The authors would like to acknowledge the financial support from Universiti Kebangsaan Malaysia research grant: UKM-GGPM-2022-069 to carry out this research.

1. Substrate preparation
<ol>
	<li>Wipe the glass substrates with lint-free cloth to remove loose dirt or debris. Wash glass substrates with water and soap, use brush to scrub any dirt on the glass.</li>
	<li>Prepare all solvents listed below in beakers, submerge the glass substrates in the solvent and sonicate accordingly at 37 kHz. Prepare methanol at 80 &#176;C for 10 min; acetone at 80 &#176;C for 10 min, ethanol at 80 &#176;C for 10 min, distilled (DI) water at 80 &#176;C for 20 min. 
	CAUTION: Handle highly volatile chemicals in a fume hood.</li>
	<li>Take out the substrates from the beaker one by one using a tweezer, put on a clean flat surface, hold down the substrate with tweezer and blow with nitrogen gas until dry.</li>
	<li>Put substrates on a hot plate at 120 &#176;C for 5-10 min to vaporize any residue. Put substrates in UV-ozone cleaner for 10 min.</li>
</ol>
2. Sputtering method
<ol>
	<li>Chamber preparation
	<ol>
		<li>Take off the aluminum shield from the gun and put the target material at the center of the cover. Tightly screw the cover on the magnetron holder and put back the aluminum shield. Cover the body of the chamber, guns, and sample holder with aluminum foil.</li>
		<li>Run short-circuit inspection by touching the probes of a multimeter between the chamber bodies (short), followed by the chamber body and the gun (short), and finally the chamber body and the target (open). This test is necessary to ensure there is no current leakage between the body (anode) and the target (cathode), which can hinder the formation of plasma.</li>
	</ol>
	</li>
	<li>Pre-sputtering
	<ol>
		<li>Close the door and vacuum the chamber for 15 - 30 min. Press the door and the body together at the beginning of the vacuuming to ensure the door is tightly closed. Make sure the reading of the pressure gauge is decreasing.</li>
		<li>Switch ON the cooler system and set to 15 &#176;C. Turn ON the pump and refrigeration button, and open the valve connected to the sputtering instrument. 
		NOTE: RF sputtering does not function without a cooling system. The formation of plasma will not happen.</li>
		<li>Set Argon flow to 4 sccm and switch ON the gas toggle switch. Wait until the flow reaches the set value.</li>
		<li>Set rotation to 10 rpm and switch ON the rotation toggle switch. Push the Power button to switch ON the automatic matching network controller and radio frequency power supply.</li>
		<li>On the automatic matching network controller, set load and tune to 50 W each by pushing the Min/Max button and push the button from Manual to Auto.</li>
		<li>On the radio frequency power supply, set RF power to 50 W and push the Start button. Set the timer to 15 min.</li>
		<li>Switch OFF the RF power and rotation. Set Argon flow to 0 and switch OFF the toggle switch. Switch OFF the vacuum. 
		NOTE: Wait until the Argon flow reaches 0.1 sccm before switching off the vacuum.</li>
		<li>Vent to open the chamber. Make sure the turbomolecular pump (TMP) is OFF before venting. Venting while TMP is running will damage the system.</li>
		<li>Open the chamber and load substrates. Place the substrates at the outer corner of the rotating sample holder for better deposition as shown in Figure 1. 
		CAUTION: Wear mask and glove when handling the inside of the chamber to avoid inhaling small particles of materials.</li>
