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The authors are grateful for the support provided by the Universiti Kebangsaan Malaysia, under grant GGPM-2022-069. The authors also thank the Solar Energy Research Institute (SERI), Universiti Kebangsaan Malaysia (UKM), for technical support and access to laboratory facilities throughout this study. The authors acknowledge the Centre for Research and Instrumentation Management (CRIM) for providing the XRD and FESEM&#8211;EDX facilities. In addition, the authors sincerely acknowledge Universiti Sains Islam Malaysia (USIM) for access to the Seebeck/resistivity measurement system used for Seebeck coefficient and electrical resistivity measurements. Finally, the authors extend their appreciation to all colleagues and staff members who contributed to the successful completion of this project.

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The authors declare no competing financial interests or other conflicts of interest.

This study demonstrated an RF co-sputtering workflow for tailoring the TE behavior of Bi2Te3 thin films by controlling Mn RF input while maintaining a constant Bi2Te3 target power. XRD confirmed the presence of the rhombohedral Bi2Te3 phase (JCPDS No. 15-0863) with a preferred (015) orientation across all samples. The systematic shift of the (015) reflection toward higher 2&#952; values is consistent with Mn-related lattice contraction and possible Mn inco...

Thermoelectric (TE) materials play a crucial role in the sustainable conversion of heat into electrical energy, primarily through the Seebeck and Peltier effects. The performance of TE materials is typically evaluated using the power factor (PF = S2/ρ), where S is the Seebeck coefficient and ρ is the electrical resistivity1,2. A high S coupled with low ρ indicates efficient carrier transport, which is essential for applications such as waste-heat recovery, micro-power generation, and solid-state cooling in industrial systems and microelectronics3,4,5.
Among various TE materials, bismuth telluride (Bi2Te3) is notable for its efficiency in near-room-temperature applications. However, its practical deployment is limited by brittleness, restricted mechanical flexibility, and a moderate figure of merit (zT), which contribute to challenges in large-scale implementation2. Recent advances in thin-film fabrication technologies, particularly magnetron sputtering, provide promising approaches to address these limitations. Thin films enable improved control over composition and microstructure, which can enhance carrier mobility and mechanical flexibility, both of which are important for high-efficiency TE devices6. The ability to tailor these properties using radiofrequency (RF) magnetron sputtering has been demonstrated previously, supporting its use for producing uniform Bi2Te3 thin films with tunable thicknesses and doping levels7.
Cationic doping, particularly with manganese (Mn), has emerged as a promising strategy for improving the TE properties of Bi2Te3. Although research on Mn-doped Bi2Te3 remains less extensive than studies involving other dopants, evidence from related systems suggests that Mn incorporation can improve both electrical and structural properties8. Mn incorporation has been reported to influence carrier concentration and mobility, affecting the Seebeck coefficient and electrical conductivity, which together determine the PF of TE material9. In addition, Mn incorporation has been discussed in terms of substitutional or defect-associated incorporation mechanisms that may introduce lattice strain and point defects. These modifications can enhance phonon scattering and potentially reduce lattice thermal conductivity, both of which are important contributors to TE performance10. Research on related Mn-doped compounds such as Bi2Si2Te6 suggests that Mn may also improve charge transport and introduce localized magnetic moments, which may strengthen phonon-scattering effects and reduce bipolar conduction11. Consequently, the influence of Mn on microstructural evolution, defect formation, and grain growth is important for improving the mechanical and thermal stability of TE materials10,12.
However, excessive Mn incorporation can promote secondary phases such as MnTe and complicate transport behavior13; therefore, Mn input must be carefully controlled14. In addition, Mn may introduce acceptor states within the Bi2Te3 lattice and potentially alter conduction behavior through suppression of topological surface transport, opening of a gap, reduced free-carrier density, and a crossover from metallic to insulating or localized conduction under sufficient doping15,16. These considerations highlight the importance of controlling Mn incorporation during sputtering to establish reliable structure–property relationships17.
Recent studies have demonstrated that Mn can be incorporated into Bi2Te3-based thin films and can measurably influence structure and electronic transport. Bi2−xMnxTe3 thin films exhibit Mn-dependent changes in structural and electrical properties18, while Mn:Bi2Te3 thin films have also been investigated through transport measurements, indicating that Mn incorporation can occur without fully suppressing the host Bi2Te3 phase19. More recently, magnetron sputtering has enabled the preparation of nanocrystalline Mn-doped Bi2Te3 thin films, supporting the feasibility of Mn incorporation using scalable thin-film deposition approaches20. However, compared with representative sputtered n-type Bi2Te3 thin films optimized through texture engineering, vacancy-defect modulation, and carrier engineering, systematic optimization of Mn-doped Bi2Te3 thin films remains comparatively underexplored7,21. This gap motivated the controlled Mn-input study presented here.
In this study, Mn-doped Bi2Te3 thin films were prepared by RF magnetron co-sputtering using a controlled Mn-input series and were evaluated using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), and temperature-dependent Seebeck coefficient and electrical resistivity measurements. Figure 1 schematically illustrates the co-sputtering configuration used in this work. The aim was to use a consistent sputtering framework to examine how Mn input influences film microstructure and PF-related transport behavior under comparable processing conditions22.
<img alt="Sputtering setup diagram for thin films; Bi₂Te₃, Mn targets on substrates for material deposition." class="xfigimg" src="/files/ftp_upload/71082/71082fig1.jpg" data-altupdatedat="1787630408000" data-alt="Figure 1"> 
Figure 1. Schematic of the RF magnetron co-sputtering configuration used for Mn-doped Bi2Te3 thin-film deposition. Schematic representation of the co-sputtering arrangement showing the Bi2Te3 target, Mn target, substrate holder, and substrate positioning inside the deposition chamber. <a href="https://www.jove.com/files/ftp_upload/71082/71082fig1large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>

