Microstructure, Mineralogical Characterization and the Metallurgical Process Reconstruction of the Zinc Calcine Relics from the Zinc Smelting Site (Qing Dynasty)
<p>Archaeological evidence found in the Doulingxia site. (<b>a</b>) Cylindrical roasting hearths; (<b>b</b>) the unearthed zinc calcine.</p> "> Figure 2
<p>Backscattered electron images showing the morphology of the zinc calcine found at the Doulingxia site. (<b>a</b>) Low magnification, (<b>b</b>) tiny particles.</p> "> Figure 3
<p>X-ray maps showing the distributions of O, S, Zn, Fe, Pb, and Si in a partially reacted sphalerite particle. (<b>a</b>) The secondary electron (SE) image shows the morphology of the grain; (<b>b</b>) Different grey levels in the backscattered electron (BSE) image imply different compositions. A—lightly reacted sphalerite (core), B—Fe-Pb-Zn-Si-O phase (brighter rim), C—Fe-Zn-Si-O phase (dark grey rim), D—a mixture of ZnFe<sub>2</sub>O<sub>4</sub> and Zn<sub>2</sub>SiO<sub>4</sub> (grey rim), E—a mixture of ZnFe<sub>2</sub>O<sub>4</sub> and Zn<sub>2</sub>SiO<sub>4</sub> (porous portion); (<b>c</b>) O Kα map; (<b>d</b>) S Kα map; (<b>e</b>) Zn Kα map; (<b>f</b>) Fe Kα map; (<b>g</b>) Pb Lα map; and (<b>h</b>) Si Kα map.</p> "> Figure 4
<p>TG-DTA analysis result of the zinc calcine (DZC-1).</p> "> Figure 5
<p>XRD analysis results showing the phase transformation of the zinc calcine (DZC-1) reheated at different temperatures.</p> "> Figure 6
<p>Backscattered electron image showing the morphology of the zinc calcine reheated at 900 °C. 1—PbZnSiO<sub>4</sub> (light), 2—ZnFe<sub>2</sub>O<sub>4</sub> (grey), 3—Zn<sub>2</sub>SiO<sub>4</sub> (dark grey), 4—pore (black), 5—Pb<sub>10</sub>(SiO<sub>4</sub>)<sub>3</sub>(SO<sub>4</sub>)<sub>3</sub>F<sub>2</sub> (light), 6—CaSO<sub>4</sub> (dark).</p> "> Figure 7
<p>Degree of desulfurization of the products obtained under different conditions. (<b>a</b>) Products roasted at 650 °C for different roasting times, (<b>b</b>) products roasted for 48 h at different temperatures.</p> "> Figure 8
<p>Backscattered electron images showing the morphology of the final products obtained under different simulated (<b>a</b>) 650 °C; (<b>b</b>) 750 °C; (<b>c</b>) 850 °C.</p> ">
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Characterization of the Unearthed Zinc Calcine
2.3. Estimate of the Roasting Temperatures
2.4. Experimental Reconstruction of the Roasting Process
2.5. Characterization
2.5.1. Scanning Electron Microscopy Coupled with X-ray Energy Dispersive Spectrometer (SEM-EDS)
2.5.2. Thermogravimetric Analysis and Differential Thermal Analysis (TG-DTA)
2.5.3. X-ray Diffraction (XRD) Analysis
2.5.4. Wavelength Dispersive X-ray Fluorescence Measurement (WDXRF)
3. Results and Discussion
3.1. Microstructure and Mineralogical Characterization of the Unearthed Zinc Calcine
3.2. Estimate of the Roasting Temperature
3.3. Experimental Reconstruction of the Roasting Process
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
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No. | Chemical Contents (wt.%) | Phases Composition | ||||||
---|---|---|---|---|---|---|---|---|
O | S | Si | Fe | Zn | Pb | Major Phases | Minor Phases | |
