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5. K--Co--Mo--Sx chalcogel: high-capacity removal of Pb2+ and Ag+ and the underlying mechanisms.

Author

Jing Nie, Roy, Subrata Chandra, Dhami, Sital, Islam, Taohedul, Amin, Ruhul, Xianchun Zhu, Taylor-Pashow, Kathryn, Han, Fengxiang X., and Islam, Saiful M.

Abstract

Chalcogenide-based aerogels, known as chalcogels, represent a novel class of nanoparticle-based porous amorphous materials characterized by high surface polarizability and Lewis base properties, exhibiting promising applications in clean energy and separation science. This work presents a K--Co--Mo--Sx (KCMS) chalcogel as a highly efficient sorbent for heavy metal ions and details its sorption mechanisms. Its incoherent structure comprises Mo2V(S2)6 and Mo3IVS(S6)2 anion-like clusters with four- and sixcoordinated Co--S polyhedra, forming a Co--Mo--S covalent network that hosts K+ ions through electrostatic attraction. The interactions of KCMS with heavy metal ions, particularly Pb2+ and Ag+, reveal that KCMS is exceptionally effective in removing these ions from ppm concentrations down to trace levels (#5 ppb). KCMS rapidly removes Ag+ (z81.7%) and Pb2+ (z99.5%) within five minutes, achieving >99.9% removal within an hour, with a distribution constant Kd $108 mL g-1. KCMS exhibits an impressive removal capacity of 1378 mg g-1 for Ag+ and 1146 mg g-1 for Pb2+, establishing it as one of the most effective materials known to date for heavy metal removal. This material is also effective for the removal of Ag+ and Pb2+ along with Hg2+, Ni2+, Cu2+, and Cd2+ from various water sources even in the presence of highly concentrated and chemically diverse cations, anions, and organic species. Analysis of the post-interacted KCMS by synchrotron X-ray pair distribution function (PDF), X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDS) revealed that the sorption of Pb2+, Ag+, and Hg2+ mainly occurs by the exchange of K+ and Co2+. Despite being amorphous, this material exhibits unprecedented ion-exchange mechanisms both for the ionically and covalently bound K+ and Co2+, respectively. This discovery advances our knowledge of amorphous gels and guides material synthesis principles for the highly selective and efficient removal of heavy metal ions from water. [ABSTRACT FROM AUTHOR]

Published
2024
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7. Amorphous K–Co–Mo–Sx Chalcogel: A Synergy of Surface Sorption and Ion‐Exchange

Author

Nie, Jing, primary, Islam, Taohedul, additional, Roy, Subrata Chandra, additional, Li, Dien, additional, Amin, Ruhul, additional, Taylor‐Pashow, Kathryn, additional, Zhu, Xianchun, additional, Feng, Renfei, additional, Chernikov, Roman, additional, Pramanik, Avijit, additional, Han, Fengxiang X., additional, Kumbhar, Amar S., additional, and Islam, Saiful M., additional

Published
2024
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9. Metal-sulfide/polysulfide functionalized layered double hydroxides – recent progress in the removal of heavy metal ions and oxoanionic species from aqueous solutions.

Author

Rohit, R. C., Roy, Subrata Chandra, Alam, Robiul, and Islam, Saiful M.

Subjects
POLYSULFIDES, LAYERED double hydroxides, HYDROXIDES, HEAVY metals, METAL ions, AQUEOUS solutions, METAL sulfides
Abstract

Water constitutes an indispensable resource for global life but remains susceptible to pollution from diverse human activities. To mitigate this issue, researchers are committed to purifying water using a variety of materials to remove harmful chemicals, such as heavy metals. Layered double hydroxides (LDHs), with their intriguing, layered structure and chemical behavior, have attained substantial attention for their effectiveness in removing heavy metal cations and various inorganic oxoanions from water. To enhance the efficiency, considerable endeavors have focused on functionalizing LDHs with different chemical species. Intercalation with metal sulfides has proven to be particularly effective, facilitating heavy metal absorption through multiple mechanisms, including ion-exchange, reductive precipitation, and surface sorption. This review concentrates on the synthesis and performance of polysulfide (Sx, x = 2–5), Mo–S, and Sn–S anion intercalated LDHs for heavy metal cations and inorganic oxoanion sorption, along with their mechanisms. Furthermore, the discussion includes prospects for expanding the chemistry of metal sulfide intercalated LDHs, with existing challenges and future outlooks. [ABSTRACT FROM AUTHOR]

Published
2024
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11. Mo3S13 Chalcogel: A High‐Capacity Electrode for Conversion‐Based Li‐Ion Batteries.

