Formation Of Pd Nanoparticles Research Articles

High N2-selectivity of nitrite reduction by palladium-laden nanocomposite with self-sufficient electron donators

Selectively reducing nitrite to gaseous nitrogen (N2) with an effective and recyclable fashion stands as an attractive alternative for treating the relevant wastewater. Herein, a Pd-based nanocomposite (Pd@EDA-CMPS) was subtly assembled by encapsulating Pd(0) nanoparticles into a porous polystyrene carrier, which was aforehand functionalized with ethylenediamine (EDA) as the endogenous electron donator. Systematical macroscopic experiments confirm that the pre-grafted EDA groups can substantially stimulate the catalytic activity of the laden Pd(0) nanoparticles with high removal efficiency and N2 selectivity of Pd@EDA-CMPS toward nitrite; specifically, high N2 selectivity (86%) was achieved by Pd@EDA-CMPS with an excellent anti-interference ability against competing anion and a broad pH-range applicability (4–11), whereas no N2 production was detected for its counterparts (CMPS, EDA-CMPS, and Pd@CMPS). Spectroscopic analyses reveal that the grafted EDA groups played a decisive role in the formation of H-loaded Pd(0) nanoparticles inside the porous substrate, which joint with the unique pH-buffering ability of EDA drove the reaction to the production of nitrogen (N2) rather than ammonia (NH3). The exhausted Pd@EDA-CMPS can be promisingly regenerated by NaOH (eluting) and NaBH4 (restoring) solution without obvious loss in treatment capacity and N2 selectivity. This work provides a feasible strategy for catalytically reducing nitrite into N2 without the provision of exogenous reductor such as hydrogen.

Spontaneously decorated palladium nanoparticles on redox active covalent organic framework for chemiresistive hydrogen gas sensing

A rapid hydrogen (H2) sensor operating at room temperature is fabricated using covalent organic framework (COF), namely Pyromellitic dianhydride and tris(4-aminophenyl)amine (PMDA-TAPA), PT COF that has a unique ability to spontaneously reduce Pd2+ into Pd0 nanoparticles without the aid of external reducing agents. The presence of surface redox sites in COF enable the rapid formation of Pd nanoparticles on COF surface under ambient conditions. The generated material, hitherto named as Pd@amicPT portrayed remarkable H2 sensing characteristics with a rare combination of high response % (67.3 ± 1) and rapid response/recovery times (5.3/3.5 s, respectively) for 1 % H2 under ambient conditions. Our results demonstrated appreciable reproducibility, repeatability, and long term stability of sensor that remained unaffected by relative humidity and a high selectivity towards H2. Further, sensor performance is found to be superior when compared to many Pd loaded 2D material based chemiresistive H2 gas sensors.

Photocatalytic activity enhancement of two-step and one-pot synthesis of Pd/ZnO nanocomposites: an experimental and DFT study.

Pd/ZnO nanocomposites were successfully synthesized by means of one and two pot synthesis and applied in the photodegradation of Rh6G. The nanocomposites were characterized by XRD, SEM, TEM, FTIR and micro-Raman spectroscopies. It was found the presence of PdZn2, PdO and agglomerated particles in the support surface for the Palladium-based nanocomposites fabricated by one-pot route; the two-step method allowed the formation of spherical Pd nanoparticles, with homogeneous distribution in the nanocomposite matrix, with an average size of 2.16nm. The results show higher photocatalytic efficiency for the samples fabricated under the two-step approach compared to the one-pot synthesis. Based on experimental results, density functional theory (DFT) calculations were carried out to understand the enhancement photocatalytic of Pd/ZnO nanocomposites. To achieve it, the ZnO (001) and (101) surfaces were built and decorated by different Pd coverages. The theoretical results indicated two different photocatalytic mechanisms. In ZnO (001) case, the electrons flowed from surface to Pd, generating the superoxide radical anion (⋅O2-). Furthermore, the density of states of the ZnO (001) surface was modified by impurity Pd-d states at proximity to the conduction states, which may work as electron acceptors states. On the other hand, we found that the electrons flow from Pd to ZnO (101) surface, inducing the formation of ⋅OH and ⋅O2- for the degradation of Rh6G. The density of states of the ZnO (101) revealed a reduction in its bandgap, due to Pd-d states localized above valence states. Hence, our theoretical results suggest that the Pd-d states may facilitate the mobility of electrons and holes in (001) and (101) surfaces, respectively, reducing the rate of charge recombination.

