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International Journal of Education & Applied Sciences Research

HYDROTHERMAL SYNTHESIS AND CHARACTERIZATION OF MOLYBDENUM DISULFIDE NANOSHEETS

Adarsh Kumar Pandey, Sajal Rai, Ashish Borah, Ahsan Ali, Amit Kumar Patel, Vikram Singh, Anchal Srivastava

Adarsh Kumar Pandey1,#, Sajal Rai2,#, Ashish Borah2,#, Ahsan Ali2,#, Amit Kumar Patel2,#,

Vikram Singh1,*, Anchal Srivastava2

1Department of Physics, Nehru Gram Bharti (Deemed to be University), Prayagraj-221505

2Department of Physics, Banaras Hindu University, Varanasi-221005

DOI : https://doi.org/10.5281/zenodo.15009755 Page No : 01-08

Published Online : 2025-03-10

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This paper reports the hydrothermal synthesis of molybdenum disulfide (MoS₂) nanosheets. The few-layered nanosheets have a potential due to their two-dimensional structure and electronic properties, making them good candidates for various applications, including nanofiltration membranes, energy storage, and sensing. A simple hydrothermal synthesis method has been used to prepare these nanosheets, involving the reaction of molybdenum and sulfur sources at higher temperatures. To know the synthesized nanosheets, we have used powder X-ray diffraction (XRD), Raman spectroscopy, Fourier-transform infrared (FT-IR) spectroscopy and transmission electron microscopy (TEM) material characterization techniques to confirm the successful synthesis of MoS₂ nanosheets.

