the second derivative spectrum on the energy scale.</li>
			<li>With the graphics window active, click on the &#34;analysis&#34; tab. Choose &#34;fitting&#34;, &#34;nonlinear curve fit&#34;, &#34;open dialog&#34; from the drop down menu. A new window will open.</li>
			<li>Select &#34;user defined&#34; in category and choose the previously built function in the function box. In the tab &#34;parameters&#34; set initial values for w to 0.1, and E to 1.99 for WS2 and 1.85 for MoS2. Press &#34;fit&#34;</li>
		</ol>
		</li>
		<li>Record the energy E&#39;0, which is the energy associated with the A-exciton, E&#39;A.</li>
		<li>Determine the number of layers according to equations 5 (MoS2) and 6 (WS2). 
		<img alt="Equation 5" src="/files/ftp_upload/54806/54806equation5.jpg" /> (Eq. 5, MoS2) 
		<img alt="Equation 6" src="/files/ftp_upload/54806/54806equation6.jpg" /> (Eq. 6, WS2) 
		with &#955;A denoting the wavelength of the A-exciton and EA denoting the energy of the A-exciton.</li>
	</ol>
	</li>
</ol>

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The authors have nothing to disclose.

Sample preparation
The samples described here are produced by tip sonication. Alternative exfoliation procedures can be used, but will lead to different concentrations, lateral sizes and degrees of exfoliation. Higher amplitudes and longer on pulses during the sonication should be avoided to prevent damaging of the sonicator. Similar results were obtained using 500 W processors. However, sonication time and amplitude has an impact on the nanosheet exfoliation and variations from this protocol may...