DZC-1 | 14.48 | 0.33 | 2.19 | 29.01 | 26.97 | 16.90 | franklinite (ZnFe2O4), cerussite (PbCO3), willemite (Zn2SiO4) | hemimorphite(Zn4Si2O7(OH)2(H2O), anglesite (PbSO4), fluorite (CaF2), quartz (SiO2), hematite (Fe2O3) |
Hsp-1 | 8.42 | 10.64 | 1.12 | 26.85 | 24.67 | 23.40 | sphalerite ((Zn,Fe)S), galena (PbS), siderite (Fe(CO3)) | pyrrhotite (Fe7S8), pyrite (FeS2), marcasite (FeS2) |
650-1 h | 12.53 | 8.55 | 1.30 | 39.76 | 17.45 | 13.57 | sphalerite, galena | pyrrhotite, hematite, orthoclase (KAlSi3O8) |
650-6 h | 13.66 | 6.14 | 1.22 | 38.08 | 18.63 | 15.58 | sphalerite, galena, hematite | anglesite, pyrrhotite, sanidine (KAlSi3O8) |
650-12 h | 14.85 | 2.84 | 1.24 | 35.50 | 19.00 | 20.90 | sphalerite, galena, hematite | anglesite, pyrrhotite |
650-24 h | 15.64 | 2.15 | 0.84 | 38.39 | 13.71 | 23.46 | sphalerite, galena, hematite, anglesite | zincite (ZnO), franklinite |
650-48 h | 15.40 | 2.13 | 0.83 | 39.43 | 13.83 | 22.58 | sphalerite, galena, hematite, anglesite, franklinite | zincite, fluorite |
650-96 h | 16.53 | 1.95 | 0.93 | 37.16 | 15.79 | 21.99 | anglesite, hematite, franklinite, galena, zincite | zinc oxide sulfate (Zn3O(SO4)) |
650-192 h | 15.97 | 2.22 | 1.33 | 35.93 | 13.93 | 24.61 | anglesite, hematite, franklinite, galena | zincite, zinc oxide sulfate |
550-48 h | 14.51 | 4.81 | 0.61 | 37.67 | 18.04 | 19.34 | sphalerite, galena, hematite | anglesite |
750-48 h | 15.29 | 1.49 | 0.48 | 28.03 | 23.54 | 26.83 | anglesite, hematite, franklinite, zincite, galena | |
850-48 h | 13.06 | 1.06 | 0.50 | 32.29 | 24.95 | 24.06 | franklinite, zincite, hematite, anglesite, lanarkite (Pb2OSO4) | |
950-48 h | 12.22 | 0.38 | 0.41 | 38.21 | 27.41 | 16.55 | franklinite, zincite, magnetoplumbite (PbFe12O19) | hematite, willemite |
650-48 h-2 | 15.21 | 2.04 | 0.61 | 36.15 | 12.80 | 27.44 | anglesite, hematite, franklinite | zincite, galena, zinc oxide sulfate |
750-48 h-2 | 14.92 | 0.73 | 1.75 | 42.49 | 19.91 | 13.79 | hematite, franklinite, zincite, anglesite | orthoclase |
850-48 h-2 | 13.45 | 0.61 | 1.02 | 37.51 | 22.89 | 17.38 | franklinite, zincite, hematite, lanarkite | willemite, anglesite |
650-48 h-3 | 15.17 | 1.89 | 0.77 | 37.79 | 16.63 | 22.36 | anglesite, hematite, franklinite, galena, zincite | zinc oxide sulfate |
750-48 h-3 | 14.81 | 0.81 | 0.99 | 38.67 | 21.37 | 17.93 | hematite, franklinite, zincite, anglesite | orthoclase |
850-48 h-3 | 13.84 | 0.43 | 0.58 | 39.63 | 22.21 | 17.06 | franklinite, zincite, hematite | lanarkite, willemite |
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Xiao, Y.; Zhou, W.; Mo, L.; Chen, J.; Li, M.; Liu, S. Microstructure, Mineralogical Characterization and the Metallurgical Process Reconstruction of the Zinc Calcine Relics from the Zinc Smelting Site (Qing Dynasty). Materials 2021, 14, 2087. https://doi.org/10.3390/ma14082087
Xiao Y, Zhou W, Mo L, Chen J, Li M, Liu S. Microstructure, Mineralogical Characterization and the Metallurgical Process Reconstruction of the Zinc Calcine Relics from the Zinc Smelting Site (Qing Dynasty). Materials. 2021; 14(8):2087. https://doi.org/10.3390/ma14082087
Chicago/Turabian StyleXiao, Ya, Wenli Zhou, Linheng Mo, Jianli Chen, Meiying Li, and Shaojun Liu. 2021. "Microstructure, Mineralogical Characterization and the Metallurgical Process Reconstruction of the Zinc Calcine Relics from the Zinc Smelting Site (Qing Dynasty)" Materials 14, no. 8: 2087. https://doi.org/10.3390/ma14082087