		<li>Close the door as shown in Figure 2 and vacuum for at least 6 h. Lower base pressure gives better deposition. The optimum base pressure for a high vacuum system such as sputtering process is 1 x 10-5 Torr.</li>
	</ol>
	</li>
	<li>Sputtering
	<ol>
		<li>Switch ON the cooler system and set to 15 &#176;C. Turn ON the pump and refrigeration button, and open the valve connected to the sputtering instrument.</li>
		<li>Set rotation to 10 rpm and switch ON the rotation toggle switch. Set Argon flow to 4 sccm and switch ON the gas toggle switch. Wait until the flow reaches the set value.</li>
		<li>Push the Power button to switch ON the automatic matching network controller and radio frequency power supply.</li>
		<li>On the automatic matching network controller, set load and tune to 50 W each by pushing the Min/Max button and push the button from Manual to Auto.</li>
		<li>On the radio frequency power supply, set RF power to 50 W and push the Start button. 
		NOTE: Wait until the Argon flow reaches the set value and becomes stable before turning on the RF power.</li>
		<li>Check for presence of plasma in the chamber. The formation of plasma is indicated by a glowing purple light in the chamber. If the plasma is not present once the RF power is turned ON, switch OFF Argon for 10 s, and turn it back ON. Repeat until plasma forms in the chamber.</li>
		<li>Gradually increase the RF power with 5 W per 10 s interval until it reaches 75 W. Set the timer to 60 min.</li>
	</ol>
	</li>
	<li>Post-sputtering
	<ol>
		<li>Switch OFF the RF power and rotation. Turn OFF the automatic matching network controller and radio frequency power supply.</li>
		<li>Set Argon flow to 0 and switch OFF the gas toggle switch. Switch OFF the vacuum. 
		NOTE: Wait until the Argon flow reaches 0.1 sccm before switching OFF the vacuum.</li>
		<li>Vent to open the chamber. Make sure the TMP is OFF before venting. Venting while TMP is running will damage the system.</li>
		<li>Take out all samples using tweezer and put in a clean Petri dish. 
		&#8203;CAUTION: Wear mask and glove when handling the inside of the chamber to avoid inhaling small particles of materials.</li>
		<li>Clean the chamber and vacuum for 10 - 15 min to keep the chamber under vacuum condition (free from impurities).</li>
	</ol>
	</li>
</ol>
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/66248/66248fig02.jpg" /> 
Figure 2: Experimental setup. Photograph of the sputtering machine used in this study. <a href="https://www.jove.com/files/ftp_upload/66248/66248fig02large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
3. Characterization
<ol>
	<li>Perform topographic and cross-sectional scanning using Field Emission Scanning Electron Microscope (FESEM, under 3.0 kV operating voltage) to obtain the surface microstructural details and thickness of the sputtered films.</li>
	<li>Perform calculation on composition of the films using data of the energy dispersive X-ray spectra (EDX), attached with the FESEM. Measure Hall voltage in a permanent magnetic field of 0.57&#8239;T and probe currents of 0.8 mA and 10&#8239;mA for Sb2Te3 and Bi2Te3,, respectively to obtain the carrier concentration and conductivity of the films35.</li>
	<li>Perform in-plane measurement of Seebeck coefficient using a similar instrument used by Isotta et al.5. Mount samples with a rectangular geometry of approximately 2 cm x 1.25 cm on the setup. Measure the absolute Seebeck coefficient in 2-contact configuration against a Pt standard, with a temperature gradient of &#8776;25 &#176;C.</li>
</ol>