The possibility to produce and process graphene, related two-dimensional (2D) crystals in the liquid phase makes them promising materials for an ever growing range of applications as composite materials, sensors, in energy storage and conversion and flexible (opto) electronics.1-6 To exploit 2D nanomaterials within applications such as these will require inexpensive and reliable functional inks with on-demand lateral size and thickness of the nanoscale constituents, as well as controlled rheological and morphological properties amenable to industrial-scale printing/coating processes.7 In this regard, liquid phase exfoliation has become an important production technique giving access to a whole host of nanostructures in large quantities.6,8,9 This method involves the sonication or shearing of layered crystals in liquids. If the liquid is appropriately chosen (i.e., suitable solvents or surfactant) the nanosheets will be stabilized against reaggregation. Numerous applications and proof-of-principle devices have been demonstrated by such techniques.6 Probably the greatest strength of this strategy is its versatility, as numerous layered parent crystals can be exfoliated and processed in a similar way, providing access to a broad palette of materials which can be tailored to the desired application.
However, despite this recent progress, the resultant polydispersity that arises due to these liquid-phase production methods (in terms of nanosheet length and thickness) still presents a bottleneck in the realization of high performance devices. This is mostly because the development of novel and innovative size selection techniques has thus far required nanosheets length and thickness characterization using tedious statistical microscopy (atomic force microscopy, AFM and/or transmission electron microscopy, TEM).
Despite these challenges, several centrifugation techniques have been reported to achieve length and thickness sorting.6,10-13 The simplest scenario is homogeneous centrifugation, where the dispersion is centrifuged at a given centrifugal acceleration and the supernatant is decanted for analysis. The centrifugation speed sets the size cut-off, whereby the higher the speed, the smaller are the nanosheets in the supernatant. However, this technique suffers from two major disadvantages; firstly, when larger nanosheets are to be selected (i.e., the dispersion is centrifuged at low speeds and the supernatant is decanted) all smaller nanosheets will also remain in the sample. Secondly, regardless of the centrifugation speed, a significant proportion of the material tends to be wasted in the sediment.
An alternative strategy for size selection is density gradient (or isopycnic) centrifugation.11,14 In this case, the dispersion is injected into a centrifuge tube containing a density gradient medium. During ultracentrifugation (typically &#62; 200,000 x g), a density gradient is formed and the nanosheets move to the point in the centrifuge where their buoyant density (density including the stabilizer and solvent shell) matches the density of the gradient. Note that the nanomaterial can also move upward during this process (depending on where it was injected). In such a way, the nanosheets are effectively sorted by thickness rather than mass (opposed to homogeneous centrifugation). While this procedure offers a unique opportunity to sort nanosheets by thickness, it suffers from notable disadvantages. For example, the yields are very low and at present do not allow for the mass production of separated nanosheets. This is partly related to low contents of monolayers in stock dispersions after liquid-exfoliation and can potentially be improved by optimizing exfoliation procedures in the future. In addition, it is typically a time-consuming multi-step ultracentrifugation process involving multiple iterations to achieve efficient size selection. Furthermore, in the case of inorganic nanomaterials, it is restricted to polymer-stabilized dispersions to obtain the required buoyant densities and the gradient medium in the dispersion may interfere with further processing.
We have recently shown that a procedure we term liquid cascade centrifugation (LCC) offers an exciting alternative,13 as we will also detail in this manuscript. This is a multi-step procedure which is extremely versatile allowing various cascades to be designed according to the desired outcome. To demonstrate this process, a standard cascade is portrayed in Figure 1 and involves multiple centrifugation steps whereby each features a higher speed than the last. After each step, the sediment is retained and the supernatant is then used in the proceeding stage. As a result, each sediment contains nanosheets in a given size range which have been &#34;trapped&#34; between two centrifugations with different speeds; the lower one removing larger nanosheets into the previous sediment while the higher speed removes the smaller nanosheets into the supernatant. Critical to LCC, the resulting sediment can be redispersed completely by mild sonication in the respective medium, which in this case is aqueous sodium cholate H2O-SC (at SC concentrations as low as 0.1 g L-1). The result is dispersions with virtually any chosen concentration. Importantly, virtually no material is wasted in LCC, resulting in the collection of relatively large masses of size-selected nanosheets. As shown here, we have applied this procedure to a number of liquid-exfoliated nanosheets including MoS2 and WS2 as well as GaS,15 black phosphorus16 and graphene17 in both solvent and surfactant systems.
This unique centrifugation procedure enables the efficient size-selection of liquid exfoliated nanosheets and has subsequently enabled a significant advancement in terms of their size and thickness determination. In particular, through this approach we demonstrated previously that optical extinction (and absorbance) spectra of the nanosheets change systematically as function of both nanosheets lateral dimensions and nanosheets thickness. As we summarize here, this has allowed us to link the nanosheet spectral profile (specifically the intensity ratio at two positions of the extinction spectrum) to the mean nanosheet length as a result of nanosheet edge effects.12,13 Importantly, the same equation can be used to quantify the size of MoS2 and WS2. Furthermore, we show that the A-exciton position shifts towards lower wavelengths as a function of mean nanosheet thickness due to confinement effects. Even though exfoliation, as well as size selection and determination are in general rather robust procedures, the quantitative outcome depends on subtleties in the protocol. However, especially for newcomers to the field, it is difficult to judge which process parameters are most relevant. This comes down to the fact that experimental sections of research papers only provide a rough protocol, without discussing what outcome is to be expected when modifying the procedure or giving a rational behind the protocol. In this contribution, we intend to address this as well as provide a detailed guide and discussion to the production of liquid-exfoliated nanosheets of controlled size and to the accurate determination of size by either statistical microscopy or analysis of the extinction spectra. We are convinced that this will help to improve reproducibility and hope it will be a useful guide for other experimentalists in this research area.
<img alt="Figure 1" src="/files/ftp_upload/54806/54806fig1.jpg" /> 
Figure 1: Schematic of the size selection by liquid cascade centrifugation. Size-selected nanosheets are collected as sediments. Each sediment is collected or &#34;trapped&#34; between two centrifugation speeds (&#969;) starting from low speeds and going to higher ones from step to step. The sediment discarded after the first centrifugation contains unexfoliated layered crystallites while the supernatant discarded after the last centrifugation step contains extremely small nanosheets. Size-selected dispersions are prepared by re-dispersing the collected sediments in the same medium (here aqueous surfactant solution) at reduced volumes. Adapted with permission from 13. <a href="http://cloudflare.jove.com/files/ftp_upload/54806/54806fig1large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>