Keywords: MoS₂, Nanosheets, Hydrothermal Synthesis, XRD, FT-IR, TEM

REFERENCES

Chhowalla, M., Shin, H. S., Eda, G., Li, L. J., Loh, K. P., & Zhang, H. (2013). The chemistry of two-dimensional layered transition metal dichalcogenide nanosheets. Nature Chemistry, 5(4), 263-275.
Wang, Q. H., Kalantar-Zadeh, K., Kis, A., Coleman, J. N., & Strano, M. S. (2012). Electronics and optoelectronics of two-dimensional transition metal dichalcogenides. Nature Nanotechnology, 7(11), 699-712.
Voiry, D., Mohite, A., &Chhowalla, M. (2015). Phase engineering of transition metal dichalcogenides. Chemical Society Reviews, 44(9), 2702-2712.
Zhang, Y., Nayak, T. R., Hong, H., & Cai, W. (2013). Graphene, graphene oxide, and their biofunctionalized derivatives: A comparative study of graphene-based nanomaterials in nanomedicine. Chemical Reviews, 113(5), 3766-3798.
Wang, S., Wang, X., & He, T. (2015). Hydrothermal synthesis of MoS₂ with controllable morphologies for energy storage applications. Materials Chemistry and Physics, 162, 577-584.
Zeng, Z., Yin, Z., Huang, X., Li, H., He, Q., Lu, G., Boey, F., & Zhang, H. (2011). Single-layer semiconducting nanosheets: High-yield preparation and device fabrication. Angewandte Chemie International Edition, 50(47), 11093-11097.
Yu, Y., Nam, G. H., He, Q., Wu, X. J., Zhang, K., Yang, Z., Chen, J., Ma, Q., Zhao, M., Liu, Z., Ran, F. R., Wang, X., & Huang, W. (2018). Morphological evolution of MoS₂ nanosheets under hydrothermal synthesis conditions. Advanced Materials, 30(14), 1705560.
Xu, X., Zhao, S., & Wang, X. (2016). Hydrothermal growth of MoS₂ nanostructures: Mechanism and morphology control. ACS Nano, 10(12), 10212-10220.
Late, D. J., Liu, B., Matte, H. S. S. R., Dravid, V. P., & Rao, C. N. R. (2012). Hysteresis in single-layer MoS₂ field effect transistors. ACS Nano, 6(6), 5635-5641.
Li, H., Wu, J., Huang, X., Lu, G., Yang, J., Lu, X., Xiong, Q., & Zhang, H. (2013). Rapid synthesis of high-quality MoS₂ nanosheets via a hydrothermal route. Journal of the American Chemical Society, 135(13), 5308-5311.
Eda, G., Fujita, T., Yamaguchi, H., Voiry, D., Chen, M., &Chhowalla, M. (2012). Coherent atomic and electronic heterostructures of single-layer MoS₂. ACS Nano, 6(8), 7311-7317.
Su, T., Shao, Q., Qin, Z., Guo, Z., & Wu, Z. S. (2020). Morphology-controlled MoS₂ nanosheets for energy storage applications. Journal of Materials Chemistry A, 8(3), 1174-1183.
Yang, S., Brüller, S., Wu, Z. S., Liu, Z., Parvez, K., Dong, R., Richard, F., Samorì, P., &Müllen, K. (2015). Organic radical-assisted electrochemical exfoliation for the scalable production of high-quality MoS₂ nanosheets. Angewandte Chemie International Edition, 54(8), 2397-2401.
Zhang, X., Lai, Z., Ma, Q., & Zhang, H. (2018). Novel structured transition metal dichalcogenide nanosheets for catalysis and energy storage. Advanced Materials, 30(10), 1706310.
Choi, W., Choudhary, N., Han, G. H., Park, J., Akinwande, D., & Lee, Y. H. (2017). Recent development of two-dimensional transition metal dichalcogenides and their applications. Materials Today, 20(3), 116-130.
Tan, C., & Zhang, H. (2015). Two-dimensional transition metal dichalcogenide nanosheet-based composites. Chemical Society Reviews, 44(9), 2713-2731.
Z. Q. Liang, Y. C. Guo, Y. J. Xue, H. Z. Cui, and J. Tian, "1T-phase MoS₂ quantum dots as a superior co-catalyst to Pt decorated on carbon nitride nanorods for photocatalytic hydrogen evolution from water," Mater. Chem. Front., vol. 3, pp. 2032–2040, 2019.
J.A. Wilson, A.D. Yoffe, “The transition metal dichalcogenides discussion and interpretation of the observed optical, electrical and structural properties,” Advances in Physics, vol. 18, no. 73, pp. 193-335, 1969.
