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Indoor air pollution can be extensively reduced by using a molecular air filtration system. However, widely utilized synthetic polymer-based filtration medium can lead to waste management difficulty after use. Consequently, this work aimed to synthesize highly efficient air nano-filters derived from renewable and biodegradable resources namely EFB and Pulp. The study successfully presented an air filter from 100 % natural cellulose using a facile physical multilayer filter fabrication method. A combination of chemical and mechanical treatment was applied to prepare nanocellulose. The chemical composition analysis showed that 66–67 % nanocellulose yield was efficiently isolated from both raw materials. The highest particle filtration efficiency (PFE) of 97.30 % (0.3 μm particle size) greater than that of commercial HEPA filters was achieved from multilayer acid-derived microfiber@mechanically treated nanofibers from EFB with low-pressure drop of 11.56 mm H2O. When %PFE and pressure drop were taken into consideration, all single-layer and multilayer-patterned fiber filters in this study provided high quality factor (QF) beyond 0.01 Pa−1which is the target of the air filter. The findings revealed that the pattern-layer filters through TBA-induced freezing-drying technique could achieve the removal of microbial model and Particulate Matters (PM1.0) represented as 0.1 and 0.3 μm particles, at the very low-pressure drop. Therefore, this study not only enhances the value of natural lignocellulosic wastes but also presents inspiring concepts for creating biodegradable cellulose-based air filters that will pave the way to more eco-friendliness and sustainability for synthetic filter replacement.

CH3NH3PbI3(MAPbI3) film was prepared by a convective method, and its X-ray diffraction spectrum displays the tetragonal perovskite structure. GeI2and GeBr2powders dissolve poorly in a mixed dimethylformamide-dimethylsulfoxide (DMF-DMSO) solvent, but the introduction of 5 wt% 5-ammonium valeric acid iodide (5-AVAI) into the mixed DMF-DMSO solvent greatly promotes GeI2and GeBr2solubility. XRD spectra of the (5-AVAI)MAPbI3, MAGexPb1–xI3, and MAGexPb1–xBr2xI3–2x(x= 0.0625 and 0.125) films exhibit a tetragonal perovskite structure, but the film morphologies become rougher than that of the pristine MAPbI3film. Discontinuous islands are formed on MAGexPb1–xI3and MAGexPb1–xBr2xI3–2x(x= 0.125) films. X-ray photoemission spectroscopy (XPS) analysis detected the Ge element on all Ge-doped films. The best performance levels of the carbon-based hole transport layer-free MAGexPb1–xI3–x(x= 0.0625, η= 3.63%) and MAGexPb1–xBr2xI3–2x(x= 0.0625, η= 2.95%) perovskite solar cells are lower than that of the pristine MAPbI3–based perovskite solar cell (η= 5.28%). This is likely due to the increased surface roughness, pin-holes, isolated islands, and the decreased light absorbance of the Ge-doped films in comparison with the pristine MAPbI3film.

The excellent giant dielectric properties (ExGDPs) are represented in the isovalent–Zr4+/pentavalent–Ta5+ions co–doped TiO2with different co–doping percentages (x%ZrTTO). The dopants were dispersed homogeneously in a highly compact–grained ZrTTO microstructure. The mean grain size and cell parameters with bond lengths slightly enlarged as x% increased. The (1%–5%) ZrTTO oxides exhibited ultra–low tanδvalues of 0.004–0.016 with the giant dielectric permittivity (ε′∼2.7–3.7 × 104); while the ε′ of the 5%ZrTTO was slightly dependent on the temperature ranging from −60 to 200 °C, following the temperature dependence requirement for application in the X7/8/9R capacitors. Impedance spectroscopy showed a very large resistance of the grain boundaries. The dielectric properties of the 1%ZrTTO were strongly dependent on the applied DC electric field, indicating the dominant internal barrier layer capacitor (IBLC) effect. However, the dielectric properties of the 5%ZrTTO were nearly independent on the applied DC electric field up to 30 V/mm, which was primarily resulted from electron localization in defect dipoles. Therefore, the ExGDPs of the x%ZrTTO were attributed to the combined effects of the IBLC and localized–electron defect–dipoles related to oxygen vacancies (Ti4+⋅e−−VO••−e−⋅Ti4+and 3Ti4+⋅e−−VO••−TaTi•) and Ti4+⋅e−−TaTi•.