Deposition of Bi2Te3 and Sb2Te3 Thin Films on Glass Substrates via RF Sputtering

The authors have nothing to disclose.

The technique presented in this paper presents no significant difficulty in setting up the equipment and implementation. However, several critical steps need to be highlighted. As mentioned in step 2.2.10 of the protocol, optimum vacuum condition is key to produce high quality thin films with less contamination as vacuum removes residual oxygen in the chamber37. The presence of oxygen can cause cracks in the films called stress cracking indicating the importance of high vacuum system in sputtering...

Thermoelectric (TE) materials have been attracting a considerable amount of research interest regarding their ability to convert thermal energy into electricity via the Seebeck effect1 and refrigeration via Peltier cooling2. The conversion efficiency of TE material is determined by the temperature difference between the hot end of the TE leg and the cold end. Generally, the higher the temperature difference, the higher the TE figure of merit and the higher its efficiency3. TE works with no requirement for additional mechanical parts involving gas or liquid in its process, producing no waste or pollution, making it environmentally safe and considered a green energy harvesting system.
Bismuth telluride, Bi2Te3, and its alloys remain the most important class of TE material. Even in thermoelectric power generation, such as the recovery of waste heat, Bi2Te3 alloys are most commonly used due to their superior efficiency up to 200 &#176;C4 and remain an excellent TE material at ambient temperature despite the zT value of more than 2 in various TE materials5. Several published papers have studied the TE properties of this material, which shows that the stoichiometric Bi2Te3 has a negative Seebeck coefficient6,7,8, indicating n-type properties. However, this compound can be adjusted to p- and n-type by alloying with antimony telluride (Sb2Te3) and bismuth selenide (Bi2Se3), respectively, which can increase their bandgap and reduce bipolar effects9.
Antimony telluride, Sb2Te3 is another well-established TE material with high figure of merit at low temperature. While stoichiometric Bi2Te3 is a great TE with n-type properties, Sb2Te3 has p-type properties. In some cases, the properties of TE materials often depend on the atomic composition of the material such as the n-type Te-rich Bi2Te3, but a p-type Bi-rich Bi2Te3 due to BiTe antisite acceptor defects4. However, Sb2Te3 is always p-type due to comparatively low formation energy of SbTe antisite defects, even in Te-rich Sb2Te34. Thus, these two materials become suitable candidates to fabricate p-n module of thermoelectric generator for various applications.
The current conventional TEGs are made of diced ingots of n-type and p-type semiconductors connected vertically in series10. They have only been used in niche fields due to their low efficiency and bulky, rigid nature. Over time, researchers have started to explore thin film structures for better performance and application. It is reported that thin film TE have advantages over their bulky counterpart such as higher zT due to their low thermal conductivity11,12, less amount of material and easier integration with integrated circuit12. As a result, niche TE research on thin film thermoelectric devices has been on the rise benefitting from the advantages of nanomaterial structure13,14.
Microfabrication of thin film is important to attain high performance TE materials. Various deposition approaches have been researched and developed including chemical vapor deposition15, atomic layer deposition16,17, pulsed laser deposition18,19,20, screen printing8,21, and molecular beam epitaxy22 to serve this purpose. However, the majority of these techniques suffer from high operation cost, complex growth process or complicated material preparation. On the contrary, magnetron sputtering is a cost-effective approach for producing high-quality thin films that are denser, exhibit smaller grain size, have better adhesion, and high uniformity23,24,25.
Magnetron sputtering is one of the plasma-based physical vapor deposition (PVD) processes which is widely used in various industrial applications. Sputtering process works when sufficient voltage is applied to a target (cathode), ions from the glow discharge plasma bombards the target and release not only secondary electrons, but also atoms of the cathode materials which eventually impact the surface of the substrate and condense as a thin film. Sputtering process was first commercialized in 1930s and improved in 1960s, gaining significant interest due to its ability to deposit wide range of materials using direct current (DC) and RF sputtering26,27. The magnetron sputtering overcomes low deposition rate and high substrate heating impact by utilizing magnetic field. The strong magnet confines the electrons in the plasma at or near the surface of the target and prevent damage to the formed thin film. This configuration preserves the stoichiometry and thickness uniformity of the deposited thin film28.
The preparation of Bi2Te3 and Sb2Te3 thermoelectric thin films using magnetron sputtering method has also been extensively studied, incorporating technique such as doping4,29,30 and annealing31 in the procedures, leading to different performance and quality. Study by Zheng et al.32 uses thermally induced diffusion method to diffuse Ag-doped Bi and Te layer which were sputtered separately. This method enables precise control on the composition of the thin films and the diffusion of Te by thermal induction protects the Te from being volatilized. The properties of the thin films can also be enhanced by pre-coating process33 before sputtering which results in better electrical conductivity due to high carrier mobility, consequently enhancing the power factor. Other than that, study by Chen et al.34 improved the thermoelectric performance of sputtered Bi2Te3 by doping Se via post-selenization diffusion reaction method. During the process, Se vaporizes and diffuses into the Bi-Te thin films to form Bi-Te-Se films, which results in 8-fold higher power factor than undoped Bi2Te3.
This paper describes our experimental setup and procedure for the RF magnetron sputtering technique to deposit Bi2Te3 and Sb2Te3 thin films on glass substrates. Sputtering was performed in a top-down configuration as shown in the schematic diagram in Figure 1, cathode was mounted at an angle to the substrate normal, leading to a more concentrated and convergent plasma to the substrate. The films were systematically characterized using FESEM, EDX, Hall effect and Seebeck coefficient measurement to study their surface morphology, thickness, composition, and thermoelectric properties.
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/66248/66248fig01.jpg" /> 
Figure 1: A schematic of the top-down configuration sputter. The diagram was designed according, but not to scale, to the actual sputtering configuration available for this study including the arrangement of glass substrates to be sputtered viewed from the top. <a href="https://www.jove.com/files/ftp_upload/66248/66248fig01large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>