<table><tbody><tr><td>Sodium cholate hydrate, from ox and/or sheep bile</td><td>Sigma Aldrich</td><td>C1254-100G</td><td>Surfactant used as stabilizer in the form of an aqueous solution (&lt;em&gt;i.e.&lt;/em&gt;, after dissolving the powder in millipore water)</td></tr><tr><td>MoS&lt;sub&gt;2&lt;/sub&gt; powder</td><td>Sigma Aldrich</td><td>69860-100G</td><td>Other distributors available, but exfoliation and outcome of size selection can vary</td></tr><tr><td>WS&lt;sub&gt;2&lt;/sub&gt;, powder 2 &amp;#956;m</td><td>Sigma Aldrich</td><td>243639-50G</td><td>Other distributors available, but exfoliation and outcome of size selection can vary</td></tr><tr><td>ImageJ Software</td><td>Developer: National Insitutes of Health</td><td>64-bit Java version 2.45 1.6.0_24</td><td>Image processing software used for TEM analysis, free download</td></tr><tr><td>Gwyddion Software</td><td>Developer: Czech Metrology Institute</td><td>64-bit Java version 2.45</td><td>Image processing software used for AFM analysis, free download</td></tr><tr><td>Origin Pro Software</td><td>OriginLab</td><td>Version 2016</td><td>Software used for data analysis such as differntiation and fitting of the extinction spectra</td></tr><tr><td>Centrifuge</td><td>HettichLab</td><td>Mikro 220R</td><td>any other benchtop centrifuge is suitable</td></tr><tr><td>Rotor 1</td><td>Hettich</td><td>Rotor 1016</td><td>for centrifugation &amp;lt;5,000 x g</td></tr><tr><td>Rotor 2</td><td>Hettich</td><td>Rotor 1195-A</td><td>for centrifugation &gt;5,000 x g</td></tr></tbody></table>

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.

Liquid cascade centrifugation (Figure 1) is a powerful technique to sort liquid-exfoliated nanosheets by size and thickness as illustrated in Figure 2 for both MoS2 and WS2. Nanosheet lateral sizes and thicknesses can be characterized by statistical TEM and AFM, respectively. A typical AFM image is shown in Figure 2A. The apparent nanosheet thickness is converted to layer number using step height analysis (Fi...

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

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. ...

preparation-liquid-exfoliated-transition-metal-dichalcogenide

Universidad de Cartagena UDEC

Research

JoVE Journal

Engineering

13.8K Views.  Ruprecht-Karls University Heidelberg. A protocol for the liquid exfoliation of layered materials to nanosheets, their size selection and size measurement by microscopic and spectroscopic techniques is presented.

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

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

Chemistry

Preparation of Carbon Nanosheets at Room Temperature

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into defined aggregates in aqueous media and at the air-water interface. In the aggregated state, the oligoynes can then be carbonized under mild conditions while preserving the morphology and the embedded chemical functionalization. This novel approach provides direct access to functionalized carbon nanomaterials. In this article, we present a synthetic approach that allows us to prepare hexayne carboxylate amphiphiles as carbon-rich siblings of typical fatty acid esters through a series of repeated bromination and Negishi-type cross-coupling reactions. The obtained compounds are designed to self-assemble into monolayers at the air-water interface, and we show how this can be achieved in a Langmuir trough. Thus, compression of the molecules at the air-water interface triggers the film formation and leads to a densely packed layer of the molecules. The complete carbonization of the films at the air-water interface is then accomplished by cross-linking of the hexayne layer at room temperature, using UV irradiation as a mild external stimulus. The changes in the layer during this process can be monitored with the help of infrared reflection-absorption spectroscopy and Brewster angle microscopy. Moreover, a transfer of the carbonized films onto solid substrates by the Langmuir-Blodgett technique has enabled us to prove that they were carbon nanosheets with lateral dimensions on the order of centimeters.

