Synthesis of glass–ceramics in the CaO–MgO–SiO2 system with B2O3, P2O5, Na2O and CaF2 additives

Glass–ceramics based on the CaO–MgO–SiO₂ system with limited amount of additives (B₂O₃, P₂O₅, Na₂O and CaF₂) were prepared. All the investigated compositions were melted at 1400 °C for 1 h and quenched in air or water to obtain transparent bulk or frit glass, respectively. Raman spectroscopy revealed that the main constituents of the glass network are the silicates Q¹ and Q² units. Scanning electron microscopy (SEM) analysis confirmed liquid–liquid phase separation and that the glasses are prone to surface crystallization. Glass–ceramics were produced via sintering and crystallization of glass-powder compacts made of milled glass-frit (mean particle size 11–15 μm). Densification started at 620–625 °C and was almost complete at 700 °C. Crystallization occurred at temperatures >700 °C. Highly dense and crystalline materials, predominantly composed of diopisde and wollastonite together with small amounts of akermanite and residual glassy phase, were obtained after heat treatment at 750 °C and 800 °C. The glass–ceramics prepared at 800 °C exhibited bending strength of 116–141 MPa, Vickers microhardness of 4.53–4.65 GPa and thermal expansion coefficient (100–500 °C) of 9.4–10.8 × 10⁻⁶ K⁻¹.     

Synthesis and photocatalysis of TiO2 hollow spheres by a facile template-implantation route

Process variables such as reaction temperature (55 to 90 °C), calcination temperature (450 to 750 °C), and concentration of TiCl₄ precursor (26 to 105 mM) have been examined in order to tailor the surface area, crystallite size, and the anatase/rutile ratio of the polycrystalline TiO₂ microcapsules prepared by a template-implantation route in heptane solvent. The hollow capsules are all non-aggregating with nanoporous shell structure. Among the process variables examined, the Brunauer–Emmett–Teller (BET) surface area and the anatase/rutile ratio are found critically dependent on the reaction temperature, in which a reduced reaction temperature (from 90 to 55 °C) leads to a higher BET value (from 8.4 to 36.4 m^?2 g^?1), a predominant anatase phase (weight fraction of the anatase phase increases from 0.20 to 0.84), and an improved photodegradation of aqueous methylene blue (MB) dye under UV exposure (the degradation rate increases from 0.5×10^?2 to 5.5×10^?2 min^?1).     

Supercritical hydrothermal synthesis of titanium dioxide nanostructures with controlled phase and morphology

A novel template- and organic-free synthesis of TiO₂ nanostructures with controlled phase and morphology was realized through batch supercritical hydrothermal treatment (400 °C) of titanate nanotubes (TNTs) with H₂O₂ in NaOH aqueous solution. Well-defined 3D titanate hierarchical spheres (THSs), 2D multilayered titanate nanosheets (TNSs), and 1D monodisperse anatase nanorods (ANRs) exposing (0 1 0) facets were prepared in 15 min by slightly varying the NaOH solution pH. Specifically, the obtained Na/H-THSs (without/with HCl neutralization) exhibited highly porous structures with large specific surface area (109 m² g⁻¹ and 196 m² g⁻¹, respectively). Temperature-dependent phase and morphology evolutions of products under subcritical condition (200 and 300 °C) were investigated. The formation of the TiO₂ nanostructures from TNTs was proposed mainly following a dissolution–nucleation-growth mechanism, suggesting that both supercritical temperature and NaOH solution pH were determinant factors governing the nucleation and growth process and thus the phase and morphology.     

Flame-made MoO3/SiO2–Al2O3 metathesis catalysts with highly dispersed and highly active molybdate species