<table><tbody><tr><td>Acetone</td><td>Chemiz (M) Sdn. Bhd.</td><td>1910151</td><td>Liquid, Flammable</td></tr><tr><td>Antimony Telluride, Sb2Te3</td><td>China Rare Metal Material Co.,Ltd</td><td>C120222-0304</td><td>Diameter 50.8 mm, Thickness 6.35 mm, 99.999% purity</td></tr><tr><td>Bismuth Telluride, Bi2Te3</td><td>China Rare Metal Material Co.,Ltd</td><td>CB151208-0501</td><td>Diameter 50.8 mm, Thickness 4.25 mm, 99.999% purity</td></tr><tr><td>Ethanol</td><td>Chemiz (M) Sdn. Bhd.</td><td>2007081</td><td>Liquid, Flammable</td></tr><tr><td>Field Emission Scanning Electron Microscope</td><td>Zeiss</td><td>MERLIN</td><td>Equipped with EDX</td></tr><tr><td>Hall effect measurement system</td><td>Aseptec Sdn. Bhd.</td><td>HMS ECOPIA 3000</td><td>-</td></tr><tr><td>Handheld digital multimeter</td><td>Prokits Industries Sdn. Bhd.</td><td>303-150NCS</td><td>-</td></tr><tr><td>HMS-3000</td><td>Aseptec Sdn Bhd.</td><td>HMS ECOPIA 3000</td><td>Hall effect measurement software</td></tr><tr><td>Linseis_TA</td><td>Linseis Messger&amp;auml;te GmbH</td><td>LSR-3</td><td>Linseis thermal analysis software</td></tr><tr><td>Methanol</td><td>Chemiz (M) Sdn. Bhd.</td><td>2104071</td><td>Liquid, Flammable</td></tr><tr><td>RF-DC magnetron sputtering</td><td>Kurt J. Lesker Company</td><td>-</td><td>Customized hybrid system</td></tr><tr><td>Seebeck coefficient measurement system</td><td>Linseis Messger&amp;auml;te GmbH</td><td>LSR-3</td><td>-</td></tr><tr><td>SmartTiff</td><td>Carl Zeiss Microscopy Ltd</td><td>-</td><td>SEM image thickness measurement software</td></tr><tr><td>Ultrasonic bath</td><td>Fisherbrand</td><td>FB15055</td><td>-</td></tr><tr><td>UV ozone cleaner</td><td>Ossila Ltd</td><td>L2002A3-UK</td><td>-</td></tr></tbody></table>

fabrication of bi2te3 and sb2te3 thermoelectric thin films using radio frequency magnetron sputtering technique