Hydrogenation of cyclohexene over single-atom Pt or Pd incorporated porous ceria nanoparticles under solvent-free conditions.

In order to maximize the utilization of noble metals in catalysis, single atom of palladium (Pd) and platinum (Pt) were incorporated individually in the framework of porous ceria (CeO2) by using a one-step flash combustion method. Samples with different Pd and Pt loading (0.5, 1, 2.5, and 5 wt%) were prepared and examined by using different analysis techniques such as XRD, ICP, N2 sorption measurements, SEM, HR-TEM, and XPS. The characterization data confirms the formation of zero-state single-atom Pt and Pd (with possible formation of Pd nanoparticles with a size less than 5 nm) incorporated onto the three-dimensional porous ceria structure. The catalytic activity of the synthesized materials was studied in the cyclohexene reduction to cyclohexane at 393 K and 3 atm of pure hydrogen (H2) gas as a model reaction. The obtained results demonstrated that the conversion percentage of cyclohexene is increasing with Pd or Pt loading. The best cyclohexene conversion, 21% and 29%, was achieved over the sample that contains 5 wt% of Pt and Pd, respectively. The collected catalytic data fit the zero-order reaction model, and the rate constant of each catalyst was determined. The catalytic experiments of the most-performed catalysts were repeated five times and the obtained loss in activity was insignificant.

A Novel Strategy for the Preparation of Supported Pd as an Efficient Catalyst for the Hydrogenation of Nitrobenzene in Mild Conditions

An advanced strategy was developed for the synthesis of molecular sieve-supported Pd catalysts. In this method, reductant containing C=C was in-situ prepared and pre-dispersed in the pore of the zeolites. The C=C group in the reductant can reduce the Pd2+ to Pd0 efficiently, leading to the formation of small and uniform Pd nanoparticles (~2 nm). The physical and chemical properties of the catalyst were characterized by XRD, TEM, XPS (ICP-OES), N2 isothermal adsorption-desorption, and H2-TPR. These catalysts showed high catalytic performance for the hydrogenation of nitrobenzene to aniline. All the TOFs for 1.5 Pd/Y, 1.5 Pd/ZSM-5, and 1.5 Pd/MOR with 1.5 wt% Pd loading are higher than 1000 h−1 at 30 °C and 0.1 MPa H2. Meanwhile, kinetic analysis for 2.0 Pd/Y was carried out, and an apparent activation energy of 28.88 kJ mol−1 was obtained, which is lower than most of the reported values in the literature. Furthermore, these catalysts were stable and recyclable.

Selective C–H activation of unprotected allylamines by control of catalyst speciation

An outstanding challenge in the Pd-catalyzed functionalization of allylamines is the control of stereochemistry. Terminal alkenes preferentially undergo Heck-type reactions, while internal alkenes may undergo a mixture of Heck and C-H activation reactions that give mixtures of stereochemical products. In the case of unprotected allylamines, the challenge in achieving C-H activation is that facile in situ formation of Pd nanoparticles leads to preferential formation of trans rather than cis-substituted products. In this study we have demonstrated the feasibility of using mono-protected amino acid (MPAA) ligands as metal protecting groups to prevent aggregation and reduction, allowing the selective synthesis of free cis-arylated allylamines. This method complements Heck-selective methods, allowing complete stereochemical control over the synthesis of cinnamylamines, an important class of amine that can serve as therapeutics directly or as advanced intermediates. To highlight the utility of the methodology, we have demonstrated rapid access to mu opioid receptor ligands.

An In Situ Fabricated Hydrogel Polymer - Palladium Nanocomposite Electrocatalyst for the HER: Critical Role of the Polymer in Realizing High Efficiency and Stability.

Development of general and simple designs of catalytic electrodes for the hydrogen evolution reaction (HER) is critical. The present work demonstrates the multiple roles played by a hydrogel polymer in the fabrication and activity enhancement of the nanoelectrocatalyst. A nanocomposite thin film of Pd with the insulating hydrogel, poly(2-hydroxyethyl methacrylate) (PHEMA), is fabricated through a facile in situ process, the polymer itself functioning as the reducing/stabilizing agent in the formation of Pd nanoparticles. Pd-PHEMA on Ni foam enables efficient HER in alkaline medium with a low overpotential; the polymer enables the electrocatalysis by its swelling and confinement of the electrolyte. Most significantly, when the electrode is subjected to an optimized cycling protocol, the overpotential decreases steadily, reaching an impressively low value of 36 mV (@10 mA cm-2 ). A low Tafel slope (68 mV dec-1 ), high exchange current density, Faradaic efficiency and TOF (3.27 mA cm-2 , 99 %, 122.7 h-1 ), and extended stability are achieved. Detailed investigations reveal the active role of the polymer in the evolution of the nanocatalyst, itself undergoing favorable morphological changes. The study illustrates the widened scope for developing efficient and stable catalytic electrodes with hydrogel polymers and unique features that promote the generation of green hydrogen.