<table><tbody><tr><td>Acetone (&amp;ge;99.5%)</td><td>Merck</td><td>100012</td><td>Substrate cleaning solvent</td></tr><tr><td>Aluminum foil</td><td>Pospaperroll</td><td>86871915</td><td>Chamber lining and substrate-holder covering</td></tr><tr><td>Argon gas (Ar)</td><td>Gaslink Industrial Gases Sdn. Bhd.</td><td>N/A (supplied by distributor)</td><td>Sputtering working gas; 4 sccm flow; grade 5.0 (99.999%)</td></tr><tr><td>Bismuth telluride sputtering target, 50.8 mm diameter, 4.25 mm thickness, 99.999%</td><td>Changsha Xinkang Advanced Materials Co., Ltd.</td><td>xk-Bi&lt;sub&gt;2&lt;/sub&gt;Te&lt;sub&gt;3&lt;/sub&gt;</td><td>Bi&lt;sub&gt;2&lt;/sub&gt;Te&lt;sub&gt;3&lt;/sub&gt; target; fixed RF power = 100 W</td></tr><tr><td>Deionized water</td><td>In-house</td><td>N/A</td><td>Substrate rinsing and ultrasonic cleaning</td></tr><tr><td>Energy-dispersive X-ray spectroscopy detector</td><td>Integrated with FESEM system</td><td>N/A</td><td>Thin-film compositional analysis</td></tr><tr><td>Field-emission scanning electron microscope</td><td>Carl Zeiss</td><td>SUPRA 55VP</td><td>Surface microstructure imaging</td></tr><tr><td>Glass substrates, soda-lime glass, 1.1 mm thickness</td><td>Mevid</td><td>B105-2002</td><td>Substrate for thin-film deposition</td></tr><tr><td>Hot plate</td><td>IKA</td><td>C-MAG HS 7</td><td>Substrate drying at 393 K</td></tr><tr><td>Isopropyl alcohol (&amp;ge;99.8%)</td><td>Merck</td><td>109634</td><td>Substrate cleaning solvent</td></tr><tr><td>Laboratory detergent</td><td>Merck</td><td>107553</td><td>Initial substrate cleaning</td></tr><tr><td>Coolant circulation unit</td><td>Fisher Scientific</td><td>250LCU</td><td>Cooling circulation for sputter guns</td></tr><tr><td>Methanol (&amp;ge;99.9%)</td><td>Merck</td><td>106009</td><td>Substrate cleaning solvent</td></tr><tr><td>Manganese sputtering target, 50.8 mm diameter, 5.08 mm thickness, 99.999%</td><td>Hunan Boyu Technology Co., Ltd.</td><td>N/A</td><td>Mn target; RF power varied from 0 to 15 W</td></tr><tr><td>Multimeter</td><td>RS PRO</td><td>EN61010-1 CATIII</td><td>Electrical isolation verification</td></tr><tr><td>Nitrogen gas (N&lt;sub&gt;2&lt;/sub&gt;)</td><td>Gaslink Industrial Gases Sdn. Bhd.</td><td>N/A (supplied by distributor)</td><td>Substrate drying after cleaning; grade 4.0 (99.99%)</td></tr><tr><td>Petri dish lid</td><td>Merck</td><td>41121812</td><td>Chamber viewing-window protection; approximately 94 mm diameter &amp;times; 16 mm height</td></tr><tr><td>RF magnetron sputtering system</td><td>Custom-built</td><td>N/A</td><td>Co-sputtering of Bi&lt;sub&gt;2&lt;/sub&gt;Te&lt;sub&gt;3&lt;/sub&gt; and Mn thin films</td></tr><tr><td>Seebeck/resistivity measurement system with platinum adapter</td><td>Linseis</td><td>LSR-3 (LSR L31)</td><td>Seebeck coefficient and electrical resistivity measurements</td></tr><tr><td>Tweezers</td><td>Fisher Scientific</td><td>10-316B</td><td>Handling cleaned substrates</td></tr><tr><td>Ultrasonic bath</td><td>Elma</td><td>ElmaSonic S30H</td><td>Solvent cleaning for methanol, acetone, isopropyl alcohol, and DI water</td></tr><tr><td>UV&amp;ndash;ozone cleaner</td><td>Novascan Technologies</td><td>PSDP-UV4</td><td>Substrate surface treatment</td></tr><tr><td>Vacuum storage container</td><td>AS ONE Corporation</td><td>VM</td><td>Sample storage after deposition</td></tr><tr><td>Stylus profilometer</td><td>Bruker</td><td>DektakXT</td><td>Thin-film thickness measurement</td></tr><tr><td>X-ray diffractometer</td><td>Bruker</td><td>D8 ADVANCE</td><td>&amp;theta;&amp;ndash;2&amp;theta; XRD scans using Cu K&amp;alpha; radiation</td></tr><tr><td>DIFFRAC.EVA</td><td>Bruker</td><td>DIFFRAC.EVA version 8</td><td>Peak fitting, diffraction analysis, and graph plotting</td></tr><tr><td>Origin</td><td>OriginLab</td><td>OriginPro (64-bit)</td><td>Peak fitting and graph plotting</td></tr></tbody></table>