Through various studies on thermoelectric (TE) materials, thin film configuration gives superior advantages over conventional bulk TEs, including adaptability to curved and flexible substrates. Several different thin film deposition methods have been explored, yet magnetron sputtering is still favorable due to its high deposition efficiency and scalability. Therefore, this study aims to fabricate a bismuth telluride (Bi2Te3) and antimony telluride (Sb2Te3) thin film via the radio frequency (RF) magnetron sputtering method. The thin films were deposited on soda lime glass substrates at ambient temperature. The substrates were first washed using water and soap, ultrasonically cleaned with methanol, acetone, ethanol, and deionized water for 10 min, dried with nitrogen gas and hot plate, and finally treated under UV ozone for 10 min to remove residues before the coating process. A sputter target of Bi2Te3 and Sb2Te3 with Argon gas was used, and pre-sputtering was done to clean the target&#39;s surface. Then, a few clean substrates were loaded into the sputtering chamber, and the chamber was vacuumed until the pressure reached 2 x 10-5 Torr. The thin films were deposited for 60 min with Argon flow of 4 sccm and RF power at 75 W and 30 W for Bi2Te3 and Sb2Te3, respectively. This method resulted in highly uniform n-type Bi2Te3 and p-type Sb2Te3 thin films.

Cross-sectional micrographs of as-deposited Bi2Te3 and Sb2Te3 thin films were recorded using FESEM as shown in Figure 3A and Figure 3B, respectively. The surface of the overall film appears uniform and smooth. It is apparent that the crystal grains of the Bi2Te3 thin film were hexagonal, conforming the crystal structure of Bi2Te3 while the crystal grains of the Sb2...

Author Spotlight: Advancements in High-Performance Thermoelectric Thin Films Through Radio Frequency Magnetron Sputtering

The manuscript describes a protocol for radio frequency magnetron sputtering of Bi2Te3 and Sb2Te3 thermoelectric thin films on glass substrates, which represents a reliable deposition method that provides a wide range of applications with the potential for further development.

Fabrication of Bi2Te3 and Sb2Te3 Thermoelectric Thin Films using Radio Frequency Magnetron Sputtering Technique

Through various studies on thermoelectric (TE) materials, thin film configuration gives superior advantages over conventional bulk TEs, including ...

fabrication-bi2te3-sb2te3-thermoelectric-thin-films-using-radio

Research

JoVE Journal

Engineering

2.6K Views.  Universiti Kebangsaan Malaysia. Ons onderzoek richt zich op het vervaardigen van hoogwaardige dunne films voor thermo-elektrische generatoren om restwarmte terug te winnen en om te zetten in elektriciteit. Er zijn verschillende dunnefilmafzettingstechnieken onderzocht en ontwikkeld, waaronder radiofrequente magnetronsputteren die in staat is om robuuste dunne films met een hoge dichtheid te produceren met een betere hechting en hoge uniformiteit. Deze methode vereist geen smelten en verdampen van de doelmaterialen, waardoor...

Video: Auteur in de schijnwerpers: vooruitgang in hoogwaardige thermo-elektrische dunne films door middel van radiofrequente magnetronsputteren

Sputter Growth and Characterization of Metamagnetic B2-ordered FeRh Epilayers

Chemically ordered alloys are useful in a variety of magnetic nanotechnologies. They are most conveniently prepared at an industrial scale using sputtering techniques. Here we describe a method for preparing epitaxial thin films of B2-ordered FeRh by sputter deposition onto single crystal MgO substrates. Deposition at a slow rate onto a heated substrate allows time for the adatoms to both settle into a lattice with a well-defined epitaxial relationship with the substrate and also to find their proper places in the Fe and Rh sublattices of the B2 structure. The structure is conveniently characterized with X-ray reflectometry and diffraction and can be visualised directly using transmission electron micrograph cross-sections. B2-ordered FeRh exhibits an unusual metamagnetic phase transition: the ground state is antiferromagnetic but the alloy transforms into a ferromagnet on heating with a typical transition temperature of about 380 K. This is accompanied by a 1% volume expansion of the unit cell: isotropic in bulk, but laterally clamped in an epilayer. The presence of the antiferromagnetic ground state and the associated first order phase transition is very sensitive to the correct equiatomic stoichiometry and proper B2 ordering, and so is a convenient means to demonstrate the quality of the layers that can be deposited with this approach. We also give some examples of the various techniques by which the change in phase can be detected.

