Smaller Primary Particle Size Research Articles

A three-dimensional TiO2-Graphene architecture with superior Li ion and Na ion storage performance

In this work, a three-dimensional TiO2-graphene composite with large specific surface area is designed by freeze drying. In this architecture, primary TiO2 nanoparticles (less than 10 nm in size) are wrapped with graphene homogeneously, forming spherical secondary particles (≈100 nm), and the spherical TiO2 particles further agglomerate into platelet-like particles with several micrometers in size. The TiO2-graphene composite delivers high de-lithiation and de-sodiation capacities of 312 mAh g−1 and 280 mAh g−1 at 17 mA g−1 as negative electrode materials in lithium and sodium cells, respectively, and excellent cycling performance with negligible capacity loss after 500 cycles at a specific current of 85 mA g−1. When coupled with an activated carbon positive electrode, it demonstrates high capacitance and long cycle life in sodium ion capacitors (81% after 2000 cycles at 1 A g−1) and lithium ion capacitors (95% after 5000 cycles at 1 A g−1). Its superior performance benefits from the designed 3D architecture, which combines the advantages of small primary particle size, a homogeneous carbon coating and an adequate contact area with the liquid electrolyte. The storage mechanisms of the superior TiO2-graphene composite in lithium and sodium cells are investigated by operando X-ray diffraction studies.

Impact of methanol alternative fuel on oxidation reactivity of soot emissions from a modern CI engine

This paper compared the soot reactivity and its primarily related factors including soot structure, graphitization degree and surface functional groups, when using mineral diesel fuel (DF) and methanol blended fuel (MBF) at two typical low and high engine loads. Results showed that the soot reactivity increases with increasing methanol concentration in the MBF. Additionally, with the constant methanol blend ratio of methanol, the reactivity of MBF soot degrades as the engine load increases. Correspondingly, the MBF soots had lower aggregate compactness, smaller primary particle size, more disordered structure and more active aliphatic C-H groups in comparison with the DF soot, providing higher concentration and accessibility of active sites for oxidation reactions. The addition of methanol creates variations in combustion kinetics and fuel formulation, which exerts reverse effects on the soot structure and chemistry. Therefore, the factors related to these properties show non-monotonic variations when alter the methanol blend ratio and engine operating mode. Especially, when the methanol blend ratio increases from 10% to 15%, the soot structure and chemistry transform onto the features that are reluctant for soot oxidation.

Morphology analysis of soot particles from a modern diesel engine fueled with different types of oxygenated fuels

Using a transmission electron microscopy (TEM), the morphological characteristic variations of exhaust soot particles have been studied on a modern diesel engine fuelled with a commercial diesel fuel (D100, as a baseline fuel) and three different oxygenated fuel blends with the same oxygen content, including a 11.5% methanol blend (M11.5), a 8.3% dimethyl carbonate blend (DMC8.3), and a 13% dimethyl methane blend (DMM13). The results showed that oxygenated fuel blends emitted smaller soot primary particles with respect to neat diesel, with the most significant decrease in M11.5 followed by DMM13 and DMC8.3. Similar variations with primary particle diameter were found in the decrease of the mean radius of gyration, mean primary particle number and estimated mass for an agglomerate when making comparisons among diesel and the three oxygenated fuel blends. Aggregates shape analysis showed that M11.5 soot had the minimal trend to form a rather circular structure and maximal boundary irregularity among the four fuels, while all soot particles showed larger deviation to the sphere (i.e. higher elongation) regardless of fuel type used. In addition, both mass and perimeter fractal dimension showed consistent results for diesel and the three oxygenated fuel blends, with the particle aggregates being the least compacted morphology for M11.5, followed by DMM13, DMC8.3 and diesel. Therefore, compared to diesel, the exhaust soot particles from the oxygenated fuel blends (especially for M11.5) are more prone to be trapped (lowest fractal dimension) and display a higher reactivity towards oxidation (smallest primary particle size).