K.F. Mak, C. Lee, J. Hone, J. Shan, T.F. Heinz, “Atomically thin MoS₂: A new direct-gap semiconductor,” Physical Review Letters, vol. 105, no. 13, p. 136805, 2010.
R. Ganatra, Q. Zhang, “Few-layer MoS₂: A promising layered semiconductor,” ACS Nano, vol. 8, no. 5, pp. 4074-4099, 2014.
S. Najmaei, Z. Liu, W. Zhou, X. Zou, G. Shi, S. Lei, B.I. Yakobson, J.C. Idrobo, P.M. Ajayan, J. Lou, “Vapour phase growth and grain boundary structure of molybdenum disulphide atomic layers,” Nature Materials, vol. 12, no. 8, pp. 754-759, 2013.
C. Lee, H. Yan, L.E. Brus, T.F. Heinz, J. Hone, S. Ryu, “Anomalous Lattice Vibrations of Single- and Few-Layer MoS₂,” ACS Nano, vol. 4, no. 5, pp. 2695-2700, 2010.
H. Li, Q. Zhang, C.C.R. Yap, B.K. Tay, T.H.T. Edwin, A. Olivier, D. Baillargeat, “From bulk to monolayer MoS₂: Evolution of Raman scattering,” Advanced Functional Materials, vol. 22, no. 7, pp. 1385-1390, 2012.
M. Mahjouri-Samani, M. Tian, K. Wang, A. Boulesbaa, A.A. Puretzky, C.M. Rouleau, G. Eres, A. Ivanov, P.D. Rack, K. Xiao, “Tailoring vacancies far beyond intrinsic levels: A new pathway to compensate n-type MoS₂,” Nano Letters, vol. 14, no. 10, pp. 5523-5527, 2014.
M. Chhowalla, H.S. Shin, G.E. Eda, L.J. Li, K.P. Loh, H. Zhang, “The chemistry of two-dimensional layered transition metal dichalcogenide nanosheets,” Nature Chemistry, vol. 5, no. 4, pp. 263-275, 2013.
S. Bertolazzi, J. Brivio, A. Kis, “Stretching and breaking of ultrathin MoS₂,” ACS Nano, vol. 5, no. 12, pp. 9703-9709, 2011.
Z. Yin, H. Li, H. Li, L. Jiang, Y. Shi, Y. Sun, G. Lu, Q. Zhang, X. Chen, H. Zhang, “Single-layer MoS₂ phototransistors,” ACS Nano, vol. 6, no. 1, pp. 74-80, 2012.
J. Kang, S. Tongay, J. Zhou, J. Li, J. Wu, “Band offsets and heterostructures of two-dimensional semiconductors,” Applied Physics Letters, vol. 102, no. 1, p. 012111, 2013.
B. Radisavljevic, A. Radenovic, J. Brivio, V. Giacometti, A. Kis, “Single-layer MoS₂ transistors,” Nature Nanotechnology, vol. 6, no. 3, pp. 147-150, 2011.
Y. Yu, G. Li, Y. Huang, J. Wang, Z. Li, Y. Liu, X. Duan, “Controlled scalable synthesis of uniform, high-quality monolayer and few-layer MoS₂ films,” Scientific Reports, vol. 3, p. 1866, 2013.
A. Gupta, T. Sakthivel, S. Seal, “Recent developments in 2D materials beyond graphene,” Progress in Materials Science, vol. 73, pp. 44-126, 2015.
K. Dolui, I. Rungger, C. Das Pemmaraju, S. Sanvito, “Possible doping strategies for MoS₂ monolayers: An ab initio study,” Physical Review B, vol. 88, no. 7, p. 075420, 2013.
O. Lopez-Sanchez, D. Lembke, M. Kayci, A. Radenovic, A. Kis, “Ultrasensitive photodetectors based on monolayer MoS₂,” Nature Nanotechnology, vol. 8, no. 7, pp. 497-501, 2013.
M. Ghorbani-Asl, A.N. Enyashin, A. Kuc, T. Heine, “Defect-induced conductivity anisotropy in MoS₂ monolayers,” Physical Review B, vol. 88, no. 24, p. 245440, 2013.
R. Lv, J. A. Robinson, R.E. Schaak, D. Sun, Y. Sun, T.E. Mallouk, M. Terrones, “Transition metal dichalcogenides and beyond: Synthesis, properties, and applications of single- and few-layer nanosheets,” Accounts of Chemical Research, vol. 48, no. 1, pp. 56-64, 2015.
H. Li, X. Wu, Z. Huang, C. Yang, X. Lu, J. Xie, Y. Jiang, “Direct growth of MoS₂ nanosheets on silicon as efficient photocathodes for hydrogen evolution,” Energy & Environmental Science, vol. 10, no. 2, pp. 467-473, 2017.
J. Pu, Y. Yomogida, K. Liu, L.J. Li, Y. Iwasa, T. Takenobu, “Highly flexible MoS₂ thin-film transistors with ion gel dielectrics,” Nano Letters, vol. 12, no. 8, pp. 4013-4017, 2012.
X. Huang, Z. Zeng, H. Zhang, “Metal dichalcogenide nanosheets: Preparation, properties, and applications,” Chemical Society Reviews, vol. 42, no. 5, pp. 1934-1946, 2013.
D. Voiry, H.S. Shin, K.P. Loh, M. Chhowalla, “Low-dimensional catalysts for hydrogen evolution and CO₂ reduction,” Nature Reviews Chemistry, vol. 2, no. 1, p. 0105, 2018.