Author

Islam, Taohedul, Chandra Roy, Subrata, Bayat, Sahar, Adigo Weret, Misganaw, Hoffman, Justin M., Rao, Keerthan R., Sawicki, Conrad, Nie, Jing, Alam, Robiul, Oketola, Oluwaseun, Donley, Carrie L., Kumbhar, Amar, Feng, Renfei, Wiaderek, Kamila M., Risko, Chad, Amin, Ruhul, and Islam, Saiful M.

Subjects
LITHIUM-ion batteries, ENERGY storage, EXTENDED X-ray absorption fine structure, DISTRIBUTION (Probability theory), X-ray absorption near edge structure, ELECTRODES
Abstract

Despite large theoretical energy densities, metal‐sulfide electrodes for energy storage systems face several limitations that impact the practical realization. Here, we present the solution‐processable, room temperature (RT) synthesis, local structures, and application of a sulfur‐rich Mo3S13 chalcogel as a conversion‐based electrode for lithium‐sulfide batteries (LiSBs). The structure of the amorphous Mo3S13 chalcogel is derived through operando Raman spectroscopy, synchrotron X‐ray pair distribution function (PDF), X‐ray absorption near edge structure (XANES), and extended X‐ray absorption fine structure (EXAFS) analysis, along with ab initio molecular dynamics (AIMD) simulations. A key feature of the three‐dimensional (3D) network is the connection of Mo3S13 units through S−S bonds. Li/Mo3S13 half‐cells deliver initial capacity of 1013 mAh g−1 during the first discharge. After the activation cycles, the capacity stabilizes and maintains 312 mAh g−1 at a C/3 rate after 140 cycles, demonstrating sustained performance over subsequent cycling. Such high‐capacity and stability are attributed to the high density of (poly)sulfide bonds and the stable Mo−S coordination in Mo3S13 chalcogel. These findings showcase the potential of Mo3S13 chalcogels as metal‐sulfide electrode materials for LiSBs. [ABSTRACT FROM AUTHOR]

Published
2024
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13. Crystal structures and crystallographic classification of titanium silicophosphates – with a note on structure and composition of silicophosphates "M3P5SiO19".

Author

Glaum, Robert, Schöneborn, Marcos, Reinauer, Felix, Shaqiri, Halil, and Islam, Saiful M.

Subjects
CRYSTAL structure, OXIDATION states, MAGNETIC susceptibility, CLASSIFICATION
Abstract

The crystal structures of TiIII4[Si2O(PO4)6] ( P 3 ‾ , Z = 3, a = 14.733(1), c = 7.363(1) Å, R1 = 0.040, wR2 = 0.098, 7649 ind. refl., 170 variables), FeII0.79TiIII2.42TiIV0.79[Si2O(PO4)6] ( P 3 ‾ , Z = 3, a = 14.6534(2), c = 7.3829(1) Å, R1 = 0.036, wR2 = 0.088, 4026 ind. refl., 171 variables), and TiIII2TiIV6(PO4)6[Si2O(PO4)6] ( R 3 ‾ , Z = 1, a = 8.446(2), c = 44.21(2) Å, R1 = 0.047, wR2 = 0.120, 1373 ind. refl., 109 variables) have been refined from single-crystal data. The structures show hexagonal closest packing of phosphate groups with metal cations and [Si2O] groups occupying octahedral voids [□(PO4)6]. The close relationship of these and other silicophosphate structures to the NiAs and β-Fe2(SO4)3 (see also NaZr2(PO4)3 "NASICON") structure types is rationalized by group/subgroup considerations. This symmetry approach shows that systematic twinning is highly likely in silicophosphates, thus possibly leading to faulty crystal structure refinements. Our investigation strongly suggests that the proper composition of silicophosphates "MIII3P5SiO19" (M = Cr, V, Fe, Mo) reported in literature is actually MIII4-[Si2O(PO4)6]. In the mixed-valent compounds oxidation states were assigned to the cation sites by comparison to Ti2O3, TiP2O7 and FeTiO3. The powder reflectance spectrum of dark-blue FeII0.79TiIII2.42TiIV0.79[Si2O(PO4)6] shows a strong IVCT transition at ν ˜ = 17,500 cm−1, and magnetic susceptibility data agree very well with the proposed oxidation states. [ABSTRACT FROM AUTHOR]