Polysaccharide-Stabilized PdAg Nanocatalysts for Hydrogenation of 2-Hexyn-1-ol

We used a new one-pot green technique to prepare polysaccharide-based Pd and PdAg nanocatalysts. Catalysts were obtained using a sequentially supporting natural polymer (2-hydroxyethyl cellulose (HEC), chitosan (Chit), pectin (Pec)) and metals on zinc oxide. Nanocatalysts based on a polysaccharide were studied using various physicochemical methods (IR spectroscopy, transmission electron microscopy, X-ray powder diffraction, etc.). The catalyst characterization results indicated the complete adsorption of polysaccharides and metal ions onto the inorganic support (ZnO). We demonstrated the formation of polysaccharide-stabilized Pd nanoparticles with a size of ~2 nm. Metal nanoparticles were uniformly located on the surface of polysaccharide-modified zinc oxide. The synthesized catalysts were tested using liquid-phase hydrogenation of 2-hexyn-1-ol under mild conditions (0.1 MPa, 40 °C). Close conversion values of 2-hexyn1-ol were obtained for all the developed catalysts. The selectivity for cis-hexen-1-ol of the polysaccharide-based PdAg nanocatalysts varied as follows: PdAg-HEC/ZnO > PdAg-Pec/ZnO > PdAg-Chit/ZnO. A similar correlation was obtained in the presence of monometallic Pd-polysaccharide/ZnO catalysts. We determined the optimum reaction temperature and catalyst loading for PdAg catalysts modified using HEC and Chit (40 °C, 0.05 g).

Highly Functionalized SWCNTs with a Dopamine Derivative as a Support for Pd Nanoparticles: A Recyclable Catalyst for the Reduction of Nitro Compounds and the Heck Reaction.

Single-walled carbon nanotubes (SWCNTs) were functionalized with a dopamine derivative in which the amine group was converted to azide (dopamine azide). The direct reaction of SWCNTs and dopamine azide in o-dichlorobenzene at high temperature (160 °C) led to very highly functionalized CNTs (≈60 wt%). Surprisingly, despite this high degree of functionalization, Raman spectroscopy detected a low disruption of the π-network of the carbonaceous support. This finding was justified by the rehybridization from sp3 to sp2 of the sidewall carbon atoms of CNTs involved in the functionalization process. Further characterization by means of different techniques such as X-ray photoelectron spectroscopy (XPS) analysis and transmission electron microscopy (TEM) allowed to shed some light on the chemical composition and morphology of the obtained material. Moreover, the estimation of the total content of phenolic units and their reducing potential after CNTs functionalization was also assessed using Folin and Ciocalteu and 2,2-diphenyl-1-picryl hydrazide (DPPH) assays. The functionalization of CNTs was exploited to immobilize palladium(II) species that were subsequently reduced with NaBH4 leading to the formation of Pd nanoparticles (NPs). The so obtained hybrid material was used as a recyclable heterogeneous catalyst for the reduction of nitro compounds and the Heck reaction.

Microwave-Assisted Synthesis of Pd Nanoparticles into Wood Block (Pd@wood) as Efficient Catalyst for 4-Nitrophenol and Cr(VI) Reduction.

Palladium (Pd) nanoparticle catalysis has attracted increasing attention due to its efficient catalytic activity and its wide application in environmental protection and chemical synthesis. In this work, Pd nanoparticles (about 71 nm) were synthesized in aqueous solution by microwave-assisted thermal synthesis and immobilized in beech wood blocks as Pd@wood catalysts. The wood blocks were first hydrothermally treated with 10% NaOH solution to improve the internal structure and increase their porosity, thereby providing favorable attachment sites for the formed Pd nanoparticles. The stable deposition of Pd nanoparticle clusters on the internal channels of the wood blocks can be clearly observed. In addition, the catalytic performance of the prepared Pd@wood was investigated through two model reactions: the reduction of 4-nitrophenol and Cr(VI). The Pd@wood catalyst showed 95.4 g-1 s-1 M-1 of normalized rate constant knorm and 2.03 min-1 of the TOF, respectively. Furthermore, Pd nanoparticles are integrated into the internal structure of wood blocks by microwave-assisted thermal synthesis, which is an effective method for wood functionalization. It benefits metal nanoparticle catalysis in the synthesis of fine chemicals as well as in industrial wastewater treatment.