Cite this Article as: Pandey A.K, Rai S, Borah A, Ali A, Patel A.K, Singh V, Srivastava A (2025), “Hydrothermal Synthesis and Characterization of Molybdenum Disulfide Nanosheets”, International Journal of Education & Applied Sciences Research, Volume 12, Issue 1, 2025, pp 01-08 DOI : https://doi.org/10.5281/zenodo.15009755

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REFERENCES

Chhowalla, M., Shin, H. S., Eda, G., Li, L. J., Loh, K. P., & Zhang, H. (2013). The chemistry of two-dimensional layered transition metal dichalcogenide nanosheets. Nature Chemistry, 5(4), 263-275.
Wang, Q. H., Kalantar-Zadeh, K., Kis, A., Coleman, J. N., & Strano, M. S. (2012). Electronics and optoelectronics of two-dimensional transition metal dichalcogenides. Nature Nanotechnology, 7(11), 699-712.
Voiry, D., Mohite, A., &Chhowalla, M. (2015). Phase engineering of transition metal dichalcogenides. Chemical Society Reviews, 44(9), 2702-2712.
Zhang, Y., Nayak, T. R., Hong, H., & Cai, W. (2013). Graphene, graphene oxide, and their biofunctionalized derivatives: A comparative study of graphene-based nanomaterials in nanomedicine. Chemical Reviews, 113(5), 3766-3798.
Wang, S., Wang, X., & He, T. (2015). Hydrothermal synthesis of MoS₂ with controllable morphologies for energy storage applications. Materials Chemistry and Physics, 162, 577-584.
Zeng, Z., Yin, Z., Huang, X., Li, H., He, Q., Lu, G., Boey, F., & Zhang, H. (2011). Single-layer semiconducting nanosheets: High-yield preparation and device fabrication. Angewandte Chemie International Edition, 50(47), 11093-11097.
Yu, Y., Nam, G. H., He, Q., Wu, X. J., Zhang, K., Yang, Z., Chen, J., Ma, Q., Zhao, M., Liu, Z., Ran, F. R., Wang, X., & Huang, W. (2018). Morphological evolution of MoS₂ nanosheets under hydrothermal synthesis conditions. Advanced Materials, 30(14), 1705560.
Xu, X., Zhao, S., & Wang, X. (2016). Hydrothermal growth of MoS₂ nanostructures: Mechanism and morphology control. ACS Nano, 10(12), 10212-10220.
Late, D. J., Liu, B., Matte, H. S. S. R., Dravid, V. P., & Rao, C. N. R. (2012). Hysteresis in single-layer MoS₂ field effect transistors. ACS Nano, 6(6), 5635-5641.
Li, H., Wu, J., Huang, X., Lu, G., Yang, J., Lu, X., Xiong, Q., & Zhang, H. (2013). Rapid synthesis of high-quality MoS₂ nanosheets via a hydrothermal route. Journal of the American Chemical Society, 135(13), 5308-5311.
Eda, G., Fujita, T., Yamaguchi, H., Voiry, D., Chen, M., &Chhowalla, M. (2012). Coherent atomic and electronic heterostructures of single-layer MoS₂. ACS Nano, 6(8), 7311-7317.
Su, T., Shao, Q., Qin, Z., Guo, Z., & Wu, Z. S. (2020). Morphology-controlled MoS₂ nanosheets for energy storage applications. Journal of Materials Chemistry A, 8(3), 1174-1183.
Yang, S., Brüller, S., Wu, Z. S., Liu, Z., Parvez, K., Dong, R., Richard, F., Samorì, P., &Müllen, K. (2015). Organic radical-assisted electrochemical exfoliation for the scalable production of high-quality MoS₂ nanosheets. Angewandte Chemie International Edition, 54(8), 2397-2401.
Zhang, X., Lai, Z., Ma, Q., & Zhang, H. (2018). Novel structured transition metal dichalcogenide nanosheets for catalysis and energy storage. Advanced Materials, 30(10), 1706310.
Choi, W., Choudhary, N., Han, G. H., Park, J., Akinwande, D., & Lee, Y. H. (2017). Recent development of two-dimensional transition metal dichalcogenides and their applications. Materials Today, 20(3), 116-130.
Tan, C., & Zhang, H. (2015). Two-dimensional transition metal dichalcogenide nanosheet-based composites. Chemical Society Reviews, 44(9), 2713-2731.
Z. Q. Liang, Y. C. Guo, Y. J. Xue, H. Z. Cui, and J. Tian, "1T-phase MoS₂ quantum dots as a superior co-catalyst to Pt decorated on carbon nitride nanorods for photocatalytic hydrogen evolution from water," Mater. Chem. Front., vol. 3, pp. 2032–2040, 2019.
J.A. Wilson, A.D. Yoffe, “The transition metal dichalcogenides discussion and interpretation of the observed optical, electrical and structural properties,” Advances in Physics, vol. 18, no. 73, pp. 193-335, 1969.