improving thermoelectric properties of bi2te3 thin films by manganese co-sputtering

Improving Thermoelectric Properties of Bi2Te3 Thin Films By Manganese Co-Sputtering

Bi2Te3 remains a benchmark n-type thermoelectric (TE) material for low-temperature energy conversion, but its small band gap can reduce efficiency because of thermally generated parasitic carriers. Elemental doping has been explored to improve TE performance, although systematic studies on manganese (Mn)-doped Bi2Te3 thin films remain limited. In this study, a radiofrequency magnetron co-sputtering workflow was used to fabricate Mn-doped Bi2Te3 thin films by varying Mn target power while maintaining constant Bi2Te3 deposition conditions. Structural, microstructural, compositional, and TE transport properties were evaluated using X-ray diffraction, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and temperature-dependent transport measurements. X-ray diffraction confirmed retention of the rhombohedral Bi2Te3 phase with a preferred (015) orientation, while peak shifts toward higher 2&#952; values were consistent with Mn-related lattice contraction. All films exhibited negative Seebeck coefficients, confirming n-type conduction. Increasing Mn doping enhanced the magnitude of the Seebeck coefficient but also increased electrical resistivity, demonstrating a transport tradeoff. The film deposited at 5 W Mn power achieved the highest power factor of 529.33 &#181;W m&#8722;1 K&#8722;2 at 523 K because of its low resistivity combined with adequate thermopower. These results demonstrate that moderate Mn incorporation can improve the power-factor-related performance of Bi2Te3 thin films within the measured temperature range.

Representative outcomes are presented for the Mn power series (0, 5, 10, 15 W), using the undoped film (0 W) as the control condition for structural and transport comparisons.
Crystal structure (XRD) 
XRD patterns confirm that all samples retained the rhombohedral Bi2Te3 phase (JCPDS No. 15-0863) across the Mn power series, as shown in Figure 4. The dominant reflections, including a strong (015) preferred orientation, indi...

A radiofrequency co-sputtering protocol was developed to fabricate manganese-doped Bi2Te3 thin films and evaluate how manganese input influences structural and thermoelectric transport properties. Moderate manganese incorporation improved film uniformity and power-factor-related transport behavior, while higher manganese input increased structural disorder and resistivity.

Bi2Te3 remains a benchmark n-type thermoelectric (TE) material for low-temperature energy conversion, but its small band gap can reduce efficiency because ...