We present the synthesis of an amphiphilic hexayne and its use in the preparation of carbon nanosheets at the air-water interface from a self-assembled monolayer of these reactive, carbon-rich molecular precursors.

Amphiphilic molecules equipped with a reactive, carbon-rich "oligoyne" segment consisting of conjugated carbon-carbon triple bonds self-assemble into ...

Ohmic Contact Fabrication Using a Focused-ion Beam Technique and Electrical Characterization for Layer Semiconductor Nanostructures

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor performance, which suggest a new direction for the development of next-generation ultrathin and flexible photonic and electronic devices. Enhanced luminescence quantum efficiency has been widely observed in these atomically thin 2D crystals. However, dimension effects beyond quantum confinement thicknesses or even at the micrometer scale are not expected and have rarely been observed. In this study, molybdenum diselenide (MoSe2) layer crystals with a thickness range of 6-2,700 nm were fabricated as two- or four-terminal devices. Ohmic contact formation was successfully achieved by the focused-ion beam (FIB) deposition method using platinum (Pt) as a contact metal. Layer crystals with various thicknesses were prepared through simple mechanical exfoliation by using dicing tape. Current-voltage curve measurements were performed to determine the conductivity value of the layer nanocrystals. In addition, high-resolution transmission electron microscopy, selected-area electron diffractometry, and energy-dispersive X-ray spectroscopy were used to characterize the interface of the metal&#8211;semiconductor contact of the FIB-fabricated MoSe2 devices. After applying the approaches, the substantial thickness-dependent electrical conductivity in a wide thickness range for the MoSe2-layer semiconductor was observed. The conductivity increased by over two orders of magnitude from 4.6 to 1,500 &#937;&#8722;1 cm&#8722;1, with a decrease in the thickness from 2,700 to 6 nm. In addition, the temperature-dependent conductivity indicated that the thin MoSe2 multilayers exhibited considerably weak semiconducting behavior with activation energies of 3.5-8.5 meV, which are considerably smaller than those (36-38 meV) of the bulk. Probable surface-dominant transport properties and the presence of a high surface electron concentration in MoSe2 are proposed. Similar results can be obtained for other layer semiconductor materials such as MoS2 and WS2.

We describe the approaches for the device fabrication and electrical characterization of molybdenum diselenide (MoSe2) layer semiconductor nanostructures with different thicknesses. In addition, the fabrication of ohmic contacts for MoSe2-layer nanocrystals by the focused-ion beam deposition method using platinum (Pt) as a contact metal is described.

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor ...

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.

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 ...

Electric-field Control of Electronic States in WS2 Nanodevices by Electrolyte Gating

A method of carrier number control by electrolyte gating is demonstrated. We have obtained WS2 thin flakes with atomically flat surface via scotch tape method or individual WS2 nanotubes by dispersing the suspension of WS2 nanotubes. The selected samples have been fabricated into devices by the use of the electron beam lithography and electrolyte is put on the devices. We have characterized the electronic properties of the devices under applying the gate voltage. In the small gate voltage region, ions in the electrolyte are accumulated on the surface of the samples which leads to the large electric potential drop and resultant electrostatic carrier doping at the interface. Ambipolar transfer curve has been observed in this electrostatic doping region. When the gate voltage is further increased, we met another drastic increase of source-drain current which implies that ions are intercalated into layers of WS2 and electrochemical carrier doping is realized. In such electrochemical doping region, superconductivity has been observed. The focused technique provides a powerful strategy for achieving the electric-filed-induced quantum phase transition.