This work investigates the electrochemical oxidation of melatonin at boron-doped diamond electrodes and demonstrates the significant enhancement in the detection of melatonin using highly boron-doped diamond nanopowder (h-BDD). Employing differential pulse voltammetry, Tween-coated h-BDD modified screen-printed electrodes (Tween/h-BDD/SPE) showed two linear response ranges for melatonin: 0.057–10 and 10–200 μM, with sensitivities of 390 ± 36 and 72.2 ± 3.4 μA mM–1, respectively, and a detection limit (3Sb/m) of 0.017 μM. The Tween/h-BDD/SPE demonstrated good selectivity against common interferences such as tryptophan, serotonin, lactate, cytidine, cytosine, and urea. The analytical utility of Tween/h-BDD/SPE was validated by quantifying melatonin in commercial pharmaceutical tablets, achieving close to 100% recoveries.

The giant dielectric behavior of CaCu3Ti4O12(CCTO) has been widely investigated owing to its potential applications in electronics; however, the loss tangent (tanδ) of this material is too large for many applications. A partial substitution of CCTO ceramics with either Al3+or Ta5+ions generally results in poorer nonlinear properties and an associated increase in tanδ(to ~0.29–1.15). However, first-principles calculations showed that self-charge compensation occurs between these two dopant ions when co-doped into Ti4+sites, which can improve the electrical properties of the grain boundary (GB). Surprisingly, in this study, a greatly enhanced breakdown electric field (~200–6588 V/cm) and nonlinear coefficient (~4.8–15.2) with a significantly reduced tanδ(~0.010–0.036) were obtained by simultaneous partial substitution of CCTO with acceptor-donor (Al3+, Ta5+) dopants to produce (Al3+, Ta5+)-CCTO ceramics. The reduced tanδand improved nonlinear properties were attributed to the synergistic effects of the co-dopants in the doped CCTO structure. The significant reduction in the mean grain size of the (Al3+, Ta5+)-CCTO ceramics compared to pure CCTO was mainly because of the Ta5+ions. Accordingly, the increased GB density due to the reduced grain size and the larger Schottky barrier height (Φb) at the GBs of the co-doped CCTO ceramics were the main reasons for the greatly increased GB resistance, improved nonlinear properties, and reduced tanδvalues compared to pure and single-doped CCTO. In addition, high dielectric constant values (ε′ ≈ (0.52–2.7) × 104) were obtained. A fine-grained microstructure with highly insulating GBs was obtained by Ta5+doping, while co-doping with Ta5+and Al3+resulted in a high Φb. The obtained results are expected to provide useful guidelines for developing new giant dielectric ceramics with excellent dielectric properties.

Solid CaO-based sorbents for CO2capture represent a promising alternative technology compared to traditional amine scrubbing methods. However, CaO-based sorbents are rapidly sinter and easily decrease CO2uptake capacity with regenerated carbonation–calcination cycle. Thus, in this study, doping CaO with CeO2make it an excellent candidate for improving stability and facilitating CO2capture efficiency. The dual function of CaO bio-based sorbents with varying ratios of cerium (Ce) were derived from naturally occurring blood clam using the gel-combustion method. Their nanostructures and physicochemical properties were characterized through the specific methods, including in situXAS, CO2chemisorption and physisorption, XPS, XRD, and SEM. An in-depth understanding of CO2adsorption mechanism was further emphasized using a density functional theory (DFT) simulation. The results demonstrate that nanosized CeO2-CaO, with a mole ratio of 1:9, exhibited the highest performance for CO2capture (6.44 mmol CO2/g sorbent). It is postulated that Ce serves as a physical barrier, effectively partitioning adjacent CaO grains and thereby diminishing the sintering rate. CaO is identified as the primary adsorption site, in contrast to CeO2. Mixing the Ce-Ca dual oxide initiates the electron-rich O at the O’ site. The electron localization at the O’ active site improves the activity of O’, making the performance CeCa(200) for capturing CO2capture dominant. This discovery suggests that CeO2-CaO holds promise as a sustainable alternative sorbent for future CO2capture applications.

AbstractIn this work, nanocomposites consisting of TiO2-nanorods (TiO2-NRs) with less than 100 nm in size and poly(vinylidene fluoride) (PVDF) were prepared using a liquid-phase assisted dispersion and hot-pressing methods. At 1 kHz and 25 °C, the high dielectric permittivity of ∼66 and loss tangent of ∼0.03 can be obtained in the nanocomposite with a filler volume fraction of 0.5, which was higher than that of a neat PVDF matrix by a factor of 6. Dielectric permittivity of TiO2-NRs/PVDF nanocomposites not only highly increased with TiO2-NRs, but also almost independent of the frequency range of 102–106 Hz. The significant enhancement in dielectric permittivity is mainly attributed to the interfacial polarization at the interfaces of TiO2-NRs and PVDF, and semiconducting properties of TiO2-NRs. Among the various models used for rationalizing the dielectric behavior, the experimental dielectric data is in close agreement with EMT (n = 0.11) and Yamada models (n = 8).