Correlation of Feedstock Powder Characteristics with Microstructure, Composition, and Mechanical Properties of La2Ce2O7 Coatings Produced by Plasma Spray-Physical Vapor Deposition

By virtue of plasma spray-physical vapor deposition (PS-PVD) process, coatings in possession of columnar structures can be obtained by suitable processing parameters coupled with specially designed powder feedstock. In this paper, the influence of powder characteristics on the La2Ce2O7 (LC) coating microstructures was investigated by using three kinds of feedstock powders with same PS-PVD processing parameters. It was found that small agglomerated feedstock, weak binding strength, and small primary particle sizes can enhance the feedstock evaporation rate, thus obtaining well columnar structured coatings. X-ray diffraction (XRD) patterns revealed that except for a very small amount of La2O3 the main phase of all the coatings is LC. The La/Ce atomic ratios reduced in the coatings compared to the feedstocks, especially the coatings with better columnar structure. Super-lattice patterns were observed by transmission electron microscope (TEM), which means that the LC phase is supposed to be pyrochlore structure. Furthermore, the mechanical properties evaluated by nano-indentation tests indicated that both the hardness and Young’s modulus of each coating show negative correlations with the porosity inside the columns.

MOF-Derived Co3O4 Polyhedrons as Efficient Polysulfides Barrier on Polyimide Separators for High Temperature Lithium-sulfur Batteries.

The incorporation of highly polarized inorganic compounds in functional separators is expected to alleviate the high temperature safety- and performance-related issues for promising lithium–sulfur batteries. In this work, a unique Co3O4 polyhedral coating on thermal-stable polyimide (PI) separators was developed by a simple one-step low-temperature calcination method utilizing metal-organic framework (MOF) of Co-based zeolitic-imidazolate frameworks (ZIF-Co) precursors. The unique Co3O4 polyhedral structures possess several structural merits including small primary particle size, large pore size, rich grain boundary, and high ionic conductivity, which endow the ability to adequately adsorb dissolved polysulfides. The flexible-rigid lithium-lanthanum-zirconium oxide-poly(ethylene oxide) (LLZO-PEO) coating has been designed on another side of the polyimide non-woven membranes to inhibit the growth of lithium dendrites. As a result, the as-fabricated Co3O4/polyimide/LLZO-PEO (Co3O4/PI/LLZO) composite separators displayed fair dimensional stability, good mechanical strength, flame retardant properties, and excellent ionic conductivity. More encouragingly, the separator coating of Co3O4 polyhedrons endows Li–S cells with unprecedented high temperature properties (tested at 80 °C), including rate performance 620 mAh g−1 at 4.0 C and cycling stability of 800 mAh g−1 after 200 cycles—much better than the state-of-the-art results. This work will encourage more research on the separator engineering for high temperature operation.

Spherical nanoparticle effects on the lower critical solution temperature phase behavior of poly(ε‐caprolactone)/poly(styrene‐co‐acrylonitrile) blends: Separation of thermodynamic aspects from kinetics

ABSTRACTThe effects of spherical nanosilica particles on the lower critical solution temperature (LCST) phase diagram of poly(ε‐caprolactone) (PCL)/poly(styrene‐co‐acrylonitrile) (SAN) blends are investigated by using isochronal dynamic temperature sweep tests at different cooling rates. A stronger dependency of the rheologically determined phase‐transition points on the cooling rate is observed in the presence of nanoparticles, which results from the large contribution of entropic surface tension of chains in the Gibbs free energy of mixing and much slower rate of PCL/SAN phase dissolution. By alleviating the effects of kinetic factors, it is found that the drop in the LCST‐type phase boundary of PCL/SAN blends by adding nanofiller is more apparent than real. However, the closest LCST phase diagram to the real steady‐state thermodynamic diagram shows an unexpected shift to lower temperatures by adding nanosilica. The migration of nanosilica particles to the SAN domains especially at lower cooling rates in the dynamic measurements is the most likely explanation of these observations. The findings that prove the profound impact of kinetic factors in dynamic temperature measurements are reached in a hybrid system, wherein the SAN chains are preferentially absorbed on the surface of a nanofiller having very small primary particle size. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019, 137, 48679.

Tribological properties of oxidized wood-derived nanocarbons with same surface chemical composition as graphene oxide for additives in water-based lubricants

The tribological properties of oxidized wood-derived nanocarbons (oWNCs), which have the same surface chemical composition as graphene oxide (GO), were investigated as additives in water-based lubricants using a sintered tungsten carbide ball and a stainless steel flat plate with a reciprocating sliding configuration. WNCs were synthesized from four kinds of Japanese wood powder by metal-catalyzed carbonization, and were strongly oxidized by a modified Hummer's method. The four oWNCs have aggregated chain-like nanostructures and maintain graphitic layers. In addition, the four oWNCs were well-dispersed in water due to their high level of oxidation. The four oWNC aqueous dispersions improved lubrication. In particular, the aqueous dispersion of the oWNC derived from Japanese cedar (J. Cedar) wood powder showed a very low friction coefficient and formed a thick tribofilm on the plate surface. The most distinctive properties of the J. Cedar oWNC, compared to the other oWNCs, were the small primary and secondary particle sizes, which were much smaller than those of the other oWNCs. The small-sized J. Cedar oWNC may possibly enter the frictional interface, preventing direct contact between the ball and plate surfaces and forming a tribofilm.