Published
2024
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14. Porous Semiconducting K–Sn–Mo–S Aerogel: Synthesis, Local Structure, and Ion-Exchange Properties

Author

Blanton, Alicia, primary, Islam, Taohedul, additional, Roy, Subrata Chandra, additional, Celik, Ahmet, additional, Nie, Jing, additional, Baker, David R., additional, Li, Dien, additional, Taylor-Pashow, Kathryn, additional, Zhu, Xianchun, additional, Pramanik, Avijit, additional, Amin, Ruhul, additional, Feng, Renfei, additional, Chernikov, Roman, additional, and Islam, Saiful M., additional

Published
2023
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16. Crystal structures and crystallographic classification of titanium silicophosphates – with a note on structure and composition of silicophosphates “M3P5SiO19”

Author

Glaum, Robert, Schöneborn, Marcos, Reinauer, Felix, Shaqiri, Halil, and Islam, Saiful M.

Abstract

The crystal structures of TiIII4[Si2O(PO4)6] (P3‾$P\overline{3}$, Z= 3, a= 14.733(1), c= 7.363(1) Å, R1 = 0.040, wR2 = 0.098, 7649 ind. refl., 170 variables), FeII0.79TiIII2.42TiIV0.79[Si2O(PO4)6] (P3‾$P\overline{3}$, Z= 3, a= 14.6534(2), c= 7.3829(1) Å, R1 = 0.036, wR2 = 0.088, 4026 ind. refl., 171 variables), and TiIII2TiIV6(PO4)6[Si2O(PO4)6] (R3‾$R\overline{3}$, Z= 1, a= 8.446(2), c= 44.21(2) Å, R1 = 0.047, wR2 = 0.120, 1373 ind. refl., 109 variables) have been refined from single-crystal data. The structures show hexagonal closest packing of phosphate groups with metal cations and [Si2O] groups occupying octahedral voids [□(PO4)6]. The close relationship of these and other silicophosphate structures to the NiAs and β-Fe2(SO4)3(see also NaZr2(PO4)3“NASICON”) structure types is rationalized by group/subgroup considerations. This symmetry approach shows that systematic twinning is highly likely in silicophosphates, thus possibly leading to faulty crystal structure refinements. Our investigation strongly suggests that the proper composition of silicophosphates “MIII3P5SiO19” (M= Cr, V, Fe, Mo) reported in literature is actually MIII4-[Si2O(PO4)6]. In the mixed-valent compounds oxidation states were assigned to the cation sites by comparison to Ti2O3, TiP2O7and FeTiO3. The powder reflectance spectrum of dark-blue FeII0.79TiIII2.42TiIV0.79[Si2O(PO4)6] shows a strong IVCT transition at ν˜$\widetilde{\nu }$= 17,500 cm−1, and magnetic susceptibility data agree very well with the proposed oxidation states.