In the research reported in this contribution, chromium-zirconium nitride (CrZrN) layers were deposited on (100) silicon wafer by balance magnetron sputtering using argon and nitrogen as working and reactive gas, respectively. The coating layers were categorized into three groups according to zirconium content; low-zirconium (Low-Zr), medium-zirconium (Med-Zr) and high-zirconium (High-Zr). All layers had thicknesses in the range of 1.0-1.3 μm and the Med-Zr was the thickest sample. From the X-ray diffraction (XRD) results, zirconium could partially dissolve in chromium nitride (CrN) and formed complex nitride of chromium-zirconium [(Cr,Zr)N]. This phasic group was dominant for all samples, and the average crystallite sizes decreased with increasing zirconium fraction. In addition, the High-Zr sample had an extra broadened peak among (Cr,Zr)N peaks which could not clearly be identified by XRD. This ambiguity was eliminated by X-ray photoelectron spectroscopy (XPS). It was determined to be amorphous of zirconium oxynitride (Zr2ON2). Because of the high oxygen sensitivity of zirconium, it reacted with nitrogen and residual oxygen forming Zr2ON2. This study is among the first to examine the resulting nanoscale structure of the CrN layers incorporated with a high amount of zirconium.

A solid–state reaction method was used to prepare (Sr2+, Ge4+) co-doped CaCu3Ti4O12ceramics. A single-phase of CaCu3Ti4O12was detected in all the ceramics. An enormous evolution of grain growth in (Sr2+, Ge4+) co-doped CaCu3Ti4O12ceramics was observed, which was due to a liquid phase sintering mechanism. Theoretical calculations showed that Ge dopant ions are more likely substituted in Cu sites rather than Ti sites. High dielectric permittivity, ∼69,889, with a low dielectric loss tangent, ∼0.038, was achieved in a Ca0.95Sr0.05Cu3Ti3.95Ge0.05O12ceramic. Furthermore, dielectric permittivity at 1 kHz of this ceramic is more temperature-stable than that of the CaCu3Ti4O12and Ca0.95Sr0.05Cu3Ti4O12ceramics. The enhanced dielectric permittivity with reduced loss tangent in the co-doped ceramics originated from a metastable insulating phase created by a liquid phase sintering mechanism. The local insulating phase along the grain boundary layers can increase the grain boundary resistance as well as the conduction activation energy of the grain boundaries, resulting in a decreased dielectric loss tangent. An internal barrier layer capacitor model supports the origin of the giant dielectric properties in CaCu3Ti4O12-based ceramics by all results in this work.

In the research reported in this contribution, chromium-zirconium nitride (CrZrN) layers were deposited on (100) silicon wafer by balance magnetron sputtering using argon and nitrogen as working and reactive gas, respectively. The coating layers were categorized into three groups according to zirconium content; low-zirconium (Low-Zr), medium-zirconium (Med-Zr) and high-zirconium (High-Zr). All layers had thicknesses in the range of 1.0-1.3 μm and the Med-Zr was the thickest sample. From the X-ray diffraction (XRD) results, zirconium could partially dissolve in chromium nitride (CrN) and formed complex nitride of chromium-zirconium [(Cr,Zr)N]. This phasic group was dominant for all samples, and the average crystallite sizes decreased with increasing zirconium fraction. In addition, the High-Zr sample had an extra broadened peak among (Cr,Zr)N peaks which could not clearly be identified by XRD. This ambiguity was eliminated by X-ray photoelectron spectroscopy (XPS). It was determined to be amorphous of zirconium oxynitride (Zr2ON2). Because of the high oxygen sensitivity of zirconium, it reacted with nitrogen and residual oxygen forming Zr2ON2. This study is among the first to examine the resulting nanoscale structure of the CrN layers incorporated with a high amount of zirconium.

