Comprehensive synthesis of Ti3C2Txfrom MAX phase to MXene

Marley Downes, Christopher E. Shuck, Bernard McBride, Jeffrey Busa, Yury Gogotsi

Published: 2024-03-19 DOI: 10.1038/s41596-024-00969-1

Synthesis

MXenes

Ti3C2Tx

MAX phase

Delamination

AI 解读

Generation of mouse–human chimeric embryos

Genome-wide quantification of transcription factor binding at single-DNA-molecule resolution using methyl-transferase footprinting

Generation of CRISPR–Cas9-mediated genetic knockout human intestinal tissue–derived enteroid lines by lentivirus transduction and single-cell cloning

A puromycin-dependent activity-based sensing probe for histochemical staining of hydrogen peroxide in cells and animal tissues

Decoding personal biotic and abiotic airborne exposome

A clinically relevant model of focal embolic cerebral ischemia by thrombus and thrombolysis in rhesus monkeys

Bioengineering human intestinal mucosal grafts using patient-derived organoids, fibroblasts and scaffolds

Biomimetic tail-to-head terpene cyclizations using the resorcin[4]arene capsule catalyst

Neuroscience robotics for controlled induction and real-time assessment of hallucinations

Scanorama: integrating large and diverse single-cell transcriptomic datasets

Single-cell RNA sequencing (scRNA-seq)（单细胞RNA测序）

Data integration（数据集成）

Heterogeneity（异质性）

查看全部

Sections

Figures

References

Naguib, M. et al. Two-dimensional nanocrystals produced by exfoliation of Ti3AlC2. Adv. Mater. 23, 4248–4253 (2011).
Downes, M. et al. M5X4: a family of MXenes. ACS Nano 17, 17158–17168 (2023).
Deysher, G. et al. Synthesis of Mo4VAlC4 MAX phase and two-dimensional Mo4VC4 MXene with five atomic layers of transition metals. ACS Nano 14, 204–217 (2020).
Maleski, K., Shuck, C. E., Fafarman, A. T. & Gogotsi, Y. The broad chromatic range of two-dimensional transition metal carbides. Adv. Opt. Mater. 9, 2001563 (2021).
Naguib, M., Barsoum, M. W. & Gogotsi, Y. Ten years of progress in the synthesis and development of MXenes. Adv. Mater. 33, 2103393 (2021).
Salles, P. et al. Electrochromic effect in titanium carbide MXene thin films produced by dip-coating. Adv. Funct. Mater. 29, 1809223 (2019).
Jiang, X. et al. Broadband nonlinear photonics in few-layer MXene Ti3C2Tx (T = F, O, or OH). Laser Photonics Rev. 12, 1700229 (2018).
Lipatov, A. et al. Electrical and elastic properties of individual single-layer Nb4C3Tx MXene flakes. Adv. Electron. Mater. 6, 1901382 (2020).
Lipatov, A. et al. Elastic properties of 2D Ti3C2Tx MXene monolayers and bilayers. Sci. Adv. 4, eaat0491 (2018).
Rosenkranz, A., Righi, M. C., Sumant, A. V., Anasori, B. & Mochalin, V. N. Perspectives of 2D MXene tribology. Adv. Mater. 35, 2207757 (2023).
Zhang, J. et al. Single platinum atoms immobilized on an MXene as an efficient catalyst for the hydrogen evolution reaction. Nat. Catal. 1, 985–992 (2018).
Ding, H. et al. Chemical scissor-mediated structural editing of layered transition metal carbides. Science 379, 1130–1135 (2023).
Lipatov, A. et al. High electrical conductivity and breakdown current density of individual monolayer Ti3C2Tx MXene flakes. Matter 4, 1413–1427 (2021).
Hantanasirisakul, K. & Gogotsi, Y. Electronic and optical properties of 2D transition metal carbides and nitrides (MXenes). Adv. Mater. 30, 1804779 (2018).
El-Demellawi, J. K. et al. Tuning the work function of Ti3C2Tx MXene by molecular doping without changing its surface functional groups. ACS Mater. Lett. 4, 2480–2490 (2022).
