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Journals / Journal of the Turkish Chemical Society Section A: Chemistry / 2026 / Volume: 2026 Issue: 2

Synthesis and Characterization of ZnSb₂S₄ in an Aqueous Sb₂S₃–ZnSO₄ System: Thermogravimetric, X-Ray Diffraction, and Electron Microscopy Analyses

Sevda Aliyeva(NAHCİVAN DEVLET ÜNİVERSİTESİ)0009-0007-7737-0578
Gunel Mammadova(NAHCİVAN DEVLET ÜNİVERSİTESİ)0000-0002-5203-0063
Gulyayra Kholikova(Buhara Devlet Üniversitesi Kimya ve Petrol-Gaz Teknolojisi Bölümü)0000-0001-5625-3347
Uktam Mardonovich Mardonov(Buhara Devlet Üniversitesi Kimya ve Petrol-Gaz Teknolojisi Bölümü)0000-0001-6344-6833
İmir Aliev(Azerbaycan Cumhuriyeti, Bilim ve Eğitim Bakanlığı, Kataliz ve İnorganik Kimya Enstitüsü)0009-0005-0548-2621
Bakhtiyor Ganiev(Buhara Devlet Üniversitesi. Kimya ve Petrol Gazı Teknolojileri Bölümü.)0000-0001-8151-1088
Sharipov Muzafar Samandarovich(Buhara Devlet Üniversitesi Kimya ve Petrol-Gaz Teknolojisi Bölümü)0000-0002-4828-3818
Sharafat Mammadov(Kataliz ve İnorganik Kimya Enstitüsü.)0000-0002-1624-7345
Pages
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Publication Date
2026-10-27
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AI Summary & Key Takeaways

AI Insight
⚡ TL;DR(Too Long; Didn't Read)

TGA results indicated that the material remained relatively stable up to approximately 300 °C, followed by a substantial mass loss at higher temperatures.

📌 3 Key Takeaways

🎯
Objective & Hypothesis:Zinc antimony sulfide (ZnSb₂S₄) is an antimony-based chalcogenide of interest because of its potential functional applications.
📊
Key Findings & Data:The quantitative assessment suggested that approximately 75% of the antimony was retained in the solid phase, whereas the remaining 25% was present in the solution.
💡
Conclusion & Impact:TGA results indicated that the material remained relatively stable up to approximately 300 °C, followed by a substantial mass loss at higher temperatures.
🔬Design:Research Article
📍Scope:Comprehensive Sample
⚙️Variables:ZnSb2S4 · antimony (III) sulfide · aqueous synthesis

Abstract

Zinc antimony sulfide (ZnSb₂S₄) is an antimony-based chalcogenide of interest because of its potential functional applications. In this study, a low-temperature aqueous route was investigated for the synthesis of ZnSb₂S₄ through the reaction of antimony(III) sulfide (Sb₂S₃) with zinc sulfate (ZnSO₄), using Sb₂S₃ derived from Daridagh antimony ore as the starting material. The effects of the reactant ratio, solution pH, and reaction conditions on product formation were examined. Chemical analysis indicated that the elemental composition of the synthesized product was consistent with the proposed ZnSb₂S₄ formula. The quantitative assessment suggested that approximately 75% of the antimony was retained in the solid phase, whereas the remaining 25% was present in the solution. Product formation was strongly influenced by solution pH, with more favorable results obtained under mildly acidic to near-neutral conditions. Strongly acidic conditions inhibited the formation of the target product. The obtained product was characterized using thermogravimetric analysis (TGA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). TGA results indicated that the material remained relatively stable up to approximately 300 °C, followed by a substantial mass loss at higher temperatures. XRD measurements provided information on the structural characteristics of the synthesized product, while SEM observations revealed its morphology and microstructure. Overall, the results suggest that the aqueous Sb₂S₃–ZnSO₄ system provides a relatively simple, low-temperature route for preparing zinc–antimony sulfide materials from ore-derived precursors.