The Effects of a Mixed Precipitant on the Morphology and Electrochemical Performance of LiNi0.5Mn1.5O4 Cathode Materials

A series of LiNi0.5Mn1.5O4 (LNMO) samples were synthesized by adjusting the molar ratio of (NH4)2CO3 to Na2CO3 in a mixed precipitant for evaluating the effects of ammonia from (NH4)2CO3 as a complexing agent and Na2CO3 as a precipitant on the morphology and electrochemical performances of LNMO. In this research, a rapid precipitation method followed by hydrothermal treatment was used to prepare the precursors of LNMO, and different molar ratios (0:1, 1:2, 1:1, 2:1, 1:0) of (NH4)2CO3 to Na2CO3 were used for mixed precipitants. The test results revealed that the cathode material exhibits the best electrochemical performance when the molar ratio of (NH4)2CO3 to Na2CO3 is set at 1:2, displaying a specific discharge capacity of 129.4 mA h g−1 at 0.5 C and a capacity retention of 82.3% after 200 charge–discharge cycles. In addition, it still shows a high rate performance with a discharge capacity of 112.7 mA h g−1 at 10 C and 98.8 mA h g−1 at 20 C, which is attributed to an accurate Ni/Mn ratio, smaller primary particle sizes and a porous spherical morphology.

Influence of calcination atmosphere on structure and electrochemical behavior of LiNi0.6Co0.2Mn0.2O2 cathode material for lithium-ion batteries

Layered Ni-rich LiNi0.6Co0.2Mn0.2O2 (LNCMO) materials are prepared by calcining the mixture of Ni0.6Co0.2Mn0.2(OH)2 precursor (co-precipitation method) and Li salts (Li2CO3). Two different caicination atmosphere (air and oxygen) are adopted to obtain final two samples of LNCMO-A (air) and LNCMO-O (oxygen) to individually investigate the influence of oxygen instead of air atmosphere on the structure and electrochemical behavior of the LNCMO materials. Both two samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and electrochemical charge/discharge tests including cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). XRD and SEM results show the LNCMO-O sample possesses relatively smaller Li+/Ni2+ cation mixing, better layer-structure ordering and smaller primary particle size. The electrochemical charge/discharge test results show the LNCMO-O sample exhibits superior discharge capacity (184.6mAhg−1 at 0.1C), higher cycling retention (91.4% after 100 cycles at 0.5C) and promoted rate performance. Further XPS, CV and EIS analyses on the promotion mechanism demonstrate that the oxygen-atmosphere calcination is important and beneficial to improve the electrochemical performance for Ni-rich LiNi0.6Co0.2Mn0.2O2 material.

Effect of Lithium Content on Spinel Phase Evolution in Lithium-Rich Layered Oxides LixNi0.25Co0.10Mn0.65O(3.4+x)/2 (0.8 ≤ x ≤ 1.6) for Li-Ion Batteries

Lithium-rich oxides LixNi0.25Co0.10Mn0.65O(3.4+x)/2 (x=1.6, 1.4, 1.2, 1.0, 0.8) were synthesized and characterized for their structural, morphological, and performance as cathode materials in Li-ion batteries. The baseline composition x=1.4 had been previously determined as having the best electrochemical performance due to its small primary particle size and homogeneous distribution of nano-domains consisting of (C2/m) and (R3¯m) phases. In this study, the Rietveld refinement results indicate the presence of two phases at high lithium levels (x=1.6 and 1.4): Li2MnO3 (C2/m) and Li M O2 ( M = Ni, Co, Mn) (R3¯m); the latter contains Ni2+ and Ni3+. At low lithium levels (x=1.2, 1.0, and 0.8) an additional spinel phase Li M 2O4 (Fd3¯m) emerges, which is known to affect the electrochemical performance of the oxide. Structural analysis reveals that the spinel phase contains mixed transition metals Ni, Co, and Mn as [Li+,Co2+][Ni2+,Co3+,Mn4+]2O4. A low lithium level is found to induce primary particle growth, as well as Co and Ni segregation within the secondary particles. These results are expected to contribute to material optimization and commercialization of lithium-rich oxide cathodes.