Methanol synthesis from CO2hydrogenation at high temperatures was investigated over ZnOx/ZrO2catalysts to illustrate the role of calcination temperatures (600–1000 °C) of the ZrO2support. Characterization results revealed that a ZnOx/ZrO2solid solution (Zn–O–Zr) was formed for all catalysts. The formation of the ZnOx/ZrO2solid solution was related to an enhancement of weak CO2adsorption. The ZnZr catalyst with the ZrO2calcined at 600 °C achieved the highest methanol selectivity (75.1%) at 300 °C, corresponding to the highest amount of weak basic sites. However, its methanol selectivity drastically declined as the reaction temperatures increased because the weakly adsorbed CO2could not be stabilized for hydrogenation to form methanol. A substantial reduction of weak basic sites was observed with ascending calcination temperature of ZrO2, enhancing methanol selectivity at elevated temperatures.

The effects of different exchanging ions on enhancing the photocatalytic activity of KNbTeO6are investigated where Ag, Cu, and Sn are substituted for K in an attempt to reduce the materials' band gap energy. The KNbTeO6parent compound has been successfully prepared by a solid state method. The Ag, Cu, and Sn doped samples were obtained by a facile ion exchange technique. Although only 20% of K+is exchanged with the guest ions, the band gap energy is significantly reduced from 3.38 eV in KNbTeO6to 2.76 (Ag-doped), 3.21 (Cu-doped), and 2.51 eV (Sn-doped). The detailed investigation based on the XPS spectra in the valence band region, O K-edge XANES spectra, and theoretical calculation indicates that the hybridization of Ag 4d, Cu 3d, and Sn 5s states with O 2p in the ion exchanged samples creates extra states at the top of the valence band. As a consequence, the valence band maximum shifts and the band gap energy is reduced. The magnitude of such band gap reduction is different for each guest ion and is related to the nature of the hybridization with O 2p. Here, the effects of each guest ion on the electronic structure, morphology, and surface properties are discussed. In addition to having the largest effect on band gap reduction, Sn2+also increases the dispersion of the conduction band. As a result, Sn-doped KNbTeO6exhibits the highest photocatalytic activity. The mechanism of methylene blue photodegradation is studied by using different quenchers in the presence of the Sn2+-doped KNbTeO6photocatalyst. The schematic band diagrams of each sample are proposed based on the experimental and theoretical results.

Chromium aluminum nitride (CrAlN) has been extensively studied because of high hardness, high oxidation and corrosion resistance, and good wear resistance. However, utilizing substrate treatments such as heating and voltage biasing during film deposition usually leads to relatively high surface roughness that affects wear rates. It has been found that sputter deposition at low substrate temperatures can produce nano-grain coatings with enhanced structure and mechanical properties. For this reason, the CrAlN in this study was prepared by a reactive co-sputtering technique without the substrate treatments. Effects of Al content on structure and mechanical properties were investigated by X-ray diffraction, field-emission scanning electron microscopy, energy-dispersive X-ray spectrometry, atomic force microscopy, X-ray photoelectron spectroscopy, and nanoindentation. The results suggest that these CrAlN films formed as solid solutions by substitution of Al for Cr in the CrN crystalline structure. The deposition with increasing Al but fixed N leads to N deficiency, therefore at high Al content these films form under 1:1 stoichiometric nitride. This lowers film crystallinity and hence refined film morphology. Surface roughness and hardness of the films decreased from 5.737 to 1.135 nm and from 31.69 to 26.56 GPa, respectively. However, the solid solution strengthening arising from the further increase of the Al content causes these values to rebound to 2.466 nm and to 30.16 GPa.

The degradation of para-cresol (p-cresol, 100 ppm) was assisted by Cu-Fe/NaP1 catalyst heterogeneous Fenton-like process. The characterizations of Cu-Fe/NaP1 catalyst were done for surface morphology, specific surface area and oxidation state of the elements by using scanning electron microscope (SEM), N2adsorption-desorption apparatus and X-ray photoelectron spectroscopy (XPS), respectively. The amount of Cu-Fe mass ratio, initial pH of the solution and initial hydrogen peroxide concentration was studied as the design variable. The degradation of p-cresol was found that over Cu-Fe/NaP1 catalyst gave a higher performance than Cu or Fe alone. Additionally, the alloy structure between Cu and Fe was observed in CuFeO2, which exhibited synergistic effects to enhance the p-cresol degradation efficiency. According to the design of experiment, the maximum p-cresol removal and initial reaction rate were computed and found at the optimum condition following, 58% Cu mass ratio, initial solution pH 4 and 120 mM of initial H2O2concentration. The 4-methylcatechol, 4-hydroxybenzoic acid, 4-hydroxybenzyl alcohol and 4-hydroxybenzaldehyde intermediates were observed during the degradation reaction and demonstrated as less toxic intermediates comparing with the original substance. The degradation of p-cresol was achieved by the heterogeneous Fenton-like process over the Cu-Fe/NaP1 catalyst.