A method to prepare epitaxial layers of ordered alloys by sputtering is described. The B2-ordered FeRh compound is used as an example, as it displays a metamagnetic transition that depends sensitively on the degree of chemical order and the exact composition of the alloy.

Chemically ordered alloys are useful in a variety of magnetic nanotechnologies. They are most conveniently prepared at an industrial scale using ...

Formation of Thick Dense Yttrium Iron Garnet Films Using Aerosol Deposition

Aerosol deposition (AD) is a thick-film deposition process that can produce layers up to several hundred micrometers thick with densities greater than 95% of the bulk. The primary advantage of AD is that the deposition takes place entirely at ambient temperature; thereby enabling film growth in material systems with disparate melting temperatures. This report describes in detail the processing steps for preparing the powder and for performing AD using the custom-built system. Representative characterization results are presented from scanning electron microscopy, profilometry, and ferromagnetic resonance for films grown in this system. As a representative overview of the capabilities of the system, focus is given to a sample produced following the described protocol and system setup. Results indicate that this system can successfully deposit 11 &#181;m thick yttrium iron garnet films that are &#160;&#62; 90% of the bulk density during a single 5 min deposition run. A discussion of methods to afford better control of the aerosol and particle selection for improved thickness and roughness variations in the film is provided.

This report describes the use of a custom-built system to perform aerosol deposition of thick films of yttrium iron garnet onto sapphire substrates at RT. The deposited films are characterized using scanning electron microscopy, profilometry, and ferromagnetic resonance to give a representative overview of the capabilities of the technique.

Aerosol deposition (AD) is a thick-film deposition process that can produce layers up to several hundred micrometers thick with densities greater than 95% ...

Speciation and Bioavailability Measurements of Environmental Plutonium Using Diffusion in Thin Films

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can potentially contribute to the exposure of biota and humans. The diffusive gradients in thin films technique is introduced here for in-situ measurements of Pu bioavailability and speciation. A diffusion cell constructed for laboratory experiments with Pu and the newly developed protocol make it possible to simulate the environmental behavior of Pu in model solutions of various chemical compositions. Adjustment of the oxidation states to Pu(IV) and Pu(V) described in this protocol is essential in order to investigate the complex redox chemistry of plutonium in the environment. The calibration of this technique and the results obtained in the laboratory experiments enable to develop a specific DGT device for in-situ Pu measurements in freshwaters. Accelerator-based mass-spectrometry measurements of Pu accumulated by DGTs in a karst spring allowed determining the bioavailability of Pu in a mineral freshwater environment. Application of this protocol for Pu measurements using DGT devices has a large potential to improve our understanding of the speciation and the biological transfer of Pu in aquatic ecosystems.

The technique of diffusive gradients in thin films (DGT) is proposed for speciation studies of plutonium. This protocol describes diffusion experiments probing the behavior of Pu(IV) and Pu(V) in presence of organic matter. DGTs deployed in a karstic spring allow assessment of the bioavailability of Pu.

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can ...

Seedless Growth of Bismuth Nanowire Array via Vacuum Thermal Evaporation

Here a seedless and template-free technique is demonstrated to scalably grow bismuth nanowires, through thermal evaporation in high vacuum at RT. Conventionally reserved for the fabrication of metal thin films, thermal evaporation deposits bismuth into an array of vertical single crystalline nanowires over a flat thin film of vanadium held at RT, which is freshly deposited by magnetron sputtering or thermal evaporation. By controlling the temperature of the growth substrate the length and width of the nanowires can be tuned over a wide range. Responsible for this novel technique is a previously unknown nanowire growth mechanism that roots in the mild porosity of the vanadium thin film. Infiltrated into the vanadium pores, the bismuth domains (~ 1 nm) carry excessive surface energy that suppresses their melting point and continuously expels them out of the vanadium matrix to form nanowires. This discovery demonstrates the feasibility of scalable vapor phase synthesis of high purity nanomaterials without using any catalysts.