Zhang, C. (John) et al. Additive-free MXene inks and direct printing of micro-supercapacitors. Nat. Commun. 10, 1795 (2019).
Maleski, K., Mochalin, V. N. & Gogotsi, Y. Dispersions of two-dimensional titanium carbide MXene in organic solvents. Chem. Mater. 29, 1632–1640 (2017).
Akuzum, B. et al. Rheological characteristics of 2D titanium carbide (MXene) dispersions: A guide for processing MXenes. ACS Nano 12, 2685–2694 (2018).
Shuck, C. E. et al. Scalable synthesis of Ti3C2Tx MXene. Adv. Eng. Mater. 22, 1901241 (2020).
Shuck, C. E. & Gogotsi, Y. Taking MXenes from the lab to commercial products. Chem. Eng. J. 401, 125786 (2020).
Chen, N. et al. Supercritical etching method for the large-scale manufacturing of MXenes. Nano Energy 107, 108147 (2023).
Li, X. et al. MXene chemistry, electrochemistry and energy storage applications. Nat. Rev. Chem. 6, 389–404 (2022).
Li, K. et al. 3D MXene architectures for efficient energy storage and conversion. Adv. Funct. Mater. 30, 2000842 (2020).
Huang, K., Li, Z., Lin, J., Han, G. & Huang, P. Two-dimensional transition metal carbides and nitrides (MXenes) for biomedical applications. Chem. Soc. Rev. 47, 5109–5124 (2018).
Feng, W. et al. Ultrathin molybdenum carbide MXene with fast biodegradability for highly efficient theory-oriented photonic tumor hyperthermia. Adv. Funct. Mater. 29, 1901942 (2019).
Unal, M. A. et al. 2D MXenes with antiviral and immunomodulatory properties: a pilot study against SARS-CoV-2. Nano Today 38, 101136 (2021).
He, S. et al. Preparation strategies and applications of MXene-polymer composites: a review. Macromol. Rapid Commun. 42, 2100324 (2021).
Gong, K., Zhou, K., Qian, X., Shi, C. & Yu, B. MXene as emerging nanofillers for high-performance polymer composites: a review. Compos. Part B Eng. 217, 108867 (2021).
Iqbal, A., Sambyal, P. & Koo, C. M. 2D MXenes for electromagnetic shielding: a review. Adv. Funct. Mater. 30, 2000883 (2020).
Shahzad, F. et al. Electromagnetic interference shielding with 2D transition metal carbides (MXenes). Science 353, 1137–1140 (2016).
Han, M. et al. Beyond Ti3C2Tx: MXenes for electromagnetic interference shielding. ACS Nano 14, 5008–5016 (2020).
VahidMohammadi, A., Rosen, J. & Gogotsi, Y. The world of two-dimensional carbides and nitrides (MXenes). Science 372, eabf1581 (2021).
Mathis, T. S. et al. Modified MAX phase synthesis for environmentally stable and highly conductive Ti3C2 MXene. ACS Nano 15, 6420–6429 (2021).
Zhao, X. et al. Annealed Ti3C2Tz MXene films for oxidation-resistant functional coatings. ACS Appl. Nano Mater. 3, 10578–10585 (2020).
Zhang, J. et al. Scalable manufacturing of free-standing, strong Ti3C2Tx MXene films with outstanding conductivity. Adv. Mater. 32, 2001093 (2020).
Zeraati, A. S. et al. Improved synthesis of Ti3C2Tx MXenes resulting in exceptional electrical conductivity, high synthesis yield, and enhanced capacitance. Nanoscale 13, 3572–3580 (2021).
Alhabeb, M. et al. Guidelines for synthesis and processing of two-dimensional titanium carbide (Ti3C2Tx MXene). Chem. Mater. 29, 7633–7644 (2017).
Zhao, X. et al. Antioxidants unlock shelf-stable Ti3C2Tx (MXene) nanosheet dispersions. Matter 1, 513–526 (2019).
Habib, T. et al. Oxidation stability of Ti3C2Tx MXene nanosheets in solvents and composite films. NPJ 2D Mater. Appl. 3, 8 (2019).
Shuck, C. E. et al. Effect of Ti3AlC2 MAX phase on structure and properties of resultant Ti3C2Tx MXene. ACS Appl. Nano Mater. 2, 3368–3376 (2019).