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Cite This Article

Aliyeva, S., Mammadova, G., Kholikova, G., Mardonov, U. M., Aliev, İ., Ganiev, B., Samandarovich, S. M., Mammadov, S. (2026). Synthesis and Characterization of ZnSb₂S₄ in an Aqueous Sb₂S₃–ZnSO₄ System: Thermogravimetric, X-Ray Diffraction, and Electron Microscopy Analyses. Journal of the Turkish Chemical Society Section A: Chemistry, Volume: 2026 Issue: 2. https://doi.org/10.18596/jotcsa.1943616

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  48. Göktaş A, Mutlu İH. Room temperature ferromagnetism in Mn-doped ZnS nanocrystalline thin films grown by sol–gel dip coating process. J Sol-Gel Sci Technol. 2014 Jan 9;69(1):120–9. Available from:.
  49. Göktaş S. Al-mediated doping boosts photocatalysis and room-temperature ferromagnetism in Sol-Gel ZnS thin films. J Sol-Gel Sci Technol. 2026 Mar 24;118(1):1. Available from:.
  50. Göktaş A, Yesilçimen M, Kilic A, Göktaş S, Tumbul A. Synergistic Co–Cu dual doping in ZnS thin Films: Unlocking high room-temperature ferromagnetism and UV-activated photocatalytic efficiency for multifunctional applications. Mater Chem Phys. 2025 Dec;346:131399. Available from:.
  51. Goktas A. Role of simultaneous substitution of Cu2+ and Mn2+ in ZnS thin films: Defects-induced enhanced room temperature ferromagnetism and photoluminescence. Phys E Low-dimensional Syst Nanostructures. 2020 Mar;117:113828. Available from:.
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  54. Li JB, Record MC, Tedenac JC. A thermodynamic assessment of the Sb–Zn system. J Alloys Compd. 2007 Jul;438(1–2):171–7. Available from:.
  55. Lo CWT, Svitlyk V, Chernyshov D, Mozharivskyj Y. The updated Zn–Sb phase diagram. How to make pure Zn13Sb10 (“Zn4Sb3”). Dalt Trans. 2018;47(33):11512–20. Available from:.
  56. He X, Fu Y, Singh DJ, Zhang L. Stability, electronic structures and thermoelectric properties of binary Zn–Sb materials. J Mater Chem C. 2016;4(47):11305–12. Available from:.
  57. Eklöf D, Fischer A, Wu Y, Scheidt EW, Scherer W, Häussermann U. Transport properties of the II–V semiconductor ZnSb. J Mater Chem A. 2013;1(4):1407–14. Available from:.
  58. Carter FL, Mazelsky R. The ZnSb structure; A further enquiry. J Phys Chem Solids. 1964 Jun;25(6):571–81. Available from:.
  59. Snyder GJ, Christensen M, Nishibori E, Caillat T, Iversen BB. Disordered zinc in Zn4Sb3 with phonon-glass and electron-crystal thermoelectric properties. Nat Mater. 2004 Jul 1;3(7):458–63. Available from:.
  60. Thorup PS, Christensen RS, Roelsgaard M, Iversen BB. Operando X-ray scattering study of segmented thermoelectric Zn4Sb3. J Mater Chem A. 2023;11(11):5819–29. Available from:.
  61. Song L, Roelsgaard M, Blichfeld AB, Dippel AC, Jensen KMØ, Zhang J, et al. Structural evolution in thermoelectric zinc antimonide thin films studied by in situ X-ray scattering techniques. IUCrJ. 2021 May 1;8(3):444–54. Available from:.
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  63. Nylén J, Lidin S, Andersson M, Iversen BB, Hongxue Liu, Newman N, et al. Low-temperature structural transitions in the phonon-glass thermoelectric material β-Zn4Sb3: Ordering of Zn interstitials and defects. Chem Mater. 2007 Feb 1;19(4):834–8. Available from:.
  64. Aliyeva SH, Baghban A, Ganiev B, Mammadova GA, Jamalova RH, Zohrab SG, et al. Controlled aqueous synthesis of Ag3SbS4 in the Na3SbS4–AgNO3–H2O precursor system with thermodynamic and physicochemical characterization. Solid State Sci. 2026 Sep;179:108373. Available from:.
  65. Mamedova G. Synthesis of different structural types of zeolites in the halloysite-dolomite-obsidian system. Chem J Mold. 2020 Jun;15(1):31–40. Available from:.
  66. Mamedova GA. The ion-exchange properties of natural zeolite mordenite. Fine Chem Technol. 2016 Feb 28;11(1):29–33. Available from:.
  67. Mamedova G, Nasirli G. Investigation of variousinfluencing factors of hydrothermal synthesis of analcime zeolite. Chem J Mold. 2021 May;16(1):60–7. Available from:.
  68. Mamedova GA. Influence of temperature and alkalescency on the crystallization of ZSM and ZK zeolites. Theor Found Chem Eng. 2021 May 29;55(3):479–89. Available from:.
  69. Mamedova GA. Influence of synthesis conditions on clinoptilolitic zeolite crystallization. Glas Ceram. 2021 Jul 16;78(3–4):168–71. Available from:.