Proton-free, alkali-containing layered metal oxides are thermally stable compared to their protonic counterparts, potentially allowing catalysis by Lewis acid sites at elevated temperatures. However, the Lewis acidic nature of these materials has not been well explored, as alkali ions are generally considered to promote basic but to suppress acidic character. Here, we report a rare example of an unusually acidic cesium-containing oxide CsxTi2–yMyO4(x= 0.67 or 0.70; M = Ti vacancy □ or Zn). These lepidocrocite-type microcrystals desorbed NH3at >400 °C with a total acidity of ≲410 μmol g–1at a specific surface area of only 5 m2g–1, without the need for lengthy proton–ion exchange, pillaring, delamination, or restacking. The soft and easily polarized Cs+ion essentially drives the formation of the Lewis acidic site on the surfaces as suggested by IR of sorbed pyridine. The two-dimensional layered structure was preserved after the oxide was employed in the ethanol conversion at 380 °C, the temperature at which the protonic form could have converted to anatase. The structure was also retained after the NH3temperature-programmed desorption measurement up to 700 °C. The production of ethylene from ethanol, well-known to occur over acid sites, unambiguously confirmed the acidic nature of this cesium titanate.

The effect of Sn promoter on a Ni/γ-Al2O3catalyst towards the catalytic activity and catalyst stability viathe deoxygenation of stearic acid for the production of diesel-range hydrocarbons has been investigated herein. The decarboxylation (DCO2) and decarbonylation (DCO) of stearic acid using NiSn catalysts are proposed as the main pathways to produce n-heptadecane (n-C17H36), whereas hydrodeoxygenation (HDO) is a minor pathway, as confirmed by the high ratio of C17 to C18 alkanes. Moreover, the Sn promoter in Ni/γ-Al2O3significantly improves the catalyst reusability by enhancing the tolerance to the carbon-induced deactivation. This improvement was investigated by a density functional theory (DFT) calculation. The calculation results clearly explained that the Sn promoter can weaken the interaction between carbon and the catalyst surface, tending to prevent carbon segregation on the NiSn surface. This retardation of coke formation expands the life time of the catalyst, leading to a cost-effective approach for industrial processes.

Iron catalysts on zeolite beta from incipient wetness impregnation, Fe/HBEA with Fe loading 0.5–2.0 wt% were prepared and characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic absorption spectroscopy (AAS), and temperature-programmed desorption of ammonia (NH3-TPD). Fe in all catalysts was in the form of Fe2O3and the acidity decreased with an increase of Fe content. From catalytic testing in phenol hydroxylation, the catalysts with lower Fe loading gave higher yields of catechol and hydroquinone and a lower amount of by-products than the catalyst with Fe loading 6.0 wt% in the previous work. The spent catalysts were analyzed by temperature-programmed oxidation using thermogravimetric analysis/mass spectrometry detector (TGA-MS). An amount of carbon deposit from all catalysts was in the range 10–15 wt%. However, carbon on the catalysts with lower Fe loading was removed at higher temperature.

Non-enzymatic urea detection in human dialysate offers a sustainable and spontaneous platform for advanced analysis and monitoring. This study investigated urea estimation in dialysate by using an indirect urea oxidation of nickel on nitrogen doped carbon with an incorporation of surface roughness (Rf) and double layer current (Idl). Fascinatingly, the second oxidation peak on (reverse) cathodic scan at 0.42 V vs Ag/AgCl in cyclic voltammetry and the first peak of differential pulse voltammetry (DPV) after background subtraction were evidenced to the exploited NiOOH binding with urea, concurrently with the regeneration of Ni(OH)2. In presence of more urea, the decreasing trends of the oxidation peaks in both techniques were observed and capable of determining urea concentrations in human dialysate. In consideration of actual reaction current, the measured total current after background subtraction in fresh simulated dialysate provides the sensitivity of −5.136 × 10−5A.mM−1(R2= 0.998) and limit of detection of 60.2 μM in 1–5 mM linear range. For validation in patients’ dialysate, the total current peak was normalized by Rfand subtracted from Idl, resulting in excellent urea estimation with recovery percentage between 99.18 and 102.68 in comparison to that of clinical standard, offering future prognostic monitoring and wearable artificial kidney.