Self-reduction synthesis of supported ultrafine Pd nanoparticles with high activity and stability in hydrogenation

Supported ultrafine metal nanoparticles display outstanding catalytic performance in heterogeneous catalysis. Nevertheless, there are limited convenient and practical approaches for synthesizing supported ultrafine metal nanoparticle catalysts, despite the development of advanced fabrication methods. High-temperature reduction is often required for the preparation of metal catalysts for catalytic hydrogenation. However, the use of reductants, such as H2, easily leads to the aggregation of nanoparticles during catalyst preparation. In this work, we developed an effective self-reduction strategy using Pd precursors with organic ligands to prepare supported ultrafine Pd catalysts. Simple calcination under an inert atmosphere leads to the formation of uniform and ultrafine Pd nanoparticles (∼1 nm). These Pd precursors were reduced following the reaction between the −CHx groups on ligands and surface hydroxyl species on oxide supports. CO and oxygen vacancies generated in situ both contributed to the stabilization of ultrafine Pd nanoparticles. The as-prepared ultrafine Pd nanoparticles were highly stable even after the high-temperature treatment at 600°C. The catalysts displayed a turnover frequency as high as 26,910 h−1 for styrene hydrogenation and maintained the catalytic activity for at least 5 test cycles.

Novel hydrazine hydrate sensor based on”fish-bait” capture mode

ABSTRACT Coordination reaction is a usual way for the concentration of metal ions in aqueous solution. In this work, 5-(5-iodine-2-pyridine azo)-2,2 amie toluene (5-PADAT) was firstly casting onto carbon glass electrode (GCE), play a role of ‘bait’; then, immersed 5-PADAT modified GCE into immersed aqueous solution containing order of magnitude ppm Palladium ions (Pd2+, play a role of ‘fishes’); ‘Fishes’ were captured by ‘bait’ with the reaction process of 5-PADAT and Pd2+, leading to the concentration of Pd2+ onto the GCE; Cyclic voltammetry was employed to reduce Pd2+ in situ, formed Pd nanoparticles (PdNPs) modified GCE. It can be used to detect the oxidation of hydrazine hydrate at a very low potential, 0.1 V.

Nonclassical Nucleation and Growth of Pd Nanocrystals from Aqueous Solution Studied by In Situ Liquid Transmission Electron Microscopy

Direct visualization and understanding of the atomic mechanisms governing the growth of nanomaterials are crucial for designing synthesis strategies of high specificity. Aside from playing a key role in numerous technological applications, palladium clusters and nanoparticles are particularly valuable due to their outstanding catalytic activity. Studies show that the properties of Pd nanomaterials depend on shape and size. Therefore, optimizing the synthesis to control the final size and shape of Pd nanoparticles is important for a large number of current and future applications. In this work, we exploit in situ liquid cell scanning transmission electron microscopy to track at the atomic scale the growth of Pd nanoparticles from the very early stage to mature, crystalline nanoparticles. We find that the formation of Pd nanoparticles consists of multiple steps. The first step in nanoparticle formation, representing a nonclassical nucleation step, can be described by the formation of agglomerates of Pd atoms. In the second step, these agglomerates grow via atomic addition to form primary nanoclusters, which coalesce to form amorphous clusters. In the third stage, these clusters continue to coalesce, leading to the formation of amorphous Pd NPs, while in parallel, growth by monomer attachment continues. Then, in the fourth step, the amorphous nanoparticles undergo a nanocrystallization process, where the continuous improvement of crystallinity and the establishment of a distinct morphology eventually give rise to the formation of facetted, crystalline nanoparticles. Similar to our earlier work with Au and Pt nanoparticles, these results confirm that even for simple systems, nonclassical nucleation and growth processes dominate and that these multi-step mechanisms are highly element-specific. Despite the fact that the synthesis conditions are identical, the element-specific interactions define the pathway of the formation of crystalline nanoparticles.