High‐Performance Flexible Solid‐State Asymmetric Supercapacitors based on Ordered Mesoporous Cobalt Oxide

AbstractAsymmetric supercapacitors (ASCs) have attracted growing interest and attention in the field of supercapacitors owing to their high energy density and power density. In this work, ordered mesoporous Co3O4 samples with different pore sizes (ca. 20 nm and ca. 70 nm) are prepared via a hard template method. Flexible solid‐state ASC devices based on mesoporous Co3O4 with pore size of 20 nm and activated carbon possesses a specific capacitance of 215 mF cm−2 (at 1.5 mA cm−2) and show excellent cycling performance. Electrochemical tests reveal that the mesoporous material with a larger specific surface area, that is, a smaller primary particle size, is more suitable for solid‐state ASC device. The results provide a potential electrode material for ACSs.

Design of spray dried insulin microparticles to bypass deposition in the extrathoracic region and maximize total lung dose

Inhaled drugs all too often deliver only a fraction of the emitted dose to the target lung site due to deposition in the extrathoracic region (i.e., mouth and throat), which can lead to increased variation in lung exposure, and in some instances increases in local and systemic side effects. For aerosol medications, improved targeting to the lungs may be achieved by tailoring the micromeritic properties of the particles (e.g., size, density, rugosity) to minimize deposition in the mouth-throat and maximize the total lung dose. This study evaluated a co-solvent spray drying approach to modulate particle morphology and dose delivery characteristics of engineered powder formulations of insulin microparticles. The binary co-solvent system studied included water as the primary solvent mixed with an organic co-solvent, e.g., ethanol. Factors such as the relative rate of evaporation of each component of a binary co-solvent mixture, and insulin solubility in each component were considered in selecting feedstock compositions. A water-ethanol co-solvent mixture with a composition range considered suitable for modulating particle shell formation during drying was selected for experimental investigation. An Alberta Idealized Throat model was used to evaluate the in vitro total lung dose of a series of spray dried insulin formulations engineered with different bulk powder properties and delivered with two prototype inhalers that fluidize and disperse powder using different principles. The in vitro total lung dose of insulin microparticles was improved and favored for powders with low bulk density and small primary particle size, with reduction of deposition in the extrathoracic region. The results demonstrated that a total lung dose >95% of the delivered dose can be achieved with engineered particles, indicating a high degree of lung targeting, almost completely bypassing deposition in the mouth-throat.

Synthesis of nanoparticles-assembled Co3O4 microspheres as anodes for Li-ion batteries by spray pyrolysis of CoCl2 solution

Nanoparticles-assembled Co3O4 microspheres with different primary particle size are synthesized via a facile one-step ultrasonic spray pyrolysis process, using CoCl2·6H2O as precursor. The as-synthesized Co3O4 powders are directly used as anode material for Li-ion batteries without further calcinations. The primary particle size is tuned by controlling the spray pyrolysis temperature and its effects on the electrochemical performance of the prepared samples are systemically investigated. The results reveal that primary particles size exerts significant effect on the initial coulombic efficiency, specific capacity and rate performance. In addition, we find that the temperature of powder collector strongly influences the chlorine content in the products, which is resulted from the chloridization of Co3O4 by gaseous HCl from the off-gas. A simple and effective strategy is proposed to prevent the chloridization reaction. The sample with the smallest primary particle size and low Cl content shows the highest initial coulombic efficiency of 73% and a high reversible capacity of 1340mAhg−1 after 50 cycles at a current density of 200mAg−1.

Structures, Electrochemical Properties, and Phase Evolution Behaviors of LiNi1-xMnxO2-δ (0 ≤ x ≤ 1/2) as Cathode Materials for Secondary Lithium Batteries

In an attempt to get Co-free layered materials for cathode of secondary lithium batteries, LiNi1-xMnxO2-δ (0 ≤ x ≤ 1/2) samples were synthesized by co-precipitation reactions followed by heating in an O2 atmosphere. The optimum heating temperature to get a single-phase hexagonal layered structure increased with Mn contents in the compound. Oxygen vacancies could be gradually reduced with Mn-substitutions. While the lattice constants, M-O distance, and MO2 slab thickness increased with Mn contents, Li-O and inter-slab distances decreased. Electrical conductivities decreased with Mn contents because of the decreased carrier mobility that resulted from smaller primary particle sizes as well as lager amounts of cation mixing. Samples of x = 1/12 and 1/9 in LiNi1-xMnxO2-δ exhibited 0.1 C-rate discharge capacities of 216.2 and 208.9 mAh g−1 and first cycle efficiencies of 93.3 and 94.0%, respectively. The sample of x = 1/9 in LiNi1-xMnxO2-δ exhibited the highest rate capability. From the systematically investigated phase evolution behaviors, a higher activation energy as well as a slower rate of phase transition reaction for higher Mn contents phase were observed.