Published
2024
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21. Removal of CrO42–, a Nonradioactive Surrogate of 99TcO4–, Using LDH–Mo3S13 Nanosheets

Author

Celik, Ahmet, primary, Li, Dien, additional, Quintero, Michael A., additional, Taylor-Pashow, Kathryn M. L., additional, Zhu, Xianchun, additional, Shakouri, Mohsen, additional, Roy, Subrata Chandra, additional, Kanatzidis, Mercouri G., additional, Arslan, Zikri, additional, Blanton, Alicia, additional, Nie, Jing, additional, Ma, Shulan, additional, Han, Fengxiang X., additional, and Islam, Saiful M., additional

Published
2022
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24. Mo3S132‐ Intercalated Layered Double Hydroxide: Highly Selective Removal of Heavy Metals and Simultaneous Reduction of Ag+ Ions to Metallic Ag0 Ribbons

Author

Yang, Lixiao, primary, Xie, Linxia, additional, Chu, Menglin, additional, Wang, Hui, additional, Yuan, Mengwei, additional, Yu, Zihuan, additional, Wang, Chaonan, additional, Yao, Huiqin, additional, Islam, Saiful M, additional, Shi, Keren, additional, Yan, Dongpeng, additional, Ma, Shulan, additional, and Kanatzidis, Mercouri G, additional

Published
2021
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27. Efficient removal of chromium(VI) ions by hexagonal nanosheets of CoAl-MoS4 layered double hydroxide.

Author

Roy, Subrata Chandra, Rahman, Mohammad Arifur, Celik, Ahmet, Wilson, Sydni, Azmy, Ali, Bieber, Jay, Spanopoulos, Ioannis, Islam, Rafiq, Zhu, Xianchun, Han, Fengxiang X., and Islam, Saiful M.

Subjects
LAYERED double hydroxides, HYDROXIDES, IONS, HEXAVALENT chromium, CHROMIUM, WATER pollution
Abstract

Water pollution by hexavalent chromium, Cr(VI), poses serious concerns due to its detrimental public health effects. In this work, we report the synthesis, characterization, and sorption properties for Cr(VI) by MoS42- intercalated layered double hydroxide, CoAl-MoS4-LDH (CoAl-MoS4). Our results show that CoAl-MoS4 can effectively remove Cr(VI) ions from acidic, neutral, and basic media. At neutral medium, it exhibits a very strong affinity, Kd ∼ 1.91 × 105 mL/g, toward Cr(VI) ions. Under such conditions, this material can remove over 99% of Cr(VI) from a ∼104 ppb of Cr(VI) contaminated solutions, leaving behind residual concentration below the World Health Organization (WHO) defined limit for drinking water. Moreover, our study shows that CoAl-MoS4 is a highly-competent Cr(VI) adsorbent exhibiting a removal capacity (qm) as high as ∼231 mg/g. The CoAl-MoS4 follows pseudo-second order rate kinetics for the sorption of chromate, and the concentration dependent sorption data can be fitted well with the Langmuir sorption isotherm. Furthermore, CoAl-MoS4 is highly selective to Cr(VI) ions in the presence of various competitive ions in contaminated water systems. All these results suggest that CoAl-MoS4 is a very efficient sorbent for decontamination of hexavalent chromate from wastewater systems. [ABSTRACT FROM AUTHOR]

Published
2022
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28. Amorphous to Crystal Phase Change Memory Effect with Two-Fold Bandgap Difference in Semiconducting K2Bi8Se13

Author

Islam, Saiful M., primary, Sangwan, Vinod K., additional, Bruce Buchholz, D., additional, Wells, Spencer A., additional, Peng, Lintao, additional, Zeng, Li, additional, He, Yihui, additional, Hersam, Mark C., additional, Ketterson, John B., additional, Marks, Tobin J., additional, Bedzyk, Michael J., additional, Grayson, Matthew, additional, and Kanatzidis, Mercouri G., additional

Published
2021
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29. Distribution and Fractionation of Uranium in Weapon Tested Range Soils

Author

Kazery, Joseph A., primary, Proctor, Georgio, additional, Larson, Steve L., additional, Ballard, John H., additional, Knotek-Smith, Heather M., additional, Zhang, Qinku, additional, Celik, Ahmet, additional, Dasari, Shaloam, additional, Islam, Saiful M., additional, Tchounwou, Paul B., additional, and Han, Fengxiang X., additional

Published
2021
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30. Functionalization of clay surface for the removal of uranium from water

Author

Bao, Li, primary, Guo, Fuyu, additional, Wang, Hanrui, additional, Larson, Steven L., additional, Ballard, John H., additional, Knotek-Smith, Heather M., additional, Zhang, Qinku, additional, Nie, Jing, additional, Celik, Ahmet, additional, Islam, Saiful M., additional, Dasari, Shalom, additional, Zhang, Naiming, additional, and Han, Fengxiang, additional

Published
2021
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32. Mo3S132− Intercalated Layered Double Hydroxide: Highly Selective Removal of Heavy Metals and Simultaneous Reduction of Ag+ Ions to Metallic Ag0 Ribbons.