Solvated electron-induced synthesis of cyclodextrin-coated Pd nanoparticles: mechanistic, catalytic, and anticancer studies.

Herein, using in situ generated solvated electrons in the reaction media, a highly time-efficient, one-pot green approach has been employed to synthesize palladium (Pd) nanoparticles (NPs) coated with a molecular assembly of α-cyclodextrin (α-CD). The appearance of a shoulder peak at 280 nm in the UV-Vis absorption spectra indicated the formation of Pd NPs, which was further confirmed from their cubic phase XRD pattern. The nanomorphology varied considerably as a function of the dose rate, wherein sphere-shaped NPs (average size ∼ 7.6 nm) were formed in the case of high dose rate electron-beam assisted synthesis, while nanoflakes self-assembled to form nanoflower-shaped morphologies in a γ-ray mediated approach involving a low dose rate. The formation kinetics of NPs was investigated by pulse radiolysis which revealed the formation of Pd-based transients by the solvated electron-induced reaction. Importantly, no interference of α-CD was observed in the kinetics of the transient species, rather it played the role of a morphology directing agent in addition to a biocompatible stabilizing agent. The catalytic studies revealed that the morphology of the NPs has a significant effect on the reduction efficiency of 4-nitrophenol to 4-aminophenol. Another important highlight of this work is the demonstration of the morphology-dependent anticancer efficacy of Pd NPs against lung and brain cancer cells. Notably, flower-shaped Pd NPs exhibited significantly higher cancer cell killing as compared to spherical NPs, while being less toxic towards normal lung fibroblasts. Nonetheless, these findings show the promising potential of Pd NPs in anticancer treatment.

Temperature-induced formation of Pd nanoparticles in heterogeneous nanobiohybrids: application in C-H activation catalysis.

The effect of the temperature in the synthesis of Pd nanoparticles in the metal-enzyme biohybrids is evaluated. The effect on the formation, size, and morphology of nanoparticles was evaluated using C. antarctica B lipase as the protein scaffold. XRD analyses confirmed the formation of crystalline Pd(0) as the metal species in all cases. TEM analyses revealed spherical crystalline nanoparticles with average diameter size from 2 nm at 4 °C synthesis to 10 nm obtained at 50 °C synthesis. The thermal phenomenon was also critical in the final hybrid formation using more complex enzymes, where the relation of the protein structure and temperature and the influence of the latter has been demonstrated to be critical in the reducing efficiency of the enzyme in the final Pd nanoparticle formation, in the metal species, or even in the final size of the nanoparticles. Different Pd biohybrids were evaluated as catalysts in the C-H activation of protected l-tryptophan under mild conditions. Pd@CALB4 showed the best results, with >99% conversion for C-2 arylation in methanol at room temperature with a TOF value of 64 min-1, being 2 or 4 times higher than that of the other synthesized hybrids. This catalyst showed a very high stability and recyclability, maintaining >95% activity after three cycles of use.

Boosted H2O2 Productivity by Sulfur-Doped Pd/Carbon Catalysts via Direct Synthesis from H2 and O2 at Atmospheric Pressure

It remains a challenge nowadays in the development of highly efficient catalysts for the direct synthesis of H2O2 from H2 and O2. In this work, we developed sulfur-doped carbon-supported Pd catalysts and systematically investigated sulfur effects on catalytic performances through various characterizations (transmission electron microscopy (TEM), N2 adsorption–desorption, H2-temperature-programmed reduction (TPR)/temperature-programmed desorption (TPD), X-ray photoelectron spectroscopy (XPS), etc.). Results showed that sulfur species promoted the in situ formation of Pd nanoparticles and enhanced their dispersion on the supports. Due to the synergistic combination of active metal and support, the catalytic performance has been improved significantly in the direct synthesis of H2O2. The catalyst doped with the highest sulfur content showed the highest H2O2 productivity of 7148 mmol gPd–1 h–1, which was nearly 4 times higher than the catalyst without sulfur doping.

The evolution of single-site Pd1/AC catalyst during the process of acetylene dialkoxycarbonylation

The stability of heterogeneous single-metal-site catalysts (HSMSCs) is always a challenging issue. Deactivation of HSMSCs often occurred and draw much intention. The investigation of the single-metal-site evolution during the deactivation process is great significance to maintain the stability of HSMSCs. Herein, a fundamental understanding of the deactivation process of an initially efficient single-Pd-site catalyst (Pd1/AC) for acetylene dialkoxycarbonylation was revealed from geometrical and electronic point of view via a series of characterizations. Synergistic effect of O2 and iodine ligands contributed to the stability of Pd1/AC catalyst to some extent. The valence of single Pd ions gradually changed from [Pdδ+] to [Pd0], leading to the formation of Pd nanoparticles (Pd black). In addition, the blockage of support microspores also worsened the deactivation of Pd1/AC.