K.F. Mak, C. Lee, J. Hone, J. Shan, T.F. Heinz, “Atomically thin MoS₂: A new direct-gap semiconductor,” Physical Review Letters, vol. 105, no. 13, p. 136805, 2010.
R. Ganatra, Q. Zhang, “Few-layer MoS₂: A promising layered semiconductor,” ACS Nano, vol. 8, no. 5, pp. 4074-4099, 2014.
S. Najmaei, Z. Liu, W. Zhou, X. Zou, G. Shi, S. Lei, B.I. Yakobson, J.C. Idrobo, P.M. Ajayan, J. Lou, “Vapour phase growth and grain boundary structure of molybdenum disulphide atomic layers,” Nature Materials, vol. 12, no. 8, pp. 754-759, 2013.
C. Lee, H. Yan, L.E. Brus, T.F. Heinz, J. Hone, S. Ryu, “Anomalous Lattice Vibrations of Single- and Few-Layer MoS₂,” ACS Nano, vol. 4, no. 5, pp. 2695-2700, 2010.
H. Li, Q. Zhang, C.C.R. Yap, B.K. Tay, T.H.T. Edwin, A. Olivier, D. Baillargeat, “From bulk to monolayer MoS₂: Evolution of Raman scattering,” Advanced Functional Materials, vol. 22, no. 7, pp. 1385-1390, 2012.
M. Mahjouri-Samani, M. Tian, K. Wang, A. Boulesbaa, A.A. Puretzky, C.M. Rouleau, G. Eres, A. Ivanov, P.D. Rack, K. Xiao, “Tailoring vacancies far beyond intrinsic levels: A new pathway to compensate n-type MoS₂,” Nano Letters, vol. 14, no. 10, pp. 5523-5527, 2014.
M. Chhowalla, H.S. Shin, G.E. Eda, L.J. Li, K.P. Loh, H. Zhang, “The chemistry of two-dimensional layered transition metal dichalcogenide nanosheets,” Nature Chemistry, vol. 5, no. 4, pp. 263-275, 2013.
S. Bertolazzi, J. Brivio, A. Kis, “Stretching and breaking of ultrathin MoS₂,” ACS Nano, vol. 5, no. 12, pp. 9703-9709, 2011.
Z. Yin, H. Li, H. Li, L. Jiang, Y. Shi, Y. Sun, G. Lu, Q. Zhang, X. Chen, H. Zhang, “Single-layer MoS₂ phototransistors,” ACS Nano, vol. 6, no. 1, pp. 74-80, 2012.
J. Kang, S. Tongay, J. Zhou, J. Li, J. Wu, “Band offsets and heterostructures of two-dimensional semiconductors,” Applied Physics Letters, vol. 102, no. 1, p. 012111, 2013.
B. Radisavljevic, A. Radenovic, J. Brivio, V. Giacometti, A. Kis, “Single-layer MoS₂ transistors,” Nature Nanotechnology, vol. 6, no. 3, pp. 147-150, 2011.
Y. Yu, G. Li, Y. Huang, J. Wang, Z. Li, Y. Liu, X. Duan, “Controlled scalable synthesis of uniform, high-quality monolayer and few-layer MoS₂ films,” Scientific Reports, vol. 3, p. 1866, 2013.
A. Gupta, T. Sakthivel, S. Seal, “Recent developments in 2D materials beyond graphene,” Progress in Materials Science, vol. 73, pp. 44-126, 2015.
K. Dolui, I. Rungger, C. Das Pemmaraju, S. Sanvito, “Possible doping strategies for MoS₂ monolayers: An ab initio study,” Physical Review B, vol. 88, no. 7, p. 075420, 2013.
O. Lopez-Sanchez, D. Lembke, M. Kayci, A. Radenovic, A. Kis, “Ultrasensitive photodetectors based on monolayer MoS₂,” Nature Nanotechnology, vol. 8, no. 7, pp. 497-501, 2013.
M. Ghorbani-Asl, A.N. Enyashin, A. Kuc, T. Heine, “Defect-induced conductivity anisotropy in MoS₂ monolayers,” Physical Review B, vol. 88, no. 24, p. 245440, 2013.
R. Lv, J. A. Robinson, R.E. Schaak, D. Sun, Y. Sun, T.E. Mallouk, M. Terrones, “Transition metal dichalcogenides and beyond: Synthesis, properties, and applications of single- and few-layer nanosheets,” Accounts of Chemical Research, vol. 48, no. 1, pp. 56-64, 2015.
H. Li, X. Wu, Z. Huang, C. Yang, X. Lu, J. Xie, Y. Jiang, “Direct growth of MoS₂ nanosheets on silicon as efficient photocathodes for hydrogen evolution,” Energy & Environmental Science, vol. 10, no. 2, pp. 467-473, 2017.
J. Pu, Y. Yomogida, K. Liu, L.J. Li, Y. Iwasa, T. Takenobu, “Highly flexible MoS₂ thin-film transistors with ion gel dielectrics,” Nano Letters, vol. 12, no. 8, pp. 4013-4017, 2012.
X. Huang, Z. Zeng, H. Zhang, “Metal dichalcogenide nanosheets: Preparation, properties, and applications,” Chemical Society Reviews, vol. 42, no. 5, pp. 1934-1946, 2013.
D. Voiry, H.S. Shin, K.P. Loh, M. Chhowalla, “Low-dimensional catalysts for hydrogen evolution and CO₂ reduction,” Nature Reviews Chemistry, vol. 2, no. 1, p. 0105, 2018.

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