Chae, Y. et al. An investigation into the factors governing the oxidation of two-dimensional Ti3C2 MXene. Nanoscale 11, 8387–8393 (2019).
Huang, S. & Mochalin, V. N. Understanding chemistry of two-dimensional transition metal carbides and carbonitrides (MXenes) with gas analysis. ACS Nano 14, 10251–10257 (2020).
Natu, V. et al. Edge capping of 2D-MXene sheets with polyanionic salts to mitigate oxidation in aqueous colloidal suspensions. Angew. Chem. 131, 12785–12790 (2019).
Huang, S. et al. Understanding the effect of sodium polyphosphate on improving the chemical stability of Ti3C2Tz MXene in water. J. Mater. Chem. A 10, 22016–22024 (2022).
Jolly, S., Paranthaman, M. P. & Naguib, M. Synthesis of Ti3C2Tz MXene from low-cost and environmentally friendly precursors. Mater. Today Adv. 10, 100139 (2021).
Bärmann, P. et al. Scalable synthesis of MAX phase precursors toward titanium-based MXenes for lithium-ion batteries. ACS Appl. Mater. Interfaces 13, 26074–26083 (2021).
Pang, Z. et al. Molten salt electrochemical synthesis of ternary carbide Ti3AlC2 from titanium-rich slag. Adv. Eng. Mater. 22, 1901300 (2020).
Bao, W. et al. Boosting performance of Na–S batteries using sulfur-doped Ti3C2Tx MXene nanosheets with a strong affinity to sodium polysulfides. ACS Nano 13, 11500–11509 (2019).
Li, C., Kota, S., Hu, C. & Barsoum, M. W. On the synthesis of low-cost, titanium-based MXenes. J. Ceram. Sci. Tech. 7, 301–306 (2016).
von Treifeldt, J. E. et al. The effect of Ti3AlC2 MAX phase synthetic history on the structure and electrochemical properties of resultant Ti3C2 MXenes. Mater. Des. 199, 109403 (2021).
Pazniak, A. et al. Ti3C2Tx MXene characterization produced from SHS-ground Ti3AlC2. Mater. Des. 183, 108143 (2019).
Wang, X. et al. Structure and electromagnetic properties of Ti3C2Tx MXene derived from Ti3AlC2 with different microstructures. Ceram. Int. 47, 13628–13634 (2021).
Chen, B. et al. Subsize Ti3C2Tx derived from molten-salt synthesized Ti3AlC2 for enhanced capacitive deionization. Ceram. Int. 47, 3665–3670 (2021).
Shekhirev, M. et al. Ultralarge flakes of Ti3C2Tx MXene via soft delamination. ACS Nano 16, 13695–13703 (2022).
Choi, S. B. et al. Role of oxygen in the Ti3AlC2 MAX phase in the oxide formation and conductivity of Ti3C2-based MXene nanosheets. ACS Appl. Mater. Interfaces 15, 8393–8405 (2023).
Michałowski, P. P. et al. Oxycarbide MXenes and MAX phases identification using monoatomic layer-by-layer analysis with ultralow-energy secondary-ion mass spectrometry. Nat. Nanotechnol. 17, 1192–1197 (2022).
Gao, Q. et al. Tracking ion intercalation into layered Ti3C2 MXene films across length scales. Energy Environ. Sci. 13, 2549–2558 (2020).
Seredych, M. et al. High-temperature behavior and surface chemistry of carbide MXenes studied by thermal analysis. Chem. Mater. 31, 3324–3332 (2019).
Benchakar, M. et al. One MAX phase, different MXenes: a guideline to understand the crucial role of etching conditions on Ti3C2Tx surface chemistry. Appl. Surf. Sci. 530, 147209 (2020).
Zhao, Q. et al. Adsorption of uremic toxins using Ti3C2Tx MXene for dialysate regeneration. ACS Nano 14, 11787–11798 (2020).
Kim, Y.-J. et al. Etching mechanism of monoatomic aluminum layers during MXene synthesis. Chem. Mater. 33, 6346–6355 (2021).
Hope, M. A. et al. NMR reveals the surface functionalisation of Ti3C2 MXene. Phys. Chem. Chem. Phys. 18, 5099–5102 (2016).
Sang, X. et al. Atomic defects in monolayer titanium carbide (Ti3C2Tx) MXene. ACS Nano 10, 9193–9200 (2016).
