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. 2022 Oct 20;7(43):38158–38192. doi: 10.1021/acsomega.2c05030

Table 2. Summary of Preparation Methods and Parameters of Ti3C2 MXenes.

synthesis method catalyst etching agents termination group synthesis parameters comments refs
HF etching TiO2/Ti3C2 HF O, OH, F 20 mL of 48% HF, 15 h etching time multilayer MXene produced with lower photocatalytic efficiency compared to monolayer counterpart (138)
2D/2D HCN/MXene HF   39% HF, 24 h etching time high purity of MXene was produced with well-defined multilayer structure (139)
39% HF, 48 h etching time the growth of anatase TiO2 on exfoliated multilayers MXene
39% HF, 96 h etching time the growth of anatase and rutile TiO2 was observed on MXene layer; more exfoliated layer and increase in the growth of TiO2 NP with increasing etching time
TiO2/Ti3C2 HF O, OH, F 49% HF, 24 h etching time (35 °C); ethyl alcohol as a washing agent; hydrothermally treated at 450 °C the formation of TiO2/Ti3C2 safflower-like morphology with ∼1 μm safflower size and shorter nanorods formation (140)
49% HF, 24 h etching time (35 °C); ethyl alcohol as a washing agent; hydrothermally treated at 550 °C average safflower size ∼2 μm upon heat increase heat treatment; well-formed safflower morphology
49% HF, 24 h etching time (35 °C); ethyl alcohol as a washing agent; hydrothermally treated at 650 °C average safflower size ∼2 μm with lower spatial density of TiO2/Ti3C2 nanorods compared to at 550 °C heat treatment; the safflower morphology slightly deformed at higher temperature
BQ/TiC/UCN HF   40% HF, 72 h etching time, 20 mL DMSO, 24 h intercalation time ultrathin MXene sheet is produced, effectively function as the electron mediator (141)
Ti3C2-QD/Ni-MOF HF   20 mL HF, 24 h etching time, DMF intercalating agent MXene QD constructed with enhance charge transfer and higher separation capabilities of the photocarriers (142)
2D/2D g-C3N4/Ti3C2TA/R (CN/TCT) MXene HF   39% HF, 24 h etching time less distribution of TiO2 NPs on the surface of MXene (121)
39% HF, 96 h etching time higher amount of TiO2 growth/conversion with more of rutile phase compared to anatase
49% HF, 24 h etching time higher distribution of TiO2 on the MXene surface when employing more concentrated etchants
49% HF, 96 h etching time both TiO2 (rutile) and TiO2 (anatase) having higher concentration due to more oxidation
acid-containing fluoride ions TiO2/Ti3C2 LiF + HCl O, OH, F LiF with 6 M HCl, 24 h etching time MXene flakes exhibit excellent hydrophilicity and dispersity with flakes size range of 10–100 nm (138)
ZnCdS/TiO2/Na-MXene LiF + HCl   LiF with 9 M of HCl, 24 h etching time (35 °C) the preintercalation of Na+ and attachment of ZnCdS nanoparticles on the MXene flakes improve the oxidation stability and slowing the oxidation to TiO2 (143)
2D-Bi2MoO6@2D MXene LiF + HCl O, OH LiF with 9 M of 20 mL HCl, 24 h etching time (35 °C) 2D MXene serves as effective platform for impeding the agglomeration and support the growth of Bi2MoO6 constructing a hierarchical composite structure (144)
Ti3AlC2/Ti3C2Tx LiF + HCl   3.08 M LiF/HCl, 6 h etching time; 1, 3, 6, 24, and 36 h delaminated MXene with more conversion to Ti3C2Tx than 1 h etched (145)
3.08 M LiF/HCl, 24 h etching time delaminated MXene are formed with residual of Ti3AlC2 was observed
3.08 M LiF/HCl, 36 h etching time delaminated MXene with residual of Ti3AlC2 was observed; partial delamination occurs even at 36 h etched time
Ti3C2Tx LiF + HCl O, OH, F LiF with 9 M HCl, 24 h etching time (30 °C) c-lattice parameter of 25.75 Å (146)
LiF with 9 M HCl, 24 h etching time (35 °C), ethanol as washing agent the highest c-lattice parameter of 30.99 Å obtained with ethanol as washing agent with improved delamination ratio
alkaline etching Ti3C2Tx KOH O, OH 5 M KOH, 120 °C hydrothermal treatment less developed of accordion-like structure of MXene; more exposed of Ti-OH sites with with alkali etching (147)
Ti3C2Tx NaOH O, OH 27.5 M NaOH treatment at 270 °C higher purity (92%) of multilayer MXene produced with removal of −F termination group (129)
27.5 M NaOH treatment at 250 °C Ti3C2Tx yield decrease with reaction temperature
5–10 M NaOH treatment at 270 °C formation of Na/K–Ti–O compounds (NTOs) due to lower concentration of NaOH, increasing the water content and facilitate oxidation
NaOH treatment at 100–220 °C no formation of MXene as reation cannot happen at lower temperature regardless of any concentration
electrochemical etching Ti3C2Tx NH4Cl, TMAOH O, OH 1 M NH4Cl, 0.2 M TMAOH higher yield of single or bilayer (>90%) with larger average dimension (126)
Ti2C HCl –Cl, −O, −OH 1 M HCl, 0.6 V, 1 day etching less conversion of MXene sheets. (128)
2 M HCl, 0.6 V, 5 days etching the formation of carbon-derived-carbide (CDC) as the results of overetching
molten salt substitution Ti3C2Tx CuCl2 –Cl, −O Ti3SiC2 in CuCl2 molten salt (750 °C) delamination of the layer proceed with the aid of SiCl4 gas molecules produced through etching process (136)
Ti3C2Tx ZnCl2 –Cl, −O Ti3ZnC2 + ZnCl2 (annealed time: 0.5 h, 1 h, 1.5 h, 3.0 h) the increasing of the ratio of molten salt, ZnCl2 in the starting precursor, a gradual conversion to Ti3C2Cl2 can be observed (134)
Ti3C2Tx NaCl2, KCl, CuCl2 –I, −Br, −Cl NaCl2, KCl, CuCl2 (mixed ratio of 1:2:2:3), 10 h annealed time in Ar (700 °C) well-configured Lewis acidic etching route could tailored the surface chemistry of MXene (148)