A protocol for seedless and high yield growth of bismuth nanowire arrays through vacuum thermal evaporation technique is presented.

Here a seedless and template-free technique is demonstrated to scalably grow bismuth nanowires, through thermal evaporation in high vacuum at RT. ...

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.

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 ...

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 ...

Solution-Processed "Silver-Bismuth-Iodine" Ternary Thin Films for Lead-Free Photovoltaic Absorbers

Bismuth-based hybrid perovskites are regarded as promising photo-active semiconductors for environment-friendly and air-stable solar cell applications. However, poor surface morphologies and relatively high bandgap energies have limited their potential. Silver-bismuth-iodine (Ag-Bi-I) is a promising semiconductor for optoelectronic devices. Therefore, we demonstrate the fabrication of Ag-Bi-I ternary thin films using material solution processing. The resulting thin films exhibit controlled surface morphologies and optical bandgaps according to their thermal annealing temperatures. In addition, it has been reported that Ag-Bi-I ternary systems crystallize to AgBi2I7, Ag2BiI5, etc. according to the ratio of the precursor chemicals. The solution-processed AgBi2I7 thin films exhibit a cubic-phase crystal structure, dense, pinhole-free surface morphologies with grains ranging in size from 200 to 800 nm, and an indirect bandgap of 1.87 eV. The resultant AgBi2I7 thin films show good air stability and energy band diagrams, as well as surface morphologies and optical bandgaps suitable for lead-free and air-stable single-junction solar cells. Very recently, a solar cell with 4.3% power conversion efficiency was obtained by optimizing the Ag-Bi-I crystal compositions and solar cell device architectures.

Herein, we present detailed protocols for solution-processed silver-bismuth-iodine (Ag-Bi-I) ternary semiconductor thin films fabricated on TiO2-coated transparent electrodes and their potential application as air-stable and lead-free optoelectronic devices.

Bismuth-based hybrid perovskites are regarded as promising photo-active semiconductors for environment-friendly and air-stable solar cell applications. ...

Chemistry

Radio Frequency Magnetron Sputtering of GdBa2Cu3O7&#8722;&#948;/ La0.67Sr0.33MnO3 Quasi-bilayer Films on SrTiO3 (STO) Single-crystal Substrates

Here, we demonstrate a method of coating ferromagnetic La0.67Sr0.33MnO3 (LSMO) nanoparticles on (001) SrTiO3 (STO) single-crystal substrates by radio frequency (RF) magnetron sputtering. LSMO nanoparticles were deposited with diameters from 10 to 20 nm and heights between 20 and 50 nm. At the same time, (Gd) Ba2Cu3O7&#8722;&#948; ((Gd) BCO) films were fabricated on both undecorated and LSMO nanoparticle decorated STO substrates using RF magnetron sputtering. This report also describes the properties of GdBa2Cu3O7&#8722;&#948;/ La0.67Sr0.33MnO3 quasi-bilayer films structures (e.g., crystalline phase, morphology, chemical composition); magnetization, magneto-transport, and superconducting transport properties were also evaluated.

Radio Frequency Magnetron Sputtering of GdBa2Cu3O7ÃƒÆ’Ã‚Â¢Ãƒâ€¹Ã¢â‚¬Â 'ÃƒÆ’Ã…Â½ Â´/ La0.67Sr0.33MnO3 Quasi-bilayer Films on SrTiO3 STO Single-crystal Substrates

Here, we present a protocol to grow LSMO nanoparticles and (Gd) BCO films on (001) SrTiO3 (STO) single-crystal substrates by radio frequency (RF)-sputtering.

Here, we demonstrate a method of coating ferromagnetic La0.67Sr0.33MnO3 (LSMO) nanoparticles on (001) SrTiO3 (STO) single-crystal substrates by radio ...