Anayee, M. et al. Kinetics of Ti3AlC2 etching for Ti3C2Tx MXene synthesis. Chem. Mater. 34, 9589–9600 (2022).
Maleski, K., Ren, C. E., Zhao, M.-Q., Anasori, B. & Gogotsi, Y. Size-dependent physical and electrochemical properties of two-dimensional MXene flakes. ACS Appl. Mater. Interfaces 10, 24491–24498 (2018).
Hart, J. L. et al. Control of MXenes’ electronic properties through termination and intercalation. Nat. Commun. 10, 522 (2019).
Inman, A. et al. Shear delamination of multilayer MXenes. J. Mater. Res. 37, 4006–4016 (2022).
Shekhirev, M. et al. Delamination of Ti3C2Tx nanosheets with NaCl and KCl for improved environmental stability of MXene films. ACS Appl. Nano Mater. 5, 16027–16032 (2022).
Wang, D. et al. Direct synthesis and chemical vapor deposition of 2D carbide and nitride MXenes. Science 379, 1242–1247 (2023).
Jawaid, A. et al. Halogen etch of Ti3AlC2 MAX phase for MXene fabrication. ACS Nano 15, 2771–2777 (2021).
Yang, S. et al. Fluoride-free synthesis of two-dimensional titanium carbide (MXene) using a binary aqueous system. Angew. Chem. 130, 15717–15721 (2018).
Kamysbayev, V. et al. Covalent surface modifications and superconductivity of two-dimensional metal carbide MXenes. Science 369, 979–983 (2020).
Li, Y. et al. A general lewis acidic etching route for preparing MXenes with enhanced electrochemical performance in non-aqueous electrolyte. Nat. Mater. 19, 894–899 (2020).
Urbankowski, P. et al. Synthesis of two-dimensional titanium nitride Ti4N3 (MXene). Nanoscale 8, 11385–11391 (2016).
Natu, V. et al. 2D Ti3C2Tz MXene synthesized by water-free etching of Ti3AlC2 in polar organic solvents. Chem 6, 616–630 (2020).
Shi, H. et al. Ambient-stable two-dimensional titanium carbide (MXene) enabled by iodine etching. Angew. Chem. Int. Ed. 60, 8689–8693 (2021).
Naguib, M. et al. Two-dimensional transition metal carbides. ACS Nano 6, 1322–1331 (2012).
Naguib, M., Mochalin, V. N., Barsoum, M. W. & Gogotsi, Y. 25th anniversary article: MXenes: a new family of two-dimensional materials. Adv. Mater. 26, 992–1005 (2014).
Hart, J. L. et al. Multimodal spectroscopic study of surface termination evolution in Cr2TiC2Tx MXene. Adv. Mater. Interfaces 8, 2001789 (2021).
Hong, W., Wyatt, B. C., Nemani, S. K. & Anasori, B. Double transition-metal MXenes: atomistic design of two-dimensional carbides and nitrides. MRS Bull. 45, 850–861 (2020).
Pinto, D. et al. Synthesis and electrochemical properties of 2D molybdenum vanadium carbides—solid solution MXenes. J. Mater. Chem. A 8, 8957–8968 (2020).
Han, M. et al. Tailoring electronic and optical properties of MXenes through forming solid solutions. J. Am. Chem. Soc. 142, 19110–19118 (2020).
Ahmed, B., Ghazaly, A. E. & Rosen, J. i-MXenes for energy storage and catalysis. Adv. Funct. Mater. 30, 2000894 (2020).
Lim, K. R. G. et al. Fundamentals of MXene synthesis. Nat. Synth. 1, 601–614 (2022).
Ghidiu, M. et al. Synthesis and characterization of two-dimensional Nb4C3 (MXene). Chem. Commun. 50, 9517–9520 (2014).
Ghidiu, M., Lukatskaya, M. R., Zhao, M.-Q., Gogotsi, Y. & Barsoum, M. W. Conductive two-dimensional titanium carbide ‘clay’ with high volumetric capacitance. Nature 516, 78–81 (2014).
Anayee, M. et al. Role of acid mixtures etching on the surface chemistry and sodium ion storage in Ti3C2Tx MXene. Chem. Commun. 56, 6090–6093 (2020).
Driscoll, N. et al. Two-dimensional Ti3C2 MXene for high-resolution neural interfaces. ACS Nano 12, 10419–10429 (2018).
Mashtalir, O. et al. Intercalation and delamination of layered carbides and carbonitrides. Nat. Commun. 4, 1716 (2013).