Author

Yang, Lixiao, Xie, Linxia, Chu, Menglin, Wang, Hui, Yuan, Mengwei, Yu, Zihuan, Wang, Chaonan, Yao, Huiqin, Islam, Saiful M., Shi, Keren, Yan, Dongpeng, Ma, Shulan, and Kanatzidis, Mercouri G.

Subjects
LAYERED double hydroxides, HEAVY metals, PRECIOUS metals, SILVER sulfide, SILVER, ADSORPTION capacity
Abstract

We demonstrate a new material by intercalating Mo3S132− into Mg/Al layered double hydroxide (abbr. Mo3S13‐LDH), exhibiting excellent capture capability for toxic Hg2+ and noble metal silver (Ag). The as‐prepared Mo3S13‐LDH displays ultra‐high selectivity of Ag+, Hg2+ and Cu2+ in the presence of various competitive ions, with the order of Ag+>Hg2+>Cu2+>Pb2+≥Co2+, Ni2+, Zn2+, Cd2+. For Ag+ and Hg2+, extremely fast adsorption rates (≈90 % within 10 min, >99 % in 1 h) are observed. Much high selectivity is present for Ag+ and Cu2+, especially for trace amounts of Ag+ (≈1 ppm), achieving a large separation factor (SFAg/Cu) of ≈8000 at the large Cu/Ag ratio of 520. The overwhelming adsorption capacities for Ag+ (qmAg=1073 mg g−1) and Hg2+ (qmHg=594 mg g−1) place the Mo3S13‐LDH at the top of performing sorbent materials. Most importantly, Mo3S13‐LDH captures Ag+ via two paths: a) formation of Ag2S due to Ag‐S complexation and precipitation, and b) reduction of Ag+ to metallic silver (Ag0). The Mo3S13‐LDH is a promising material to extract low‐grade silver from copper‐rich minerals and trap highly toxic Hg2+ from polluted water. [ABSTRACT FROM AUTHOR]

Published
2022
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33. Hierarchical Nanoassembly of MoS2/Co9S8/Ni3S2/Ni as a Highly Efficient Electrocatalyst for Overall Water Splitting in a Wide pH Range

Author

Yang, Yan, primary, Yao, Huiqin, additional, Yu, Zihuan, additional, Islam, Saiful M., additional, He, Haiying, additional, Yuan, Mengwei, additional, Yue, Yonghai, additional, Xu, Kang, additional, Hao, Weichang, additional, Sun, Genban, additional, Li, Huifeng, additional, Ma, Shulan, additional, Zapol, Peter, additional, and Kanatzidis, Mercouri G., additional

Published
2019
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35. Abrupt Thermal Shock of (NH4)2Mo3S13 Leads to Ultrafast Synthesis of Porous Ensembles of MoS2 Nanocrystals for High Gain Photodetectors

Author

Islam, Saiful M., primary, Sangwan, Vinod K., additional, Li, Yuan, additional, Kang, Joohoon, additional, Zhang, Xiaomi, additional, He, Yihui, additional, Zhao, Jing, additional, Murthy, Akshay, additional, Ma, Shulan, additional, Dravid, Vinayak P., additional, Hersam, Mark C., additional, and Kanatzidis, Mercouri G., additional

Published
2018
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36. Morphological Engineering of Winged Au@MoS2 Heterostructures for Electrocatalytic Hydrogen Evolution

Author

Li, Yuan, primary, Majewski, Marek B., additional, Islam, Saiful M., additional, Hao, Shiqiang, additional, Murthy, Akshay A., additional, DiStefano, Jennifer G., additional, Hanson, Eve D., additional, Xu, Yaobin, additional, Wolverton, Chris, additional, Kanatzidis, Mercouri G., additional, Wasielewski, Michael R., additional, Chen, Xinqi, additional, and Dravid, Vinayak P., additional