In vitro and in vivo genotoxicity investigations of differently sized amorphous SiO2 nanomaterials

In vitro and in vivo genotoxic effects of differently sized amorphous SiO2 nanomaterials were investigated. In the alkaline Comet assay (with V79 cells), non-cytotoxic concentrations of 300 and 100–300μg/mL 15nm-SiO2 and 55nm-SiO2, respectively, relevant (at least 2-fold relative to the negative control) DNA damage. In the Alkaline unwinding assay (with V79 cells), only 15nm-SiO2 significantly increased DNA strand breaks (and only at 100μg/mL), whereas neither nanomaterial (up to 300μg/mL) increased Fpg (Formamidopyrimidine DNA glycosylase)-sensitive sites reflecting oxidative DNA base modifications. In the Comet assay using rat precision-cut lung slices, 15nm-SiO2 and 55nm-SiO2 induced significant DNA damage at ≥100μg/mL. In the Alkaline unwinding assay (with A549 cells), 30nm-SiO2 and 55nm-SiO2 (with larger primary particle size (PPS)) induced significant increases in DNA strand breaks at ≥50μg/mL, whereas 9nm-SiO2 and 15nm-SiO2 (with smaller PPS) induced significant DNA damage at higher concentrations. These two amorphous SiO2 also increased Fpg-sensitive sites (significant at 100μg/mL). In vivo, within 3 days after single intratracheal instillation of 360μg, neither 15nm-SiO2 nor 55nm-SiO2 caused genotoxic effects in the rat lung or in the bone marrow. However, pulmonary inflammation was observed in both test groups with findings being more pronounced upon treatment with 15nm-SiO2 than with 55nm-SiO2. Taken together, the study shows that colloidal amorphous SiO2 with different particle sizes may induce genotoxic effects in lung cells in vitro at comparatively high concentrations. However, the same materials elicited no genotoxic effects in the rat lung even though pronounced pulmonary inflammation evolved. This may be explained by the fact that a considerably lower dose reached the target cells in vivo than in vitro. Additionally, the different time points of investigation may provide more time for DNA damage repair after instillation.

Salt-assisted synthesis of mesostructured cellular foams consisting of small primary particles with enhanced hydrothermal stability

Mesoporous silica materials have attracted considerable attention as adsorbents, catalyst supports, and drug delivery carriers due to their large surface area, high pore volume, and controllable pore size. To increase the adsorption or mass transport properties, large pore sized mesoporous silica is highly desired. Here, we demonstrate a new green synthetic route for obtaining salt-assisted mesostructured cellular foams (S-MCFs) using a triblock copolymer as a single structure-directing agent by addition of inorganic salt without using a hydrophobic pore expander. The S-MCF was composed of ∼27 nm cellular pores and 10 nm windows and had distinct pore walls and a cellular structure. S-MCFs showed an enhanced hydrothermal stability compared to other mesocellular silica. In addition, the primary particle size of the S-MCF was 100–300 nm, which is much smaller than that of previously reported mesostructured cellular foams (MCFs) and mesocellular silica foam (MSU-F). The adsorption study using a model protein revealed that small primary particle size in S-MCF is beneficial for mass transfer in a short period of time. Therefore, S-MCF may serve as a potential platform for higher mass transport or adsorption of large molecules with good stability.