My research examine the change in the thermoelectric performance of the manganese-doped bismuth telluride thin film deposited through control co-sputtering. Existing methods failed to adequately examine the impact of the manganese doping on the bismuth telluride thin film. So this protocol addresses this gap through systematic investigation.After placing the prepared and cleaned soda lime glass substrates on the rotating substrate holder, close the chamber door and initiate pump down. Apply gentle pressure around the chamber door at the start to ensure proper sealing and confirm the pressure drop on the gauge. Continue pumping until the chamber pressure reaches less than or equal to five times 10 to the power of negative three torr.Switch on the cooling system and set the temperature to 288 Kelvin to ensure continuous circulation of recirculated deionized water through both sputter guns prior to plasma ignition. Introduce high purity argon gas and allow it to stabilize for approximately two to five minutes, or until it remains steady at greater than or equal to 3.9 standard cubic centimeters per minute. Set the substrate rotation to 10 RPM in a single fixed direction and maintain continuous rotation throughout pre-sputtering and deposition.Power on the radiofrequency power supply and the matching network controller. Adjust the matching network settings for both radiofrequency guns using the minimum or maximum function until the load value and the tune value reach 50 watts. Switch the controller mode from manual to auto-matching.Set the radiofrequency power to 50 watts on the bismuth telluride gun and 10 watts on the manganese gun before plasma ignition. Minimize reflected power before plasma ignition, keeping it at or below five watts. Ignite the plasma for both guns and confirm stable plasma by observing a steady glow maintained for approximately one to two minutes without visible flicker or sudden pressure spikes.Once stable plasma was achieved at both guns, pre-sputter both targets for 15 minutes to remove surface contamination and native oxides after stable plasma is achieved. Remove the test substrates after pre-sputtering. Before loading the substrates for the deposition run, remove dust from the chamber interior and the sample holder region using a clean rubber blower.Keep the viewing window protected with a clean Petri dish lid for plasma observation. Inspect the targets to ensure that they are properly seated, centered, and in good condition. Verify that each target is firmly clamped and properly centered within the sputter gun.Place the cleaned substrates symmetrically near the outer region of the rotating holder at approximately 5 to 10 millimeters from the holder center. Align the longer side of each substrate parallel to the holder edge. Fix the target to substrate distance at 55 millimeters for both sputter guns.Pump down the chamber and continue evacuation for at least five hours or until the base pressure stabilizes at the target value. Confirm base pressure stability when the pressure drift remains less than or equal to 5%over approximately 10 minutes and the base pressure reaches five times 10 to the power of negative five torr or lower. Stabilize the cooling system at 288 Kelvins after reaching base pressure.Set the argon flow to four standard cubic centimeters per minute and allow it to stabilize. Maintain substrate rotation at 10 RPM. Confirm the matching network settings for both guns and enable auto-matching on the controller.Initiate the bismuth telluride gun at 70 watts for easier plasma ignition. Increase the power by five watts every 10 seconds until reaching 100 watts. Start the deposition timer only after the bismuth telluride power readback remains at 100 watts for approximately 30 seconds and plasma stability is confirmed.Deposit the films for 30 minutes