Lukatskaya, M. R. et al. Cation intercalation and high volumetric capacitance of two-dimensional titanium carbide. Science 341, 1502–1505 (2013).
Mashtalir, O., Lukatskaya, M. R., Zhao, M.-Q., Barsoum, M. W. & Gogotsi, Y. Amine-assisted delamination of Nb2C MXene for Li-ion energy storage devices. Adv. Mater. 27, 3501–3506 (2015).
Lipatov, A. et al. Effect of synthesis on quality, electronic properties and environmental stability of individual monolayer Ti3C2 MXene flakes. Adv. Electron. Mater. 2, 1600255 (2016).
Wei, Y., Zhang, P., Soomro, R. A., Zhu, Q. & Xu, B. Advances in the synthesis of 2D MXenes. Adv. Mater. 33, 2103148 (2021).
Verger, L. et al. Overview of the synthesis of mxenes and other ultrathin 2D transition metal carbides and nitrides. Curr. Opin. Solid State Mater. Sci. 23, 149–163 (2019).
Verger, L., Natu, V., Carey, M. & Barsoum, M. W. MXenes: an introduction of their synthesis, select properties, and applications. Trends Chem. 1, 656–669 (2019).
Shekhirev, M., Shuck, C. E., Sarycheva, A. & Gogotsi, Y. Characterization of MXenes at every step, from their precursors to single flakes and assembled films. Prog. Mater. Sci. 120, 100757 (2021).
Shuck, C. E. et al. Safe synthesis of MAX and MXene: guidelines to reduce risk during synthesis. ACS Chem. Health Saf. 28, 326–338 (2021).
Lakhe, P. et al. Process safety analysis for Ti3C2Tx MXene synthesis and processing. Ind. Eng. Chem. Res. 58, 1570–1579 (2019).
Kotasthane, V. et al. Selective etching of Ti3AlC2 MAX phases using quaternary ammonium fluorides directly yields Ti3C2Tz MXene nanosheets: implications for energy storage. ACS Appl. Nano Mater. 6, 1093–1105 (2023).
Li, M. et al. Element replacement approach by reaction with Lewis acidic molten salts to synthesize nanolaminated MAX phases and MXenes. J. Am. Chem. Soc. 141, 4730–4737 (2019).
Chen, J. et al. Molten salt-shielded synthesis (MS3) of MXenes in air. Energy Environ. Mater. 6, e12328 (2023).
Liu, L. et al. Exfoliation and delamination of Ti3C2Tx MXene prepared via molten salt etching route. ACS Nano 16, 111–118 (2022).
Arole, K. et al. Water-dispersible Ti3C2Tz MXene nanosheets by molten salt etching. iScience 24, 103403 (2021).
Li, T. et al. Fluorine-free synthesis of high-purity Ti3C2Tx (T = OH, O) via alkali treatment. Angew. Chem. Int. Ed. 57, 6115–6119 (2018).
Wang, C. et al. HCl-based hydrothermal etching strategy toward fluoride-free MXenes. Adv. Mater. 33, 2101015 (2021).
Yang, Y. et al. Correlating electronic properties with M-site composition in solid solution TiyNb2-yCTx MXenes. 2D Mater. 10, 014011 (2022).
Matthews, K., Zhang, T., Shuck, C. E., VahidMohammadi, A. & Gogotsi, Y. Guidelines for synthesis and processing of chemically stable two-dimensional V2CTx MXene. Chem. Mater. 34, 499–509 (2022).
Mendoza-Sánchez, B. et al. Systematic study of the multiple variables involved in V2AlC acid-based etching processes, a key step in MXene synthesis. ACS Appl. Mater. Interfaces http://doi.org/10.1021/acsami.3c01671 (2023).
Alhabeb, M. et al. Selective etching of silicon from Ti3SiC2 (MAX) to obtain 2D titanium carbide (MXene). Angew. Chem. 130, 5542–5546 (2018).
Forsberg, K., Van den Borre, A., Henry, N. III & Zeigler, J. P. Quick Selection Guide to Chemical Protective Clothing 7th edn (John Wiley & Sons, 2020).

Comprehensive synthesis of Ti3C2Txfrom MAX phase to MXene

Supplementary information

Supplementary Information

Reporting Summary

推荐阅读