Thermo- and pH-responsive fluorescence behaviors of sulfur-functionalized detonation nanodiamond-poly(N-isopropylacrylamide)

Detonation nanodiamonds (DNDs) are emerging as bioimaging platforms due to their biocompability, small primary particle size, reactive surface, and stable fluorescence after modification. In this paper, a heteroatom engineering method is provided to fabricate the fluorescent DNDs through pyrolysis of dibenzyl disulfide. The quantum yield of these sulfur (S)-functionalized DNDs (SDNDs) increases with sulfur percentage. The solubility and stability of SDNDs in aqueous solution are also significantly increased due to the formation of hydrophilic sulfur groups on DND. Furthermore, these SDNDs are used to conjugate the stimuli-responsive poly(N-isopropylacrylamide) (PNIPAM) through the ‘graft from’ method. The conjugation demonstrated both pH- and thermo-responsive fluorescence behaviors, which shows promise to be used in ratiometric fluorescence sensing for the detection of intracellular pH and temperature values.

Methanol synthesis over Cu–ZnO aggregates supported on carbon nanotubes

Methanol synthesis was studied with catalysts containing Cu and ZnO in the interior space or on the exterior surface of multi-walled carbon nanotubes (CNTs) and were activated by different procedures – reduction in dilute H2 at 513K with or without subsequent exposure to 10% CO/H2 at 673K for 30min. Characterization of the transition-metal species after these treatments by XRD and XAFS revealed striking differences. After mild reduction, XRD reflections related to Cu were missing or were of weak intensity, which could be assigned to very low primary particle sizes as detected by EXAFS. After treatment in CO/H2, reflections arising from alloy phases were obtained for all samples while non-alloyed Cu, although observed by EXAFS, escaped detection by XRD due to small primary particle sizes. Reduction of Zn2+ to Zn(0) was revealed by ZnK XANES only for some samples, which qualifies Zn(0) as a minority oxidation state for the remaining ones. Based on the XANES evidence, a new feature in ZnK EXAFS developing after CO/H2 treatment was interpreted as arising from either alloying or from an SMSI-type interaction of ZnO1−x entities with Cu nanoparticle surfaces. The catalysts exhibited very different productivities and responses to the CO/H2 treatment. In terms of specific activity (related to m2 Cu), the better samples achieved a multiple of the performance shown by a commercial reference, but suffered from insufficient stability. By contrast, such stability was demonstrated for a catalyst containing Cu/ZnO hosted in SBA-15. A catalyst series based on narrow CNTs previously functionalized by thermal shocks in flowing air stood out due to poor performance for unknown reasons. Due to these uncertainties, the data does not permit clear conclusions on the oxidation state of Zn in the promoting interaction with Cu although the general trends favor Zn2+ over Zn(0).

Micro-nano structure Na2MnPO4F/C as cathode material with excellent sodium storage properties

Micro-nano structure Na2MnPO4F/C composite was prepared via wet ball milling and in situ pyrolytic carbon coating process. The micrometre-scale secondary aggregates are composed of small primary nanoparticles (10–30nm) wrapped in carbon network, and present mesoporous structure. The material served as cathode in sodium ion (Na-ion) battery exhibits excellent capacity capability and cycling behavior. At a current density of 10mAg−1, it can deliver a specific discharge capacity of 85.3mAhg−1 at 30th cycle, with more than 70% of its original capacity. The enhanced electrochemical property can be attributed to the small primary particle size, high specific surface area and carbon coating effect. The current study suggests that the as-prepared Na2MnPO4F/C material shows promising electrochemical performance in Na-ion battery.

Interaction between Human Serum Albumin and Different Anatase TiO2 Nanoparticles: A Nano-bio Interface Study

In this investigation, differently shaped and surface functionalized TiO2 anatase nanoparticles and human serum albumin (HSA) were selected to study protein-nanoparticles interaction both in a solution and on flat surfaces, thereby mimicking a medical device. Anatase nanocrystals were characterized by transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) surface analysis and dynamic light scattering (DLS). The protein-nanoparticles' interactions and their eventual reversibility were studied by pH dependent ζ- potential measurements in different media: ultra-pure water, a phosphate buffer simulating physiological conditions and in a culture medium supplemented with foetal bovine serum. The protein corona masking effect was evidenced and the interaction HSA-nanocrystals resulted irreversible. The interaction HSA-silicon supported TiO2 nanocrystals films was studied by atomic force microscopy (AFM), and resulted driven by the substrate hydrophilicity degree plus was different for the diverse range of nanocrystals tested. Surface roughness measurements showed that on some of the nanocrystals, HSA were arranged in a more globular manner. A lower protein affinity was found for nanocrystals that had a smaller primary particle size, which may correspond to their higher biocompatibility. This nano-bio interface research aimed to study the HSA protein-TiO2 anatase nanocrystals under conditions similar to those for in vitro and in vivo toxicity analyses.