Skip to main content
Log in

Experimental Investigation of Molybdenum Disulfide Purification Through Vacuum Distillation

  • Research Article
  • Published:
Journal of Sustainable Metallurgy Aims and scope Submit manuscript

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. 1.

    Vacuum distillation is a scalable one-step approach to separate impurities from molybdenum disulfide.

  2. 2.

    The purity of the residual MoS2 significantly depends on the distillation temperature and duration.

  3. 3.

    Tiny amounts of impurities were collected and analyzed by phase determination.

  4. 4.

    The transformation to multilayer stacks is attributed to the high temperature used during vacuum distillation.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9
Fig. 10

Similar content being viewed by others

References

  1. 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

    Article  Google Scholar 

  2. 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

    Google Scholar 

  3. Li T, Galli G (2007) Electronic properties of MoS2 nanoparticles. J Phys Chem C 111:16192–16196

    Article  CAS  Google Scholar 

  4. Krishnan U, Kaur M, Singh K, Kumar M, Kumar A (2019) A synoptic review of MoS2: synthesis to applications. Superlattices Microstruct 128:274–297

    Article  CAS  Google Scholar 

  5. 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

    Article  CAS  Google Scholar 

  6. 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

    Article  CAS  Google Scholar 

  7. 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

    Article  Google Scholar 

  8. 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

    Article  CAS  Google Scholar 

  9. Radisavljevic B, Radenovic A, Brivio J, Giacometti V, Kis A (2011) Single-layer MoS2 transistors. Nat Nanotechnol 6:147–150

    Article  CAS  Google Scholar 

  10. 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

    Article  CAS  Google Scholar 

  11. 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

    Article  CAS  Google Scholar 

  12. 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

    Article  CAS  Google Scholar 

  13. 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)

    Google Scholar 

  14. 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)

    Google Scholar 

  15. Guo PM, Pang JM, Zhao P (2012) Preparation of ultra pure MoS2 powder. Nonferr Met (Extr Metall) 7:50–52 (In Chinese)

    CAS  Google Scholar 

  16. Zhang L, Li H, Zhang H, Liang J (2019) Progress on preparation process of molybdenum disulphide. Hydrometall China 38:7–11 (In Chinese)

    Google Scholar 

  17. Yang J (2000) Preparation of high purity molybdenum disulfide. Nonferr Met 19–23:28 (In Chinese)

    Google Scholar 

  18. 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)

    Article  Google Scholar 

  19. Dai Y, Yang B, Ma W, Chen W (2004) Advances in vacuum metallurgy of nonferrous metals. Vacuum 41:5–8 (In Chinese)

    CAS  Google Scholar 

  20. 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)

    CAS  Google Scholar 

  21. 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

    Article  Google Scholar 

  22. Liang Y, Che Y (1993) Manual of thermodynamic data of inorganic materials. Northeastern University, Shenyang

    Google Scholar 

  23. 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

    Article  CAS  Google Scholar 

  24. 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

    Article  CAS  Google Scholar 

  25. 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

    Article  CAS  Google Scholar 

  26. 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

    Article  CAS  Google Scholar 

Download references

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

Authors

Corresponding authors

Correspondence to Fei Wang or Bin Yang.

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

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

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

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s40831-020-00284-5

Keywords

Navigation