Pd Supported on Pr-Rich Cerium–Zirconium–Praseodymium Mixed Oxides for Propane and CO Oxidation

The activity of emission control catalysts must be improved in urban mode at low temperatures. One possible way is to tailor the metal-support interaction between platinum group metals (PGMs) and ceria to stabilize small clusters or single atoms, optimizing the utilization of costly PGMs. In this study, a small loading of Pd (<0.2 wt.%) was dispersed on Pr-rich cerium–zirconium–praseodymium mixed oxides (CZP45: Ce0.45Zr0.10Pr0.45O2−x). After the initial calcination at 800 °C, Pd was mainly in the form of dispersed isolated cations which were found to be efficient for low-temperature CO oxidation but inactive for propane combustion. Nevertheless, a pre-reduction step can trigger the formation of Pd nanoparticles and promote the propane oxidation. Pd nanoparticles, formed during the reduction step, coupled with the high oxygen mobility of CZP45, lead to outstanding catalytic activity for propane oxidation starting from 250 °C. However, the re-oxidation of Pd nanoparticles and their partial re-dispersion, promoted by the fast oxygen mobility of the mixed oxide, rapidly deactivate the catalysts in lean conditions.

Enhanced Hydrogen Permeability of Mixed Protonic–Electronic Conducting Membranes through an In‐Situ Exsolution Strategy

AbstractMixed protonic–electronic conducting (MPEC) ceramic membranes with high H2 permeability and stability are significant for practical H2 separation. CO2‐tolerant lanthanum tungstate oxides have received much attention, but their low H2 permeability is their main problem for membrane applications. Herein, an efficient in‐situ exsolution strategy is proposed to enhance the H2 permeability and CO2 stability of lanthanum tungstate‐type membranes. During H2 permeation, the catalytic Pd nanoparticles are in‐situ generated from the bulk oxide lattices and dispersed evenly on the membrane surfaces, which greatly promotes the H2 surface exchange kinetics. Also, the protonic conductivity of the membranes is effectively improved through the introduction of Pd. Consequently, the H2 permeation flux is increased by 3.5 times and a maximum H2 flux of 1.3 mL min−1 cm−2 is achieved at 1000 °C through the La5.5(W0.6Mo0.4)0.95Pd0.05O11.25‐δ (LWMPd) membrane. The LWMPd membrane shows outstanding long‐term chemical stability during 300 h continuous operation in a CO2‐containing atmosphere. Therefore, this in‐situ exsolution formation of Pd nanoparticles provides effective guidance for developing competitive MPEC membranes for H2 separation and purification.

CO Oxidation over Pd Catalyst Supported on Porous TiO2 Prepared by Plasma Electrolytic Oxidation (PEO) of a Ti Metallic Carrier.

A porous TiO2 layer was prepared with the plasma electrolytic oxidation (PEO) of Ti. In a further step, Pd was deposited on the TiO2 surface layer using the adsorption method. The activity of the Pd/TiO2/Ti catalyst was investigated during the oxidation of CO to CO2 in a mixture of air with 5% CO. The structure of the catalytic active layer was studied using a scanning electron microscope equipped with an energy dispersive spectrometer (SEM-EDS), time-of-flight secondary ion mass spectrometry (TOF-SIMS), inductively coupled plasma mass spectrometry (ICP-MS), and X-ray diffraction (XRD). The PEO process provided a porous TiO2 layer with a uniform thickness in the range of 5–10 µm, which is desirable for the production of Pd-supported catalysts. A TOF-SIMS analysis showed the formation of Pd nanoparticles after the adsorption treatment. The conversion of CO to CO2 in all samples was achieved at 150–280 °C, depending on the concentration of Pd. The composition of Pd/ TiO2/Ti was determined using ICP-MS. The optimum concentration of Pd on the surface of the catalyst was approximately 0.14% wt. This concentration was obtained when a 0.4% PdCl2 solution was used in the adsorption process. Increasing the concentration of PdCl2 did not lead to a further improvement in the activity of Pd/ TiO2/Ti.