while maintaining stable plasma conditions during the deposition process. Using the same parameters, repeat the deposition steps for manganese at radiofrequency powers of 10 watts and 15 watts using fresh substrates. Initiate shutdown through the system controller by switching off the radiofrequency output first.Reduce the argon flow to 10 to 11 standard cubic centimeters per minute while keeping the cooling system active until the chamber is vented and the sputter guns return to near ambient temperature. Confirm that the turbomolecular pump has stopped completely and the speed reading is zero before venting the chamber. Vent the chamber slowly using dry nitrogen through the vent valve to allow gradual pressure, equalization, and minimize particle disturbance.Open the chamber only after the pressure returns to approximately atmospheric pressure at approximately 760 torr and the chamber door can be released without resistance. Wear a mask and gloves during sample removal to reduce contamination and exposure to fine particles. Remove the deposited samples from the chamber.Transfer the samples into a clean Petri dish. Store the samples in a vacuum storage container and perform characterization within 24 to 72 hours after deposition. After sample removal, rough pump the chamber for 10 to 15 minutes to reach the required pre-TMP pressure, minimizing exposure to ambient air and moisture.X-ray diffraction patterns confirm that all samples retain the rhombohedral bismuth telluride phase across the manganese power series. The dominant diffraction peak shifted toward higher two theta values with increasing manganese input. The crystallite size generally decreased from 14.23 nanometers at zero watts to 8.35 nanometers at 15 watts, consistent with reduced coherent domain size and increased microstrain at higher manganese power.Surface field emission scanning electron microscopy images demonstrated clear changes in film microstructure with increasing manganese input. The zero watt control film showed larger polygonal grains with distinct grain boundaries, while the five watt manganese-doped film exhibited a more compact surface with finer grains. Films deposited at 10 watt and 15 watt manganese power appeared denser with fewer intergranular gaps than the zero watt and five watt samples.Elemental composition analysis confirmed that manganese incorporation increased with increasing manganese target power. All films exhibited a negative Seebeck coefficient, confirming n-type conduction behavior, and the magnitude of the Seebeck coefficient generally increased with temperature for all samples. The highest Seebeck coefficient magnitude was observed for the 15 watt film, reaching minus 162.08 microvolts per Kelvin at 523 Kelvins.All films exhibited semi-conducting transport behavior where resistivity decreased with increasing temperature. The maximum power factor was achieved for the five watt film, reaching approximately 529.33 microwatts per meter per Kelvin squared at 523 Kelvins. Although the 15 watt film exhibited the highest Seebeck coefficient magnitude, the increased resistivity reduced the power factor to 300.59 microwatts per meter per Kelvin squared.This protocol allowed the researcher to co-sputter the manganese-doped on the bismuth telluride film, and evaluate how the doping input level change the thermoelectric performance. The key challenge of this protocol is to maintain the stable plasma and also the sputtering condition to incorporate mechanisms reliably and consistently. For the future study can be built by optimizing thermoelectric properties, post-synthesis, and bifurcating a thin film thermoelectric generator for the device level testing.

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Research

JoVE Journal

Engineering

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