Published
2018
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38. Multistates and Polyamorphism in Phase-Change K2Sb8Se13

Author

Islam, Saiful M., primary, Peng, Lintao, additional, Zeng, Li, additional, Malliakas, Christos D., additional, Chung, Duck Young, additional, Buchholz, D. Bruce, additional, Chasapis, Thomas, additional, Li, Ran, additional, Chrissafis, Konstantinos, additional, Medvedeva, Julia E., additional, Trimarchi, Giancarlo G., additional, Grayson, Matthew, additional, Marks, Tobin J., additional, Bedzyk, Michael J., additional, Chang, Robert P. H., additional, Dravid, Vinayak P., additional, and Kanatzidis, Mercouri G., additional

Published
2018
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39. Conversion of Single Crystal (NH4)2Mo3S13·H2O to Isomorphic Pseudocrystals of MoS2 Nanoparticles

Author

Islam, Saiful M., primary, Cain, Jeffrey D., additional, Shi, Fengyuan, additional, He, Yihui, additional, Peng, Lintao, additional, Banerjee, Abhishek, additional, Subrahmanyam, Kota S., additional, Li, Yuan, additional, Ma, Shulan, additional, Dravid, Vinayak P., additional, Grayson, Matthew, additional, and Kanatzidis, Mercouri G., additional

Published
2018
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44. Abstract 5722: Serum Sonic hedgehog (Shh) and interleukin-(IL-6) as dual prognostic biomarkers in progressive metastatic breast cancer

Author

Akther, Sonam, primary, Noman, Abu Shadat M., additional, Nayeem, Junayed, additional, Raihan, Zaheer, additional, Rashid, Irfanur, additional, Rahman, Lutfur, additional, Barua, David, additional, Sultana, Afrin, additional, Shirin, Afsana, additional, Ferdous, Jannatul, additional, Parag, Rashed, additional, Rahman, Mizanur, additional, Mahmud, Reaz, additional, Jerin, Chandsultana, additional, Jahan, Nusrat, additional, Siddiqua, Ayesha, additional, Sabur, Emran, additional, Alam, Sabrina, additional, Baidya, Sunanda, additional, Islam, Saiful M., additional, and Islam, Syed S., additional

Published
2017
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45. Defect Antiperovskite Compounds Hg3Q2I2 (Q = S, Se, and Te) for Room-Temperature Hard Radiation Detection

Author

He, Yihui, primary, Kontsevoi, Oleg Y., additional, Stoumpos, Constantinos C., additional, Trimarchi, Giancarlo G., additional, Islam, Saiful M., additional, Liu, Zhifu, additional, Kostina, Svetlana S., additional, Das, Sanjib, additional, Kim, Joon-Il, additional, Lin, Wenwen, additional, Wessels, Bruce W., additional, and Kanatzidis, Mercouri G., additional

Published
2017
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46. Chalcogels as electrode materials for Li-ion batteries

Author

Doan-Nguyen, Vicky V. T., primary, Subrahmanyam, Kota S., additional, Butala, Megan M., additional, Gerbec, Jeffrey A., additional, Islam, Saiful M., additional, Kanipe, Katherine N., additional, Wilson, Catrina E., additional, Balasubramanian, Mahalingam, additional, Wiaderek, Kamila M., additional, Borkiewicz, Olaf J., additional, Chapman, Karena W., additional, Chupas, Peter J., additional, Moskovits, Martin, additional, Dunn, Bruce S., additional, Kanatzidis, Mercouri G., additional, and Seshadri, Ram, additional

Published
2017
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49. The New Semiconductor Cs4Cu3Bi9S17

Author

Zhao, Jing, primary, Islam, Saiful M., additional, Tan, Gangjian, additional, Hao, Shiqiang, additional, Wolverton, Chris, additional, Li, R. K., additional, and Kanatzidis, Mercouri G., additional

Published
2017
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