Abstract
The properties and applications of molybdenum disulfide (MoS2) are significantly dependent on its purity. Physical purification is proposed for separating impurities from MoS2. Meanwhile, the feasibility of separation of impurities was analyzed by thermodynamic calculations. The effects of the temperature and heating duration on the volatilization of impurities were studied experimentally. The purity of MoS2 was notably improved by vacuum distillation at optimized processing conditions. The phase of the volatiles and the microstructural change of the residues were investigated and characterized by X-ray diffraction analysis, scanning electron microscopy, electron probe microanalysis, Raman spectroscopy, and atomic force microscopy.
Graphical Abstract
-
1.
Vacuum distillation is a scalable one-step approach to separate impurities from molybdenum disulfide.
-
2.
The purity of the residual MoS2 significantly depends on the distillation temperature and duration.
-
3.
Tiny amounts of impurities were collected and analyzed by phase determination.
-
4.
The transformation to multilayer stacks is attributed to the high temperature used during vacuum distillation.
Similar content being viewed by others
References
Chhowalla M, Shin HS, Eda G, Li L-J, Loh KP, Zhang H (2013) The chemistry of two-dimensional layered transition metal dichalcogenide nanosheets. Nat Chem 5:263–275
Miremadi BK, Singh RC, Morrison SR, Colbow K (1996) A highly sensitive and selective hydrogen gas sensor from thick oriented films of MoS2. Appl Phys A Mater Sci Process 63:271–275
Li T, Galli G (2007) Electronic properties of MoS2 nanoparticles. J Phys Chem C 111:16192–16196
Krishnan U, Kaur M, Singh K, Kumar M, Kumar A (2019) A synoptic review of MoS2: synthesis to applications. Superlattices Microstruct 128:274–297
Kibsgaard J, Lauritsen J, Clausen BS, Topsøe H, Besenbacher F (2006) Cluster–support interactions and morphology of MoS2 nanoclusters in a graphite-supported hydrotreating model catalyst. J Am Chem Soc 128:13950–13958
Hinnemann B, Moses PG, Bonde J, Joergensen KP, Nielsen JH, Horch S, Chorkendorff I, Noerskov JK (2005) Biomimetic hydrogen evolution: MoS2 nanoparticles as catalyst for hydrogen evolution. J Am Chem Soc 127:5308
Li D, Cheng R, Zhou H, Wang C, Yin A, Chen Y, Weiss NO, Huang Y, Duan X (2015) Electric-field-induced strong enhancement of electroluminescence in multilayer molybdenum disulfide. Nat Commun 6:7509
Ha HD, Dong JH, Choi JS, Park M, Seo TS (2014) Dual role of blue luminescent MoS2 quantum dots in fluorescence resonance energy transfer phenomenon. Small 10:3814–3814
Radisavljevic B, Radenovic A, Brivio J, Giacometti V, Kis A (2011) Single-layer MoS2 transistors. Nat Nanotechnol 6:147–150
Li H, Yin Z, He Q, Li H, Huang X, Lu G, Fam DWH, Tok AIY, Zhang Q, Zhang H (2012) Fabrication of single- and multilayer MoS2 film-based field-effect transistors for sensing NO at room temperature. Small 8:63–67
Li Y, Li Y-L, Araujo CM, Luo W, Ahuja R (2013) Single-layer MoS2 as an efficient photocatalyst. Catal Sci Technol 3:2214–2220
Guo D, Fu L, Wang S, Zhang L, Peng J (2018) Application of Taguchi method for optimization of process parameters in preparation of high-purity molybdenum disulfide. Chem Pap 72:2997–3003
Feng M, Hao Y, Cheng W, Wang Z, Wang Y, Gao Q, Huo E (2018) Research progress in preparation method and application of high-purity molybdenum disulfide. Henan Chem Ind 35:3–8 (In Chinese)
Wei Z, Wang Q-Q, Guo Y-T, Li J-W, Shi D-X, Zhang G-Y (2018) Research progress of high-quality monolayer MoS2 films. Acta Phys Sin 67:263–295 (In Chinese)
Guo PM, Pang JM, Zhao P (2012) Preparation of ultra pure MoS2 powder. Nonferr Met (Extr Metall) 7:50–52 (In Chinese)
Zhang L, Li H, Zhang H, Liang J (2019) Progress on preparation process of molybdenum disulphide. Hydrometall China 38:7–11 (In Chinese)
Yang J (2000) Preparation of high purity molybdenum disulfide. Nonferr Met 19–23:28 (In Chinese)
Wang H (2019) Development and application of nonferrous metal vacuum metallurgy technology. World Nonferr Met. https://doi.org/10.3969/j.issn.1002-5065.2019.05.002(In Chinese)
Dai Y, Yang B, Ma W, Chen W (2004) Advances in vacuum metallurgy of nonferrous metals. Vacuum 41:5–8 (In Chinese)
Wang L, Guo PM, Pang J, Zhao P (2015) Thermodynamic analysis of vacuum decomposition process of molybdenum concentrate. Chin J Nonferr Met 25:190–196 (In Chinese)
Medvedev AS, Aleksandrov PV (2009) Investigations on processing low-grade molybdenum concentrate by the nitric-acid method. Russ J Non-Ferr Met 50:353–356
Liang Y, Che Y (1993) Manual of thermodynamic data of inorganic materials. Northeastern University, Shenyang
Zhou Y, Lu Y, Liu D, Chen X, Li W, Li Z (2015) Thermodynamic analysis and experimental rules of vacuum decomposition of molybdenite concentrate. Vacuum 121:166–172
Xu S, Li D, Wu P (2015) One-Pot, facile, and versatile synthesis of monolayer MoS2/WS2 quantum dots as bioimaging probes and efficient electrocatalysts for hydrogen evolution reaction. Adv Funct Mater 25:1127–1136
Qiao W, Yan S, Song X, Zhang X, He X, Zhong W, Du Y (2015) Luminescent monolayer MoS2 quantum dots produced by multi-exfoliation based on lithium intercalation. Appl Surf Sci 359:130–136
Kim MS, Nam G, Park S, Kim H, Han GH, Lee J, Dhakal KP, Leem J-Y, Lee YH, Kim J (2015) Photoluminescence wavelength variation of monolayer MoS2 by oxygen plasma treatment. Thin Solid Films 590:318–323
Acknowledgements
This research work is financially supported by Yunnan Provincial Scientists’ Workshop, special funds for guiding local scientific and technological development by the central government and National Natural Science Foundation of China (no. 51964033). We also greatly appreciate Professor Li Kongzhai who offered detection of Raman spectra.
Author information
Authors and Affiliations
Corresponding authors
Ethics declarations
Conflict of interest
The authors declared that they have no conflicts of interest to this work.
Additional information
The contributing editor for this article was Yongxiang Yang.
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Rights and permissions
About this article
Cite this article
Li, Y., Wang, F., Yang, B. et al. Experimental Investigation of Molybdenum Disulfide Purification Through Vacuum Distillation. J. Sustain. Metall. 6, 419–427 (2020). https://doi.org/10.1007/s40831-020-00284-5
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s40831-020-00284-5