Electric-field Control of Electronic States in WS2 Nanodevices by Electrolyte Gating

Here, we present a protocol to control the carrier number in solids by using the electrolyte.

A method of carrier number control by electrolyte gating is demonstrated. We have obtained WS2 thin flakes with atomically flat surface via scotch tape ...

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We present methods for depositing and passively manipulating C60 molecules on rippled graphene that advance the pursuit of realizing applications involving 1D C60/graphene hybrid structures. The techniques applied in this exposition are geared towards high vacuum systems with preparation areas capable of supporting molecular deposition as well as thermal annealing of the samples. We focus on C60 deposition at low pressure using a homemade Knudsen cell connected to a scanning tunneling microscopy (STM) system. The number of molecules deposited is regulated by controlling the temperature of the Knudsen cell and the deposition time. One-dimensional (1D) C60 chain structures with widths of two to three molecules can be prepared via tuning of the experimental conditions. The surface mobility of the C60 molecules increases with annealing temperature allowing them to move within the periodic potential of the rippled graphene. Using this mechanism, it is possible to control the transition of 1D C60 chain structures to a hexagonal close packed quasi-1D stripe structure.

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Here we present a protocol for the fabrication of C60/graphene hybrid nanostructures by physical thermal evaporation. Particularly, the proper manipulation of deposition and annealing conditions allow the control over the creation of 1D and quasi 1D C60 structures on rippled graphene.

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We ...

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 ...

Exfoliation and Analysis of Large-area, Air-Sensitive Two-Dimensional Materials

We describe methods for producing and analyzing large, thin flakes of air-sensitive two-dimensional materials. Thin flakes of layered or van der Waals crystals are produced using mechanical exfoliation, in which layers are peeled off a bulk crystal using adhesive tape. This method produces high-quality flakes, but they are often small and can be hard to find, particularly for materials with relatively high cleavage energies such as black phosphorus. By heating the substrate and the tape, two-dimensional material adhesion to the substrate is promoted, and the flake yield can be increased by up to a factor of ten. After exfoliation, it is necessary to image or otherwise analyze these flakes but some two-dimensional materials are sensitive to oxygen or water and will degrade when exposed air. We have designed and tested a hermetic transfer cell to temporarily maintain the inert environment of a glovebox so that air-sensitive flakes can be imaged and analyzed with minimal degradation. The compact design of the transfer cell is such that optical analysis of sensitive materials can be performed outside of a glovebox without specialized equipment or modifications to existing equipment.

A method for exfoliating large thin flakes of air sensitive two-dimensional materials and safely transporting them for analysis outside of a glovebox is presented.

We describe methods for producing and analyzing large, thin flakes of air-sensitive two-dimensional materials. Thin flakes of layered or van der Waals ...

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 ...

Synthesis of Graphene Nanofluids with Controllable Flake Size Distributions

A method for synthesizing graphene nanofluids with controllable flake size distributions is presented. Graphene nanoflakes can be obtained by the exfoliation of graphite in the liquid phase, and the exfoliation time is used to control the lower limits of the graphene nanoflake size distributions. Centrifugation is successfully used to control the upper limits of the nanoparticle size distributions. The objective of this work is to combine exfoliation and centrifugation to control the graphene nanoflake size distributions in the resulting suspensions.

A method for synthesizing graphene nanofluids with controllable flake size distributions is presented.

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

Summary

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Chapters in this video

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Preparation of Carbon Nanosheets at Room Temperature

Ohmic Contact Fabrication Using a Focused-ion Beam Technique and Electrical Characterization for Layer Semiconductor Nanostructures

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

Electric-field Control of Electronic States in WS₂ Nanodevices by Electrolyte Gating

Preparation and Characterization of C₆₀/Graphene Hybrid Nanostructures

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

Exfoliation and Analysis of Large-area, Air-Sensitive Two-Dimensional Materials

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

Synthesis of Graphene Nanofluids with Controllable Flake Size Distributions