Herein, NO2noxious gas sensors based on precipitation/impregnation synthesized SnO2nanoparticles loaded with Cu2O (Cu2O–SnO2) are presented. The particle properties are characterized by nitrogen adsorption, X‐ray spectroscopic, and microscopic analyses. The NO2‐sensing performances in terms of sensor response, response times, selectivity, and stability are optimized by varying Cu contents. The optimal sensing film (1.0 wt%Cu–SnO2) shows a high sensor response of ≈5680–5 ppm of NO2at a low operating temperature of 200 °C. In addition, 1.0 wt%Cu–SnO2sensor exhibits very high NO2selectivity against SO2, H2S, C2H5OH, H2, C2H2, C2H4, and CH4compared with unloaded one. Therefore, the 1.0 wt%Cu–SnO2sensor is a promising candidate for highly sensitive and selective detection of NO2. The 1.0 wt% Cu‐loaded SnO2sensor shows an ultrahigh response of 5680 to low‐ppm NO2concentrations (5 ppm) at 200 °C and very high NO2selectivity against H2S, SO2, CH4, H2, and C2H2.

The corrosion resistance of materials composed of metal is an essential property for preventing material deterioration caused by corrosion. In this study, we demonstrate that corrosion resistance can be significantly improved through the electrodeposition of molybdenum oxide onto a metal plating containing iron-group elements. Mo oxide can be electrodeposited using a simple plating bath, low current density, and short deposition time, exhibiting a fascinating metallic gloss appearance. GI-XRD and XPS analyses revealed that amorphous Mo oxide adhered to the substrate by a seed layer partially reduced to metallic Mo by the iron-group element in the substrate, based on the principle of “induced co-deposition.” A Mo oxide coating with a thickness of approximately 100 nm decreases the corrosion current density of Ni-W plating by approximately 5 times and the passivation current density by approximately 10 times in a 3 mass% NaCl solution. Mo oxide coatings represent an attractive strategy for improving the corrosion resistance of various metal materials containing iron-group elements.

The utilization of lignin as a source of phenolic compounds requires highly efficient and selective depolymerization catalysts. Herein, lignin depolymerization was investigated over Ni2P catalysts supported on nitrogen-doped activated carbon (Ni2P/AC_N). The catalysts were prepared by an incipient wetness co-impregnation method followed by reduction with H2gas. The presence of nitrogen-containing functional groups on the activated carbon surface resulted in the dispersion of Ni2P particles. The good distribution and small crystal size of Ni2P significantly increased the active surface area, which enhanced both the catalytic activity and phenol selectivity. Investigations of the catalytic activity at different reaction temperatures and lignin-to-catalyst ratios using pyrolysis–gas chromatography/mass spectrometry revealed that the highest phenol selectivity of 80% was achieved using the Ni2P/AC_N25% catalyst. The proposed reaction mechanism involves lignin depolymerization via C–O and C–C cleavage with subsequent phenol formation by demethoxylation. Owing to its high phenol selectivity, the Ni2P/AC_N catalyst has good potential for the transformation of lignin to phenol.

The studies on mechanical treatments of layered alkali metal oxides are limited despite their diverse compositions/structures and potential for property tuning. In this work, we vibratory mill Cs0.7Zn0.35Ti1.65O4, K0.8Zn0.4Ti1.6O4, and Cs2Ti6O13for up to 4 h, during which the lepidocrocite-type structure and the plate-like morphology are well preserved. X-ray diffraction (XRD) indicates a tiny (≤0.6 Å) interlayer expansion accompanied by the enhancement of the preferred orientation along the stacking direction. Chemical analyses across multiple length scales suggest Cs deintercalation, elemental redistributions, and bulk-to-surface (or crystal edge) Cs migration. This ball-milling-induced Cs-rich moiety partially blocks the surface acid sites, although the solids still show a dominating acidic character. The ball-milled samples Cs0.7–pZn0.35–qTi1.65O4−δcontain vacancies between the sheets (p) and at the sheets (qand δ). It is deduced from Sanderson’s electronegativity equalization principle and experimentally verified by X-ray photoelectron spectroscopy (XPS) that ball milling increases (decreases) the partial charge at the surface acidic Ti4+/Zn2+(basic O2–) sites. These nonporous solids (≤20 m2·g–1) contain water sorbed on the external surface as high as 1.1 mol·mol–1, which is comparable to that in a water-intercalated sample. Our work expands the current understanding of the reactivity vsrobustness in layered alkali titanates under physically demanding conditions, complementing knowledge gathered viathe soft chemistry approach.