Fabrication of Schottky Diodes on Zn-polar BeMgZnO/ZnO Heterostructure Grown by Plasma-assisted Molecular Beam Epitaxy

Heterostructure field effect transistors (HFETs) utilizing a two dimensional electron gas (2DEG) channel have a great potential for high speed device applications. Zinc oxide (ZnO), a semiconductor with a wide bandgap (3.4 eV) and high electron saturation velocity has gained a great deal of attention as an attractive material for high speed devices. Efficient gate modulation, however, requires high-quality Schottky contacts on the barrier layer. In this article, we present our Schottky diode fabrication procedure on Zn-polar BeMgZnO/ZnO heterostructure with high density 2DEG which is achieved through strain modulation and incorporation of a few percent Be into the MgZnO-based barrier during growth by molecular beam epitaxy (MBE). To achieve high crystalline quality, nearly lattice-matched high-resistivity GaN templates grown by metal-organic chemical vapor deposition (MOCVD) are used as the substrate for the subsequent MBE growth of the oxide layers. To obtain the requisite Zn-polarity, careful surface treatment of GaN templates and control over the VI/II ratio during the growth of low temperature ZnO nucleation layer are utilized. Ti/Au electrodes serve as Ohmic contacts, and Ag electrodes deposited on the O2 plasma pretreated BeMgZnO surface are used for Schottky contacts.

Attainment of high-quality Schottky contacts is imperative for achieving efficient gate modulation in heterostructure field effect transistors (HFETs). We present the fabrication methodology and characteristics of Schottky diodes on Zn-polar BeMgZnO/ZnO heterostructures with high-density two dimensional electron gas (2DEG), grown by plasma-assisted molecular beam epitaxy on GaN templates.

Heterostructure field effect transistors (HFETs) utilizing a two dimensional electron gas (2DEG) channel have a great potential for high speed device ...

Synthesis of High-ZT Thermoelectric Materials via Mechanochemical Methods

Demonstrating the Simplicity and In Situ Temperature Monitoring of the Mechanochemical Synthesis of Metal Chalcogenides Suitable for Thermoelectrics

Mechanochemical synthesis is an extremely useful strategy to reach thermoelectric materials due to its solvent-free one-step character, as the targeted thermoelectricity (TE) materials in a nanocrystalline format can be prepared by mere high-energy milling of elemental precursors. Nevertheless, the subsequent densification method (e.g., spark plasma sintering or hot pressing) is required afterward, similarly to other synthetic methodologies. In this study, the simplicity of mechanochemical synthesis is&#160;presented for two selected metal chalcogenides, namely copper sulfide (Cu1.8S, digenite) and tin selenide (SnSe, svetlanaite), which are known for high ZT values. These compounds can be prepared via a mechanically induced self-propagating reaction (MSR), which is a combustion-like process instantly yielding the products in a very short timeframe (within 1 min). The occurrence of MSR can be well-tracked by in situ temperature monitoring since an abrupt temperature increase occurs at the moment of MSR. We have developed a device which is capable of monitoring the temperature inside the milling jar every 80 ms during planetary ball milling, and it is therefore possible to very precisely track the moment of MSR ignition. The developed device presents an improvement in the monitoring capabilities in comparison with commercially available analogs. This contribution aims to provide a visual insight into all steps, with simple high-energy ball milling of elements to reach TE materials and in situ temperature monitoring being the central points.

Here, we present a protocol to synthesize two metal chalcogenides (Cu1.8S and SnSe) suitable for thermoelectrics via an ultrafast (second-range), solvent-free, and one-step mechanochemical synthesis using elemental precursors. Simultaneously, we demonstrate the monitoring of the temperature in the jar during planetary ball milling in situ by the newly developed device.

Mechanochemical synthesis is an extremely useful strategy to reach thermoelectric materials due to its solvent-free one-step character, as the targeted ...

Fabrication of Bi₂Te₃ and Sb₂Te₃ Thermoelectric Thin Films using Radio Frequency Magnetron Sputtering Technique

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