MoO₃/SiO₂–Al₂O₃ catalysts are prepared via flame spray pyrolysis and evaluated in the self-metathesis of propene to ethene and butene. Their specific surface area ranges between 100 and 170 m² g^?1 depending on the MoO₃ loading (1–15 wt.%, corresponding to Mo surface density between 0.3 and 6.1 Mo atoms per nm²). The catalysts were characterized by N₂-physisorption, X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and time of flight secondary ion mass spectroscopy (ToF-SIMS). The silica–alumina matrix condenses first in the flame and forms non-porous spherical particles of 5–20 nm, followed by the dispersion of Mo oxide at their surface. Depending on the MoO₃ loading, different MoO_x species are stabilized: dispersed and amorphous molybdates (mono- and oligomeric) at low loadings (<5 wt.%, <1.5 Mo nm^?2) and crystalline MoO₃ species at higher loadings. Raman spectroscopy suggests the presence of monomeric species for surface densities of 0.3, 0.5 and 0.8 Mo nm^?2. The formation of MoOMo bonds is, however, clearly established by ToF-SIMS from surface densities as low as 0.5 Mo nm^?2. At 1.5 Mo nm^?2, crystallites of β-MoO₃ (2–3 nm) are detected and further increasing the loading induces the formation of bigger α- and β-MoO₃ crystals (around 20 nm). The speciation of Mo proves to have a marked impact on the metathesis activity of the catalysts. Catalysts with high Mo loading and exhibiting MoO₃ crystals are poorly active, whereas catalysts with low Mo loading (<5 wt.%) perform well in the reaction. The catalyst loaded with only 1 wt.% of MoO₃ (0.3 Mo nm^?2) is the most active, reaching turn over frequencies seven times higher than reference catalysts reported in the literature. Moreover, the specific metathesis activity is clearly inversely correlated to the degree of condensation of the molybdenum oxide phase (as evaluated by ToF-SIMS). The latter finding indicates that monomeric MoO_x species are the main active centres in the olefin metathesis.     

Thermally stable ceria–zirconia catalysts for soot oxidation by O2

Ce–Zr mixed oxides calcined at 1000 °C are more active catalysts for soot oxidation than pure CeO₂ calcined at the same temperature, both in loose and tight contact between soot and catalyst. 1000 °C sinterised-CeO₂ presents a very low surface area (2 m²/g), a large crystal size (110 nm) and a lack of surface redox properties. Ce–Zr mixed oxides present higher BET surface areas (typically 17–19 m²/g), smaller crystal sizes and enhanced redox properties. The Zr molar fraction does not affect appreciably the catalytic activity of Ce–Zr mixed oxides in the range studied (Zr molar fraction from 0.11 to 0.51).     

Effect of post-sintering heat-treatment on thermal and mechanical properties of Si3N4 ceramics sintered with different additives

To improve the thermal conductivity of Si₃N₄ ceramics, elimination of grain-boundary glassy phase by post-sintering heat-treatment was examined. Si₃N₄ ceramics containing SiO₂–MgO–Y₂O₃-additives were sintered at 2123 K for 2 h under a nitrogen gas pressure of 1.0 MPa. After sintering, the SiO₂ and MgO could be eliminated from the ceramics by vaporization during post-sintering heat-treatment at 2223 K for 8 h under a nitrogen gas pressure of 1.0 MPa. Thermal conductivity of 3 mass% SiO₂, 3 mass% MgO and 1 mass% Y₂O₃-added Si₃N₄ ceramics increases from 44 to 89 Wm⁻¹ K⁻¹ by the decrease in glassy phase and lattice oxygen after the heat-treatment. Relatively higher fracture toughness (3.8 MPa m^1/2) and bending strength (675 MPa) with high hardness (19.2 GPa) after the heat-treatment were achieved in this specimen. Effects of heat-treatment on microstructure and chemical composition were also observed, and compared with those of Y₂O₃–SiO₂-added and Y₂O₃–Al₂O₃-added Si₃N₄ ceramics.     

Mild hydrothermal formation and comparative coprecipitation route for EuTiNbO6 fine phosphor

Aeschynite-type EuTiNbO₆ fine phosphor with sufficient luminescence intensity was directly formed as homogeneous cuboid particles with high crystallinity in the range of 1–2 μm from precursor solution mixtures of EuCl₃, TiOSO₄, and NbCl₅ under weakly basic conditions via hydrothermal treatment at 240 °C for 5 h. The as-prepared aeschynite phase stably existed after heating at 1000–1400 °C for 1 h in air. Under excitation at wavelengths of 395 nm, among all samples before and after heating in air, the as-prepared EuTiNbO₆ fine crystals before heating emitted luminescence with the highest intensity in the red spectral region with strong red and weak orange light corresponding to ⁵D_0→⁷F₂ and ⁵D_0→⁷F₁ transitions of Eu³⁺, respectively. The amorphous coprecipitation powder crystallized into euxenite-type phase at 700–1000 °C and transformed into aeschynite-type phase at 1000–1200 °C. High-temperature heating at 1400 °C was essential for the coprecipitation powder to obtain almost a single phase of aeschynite-type EuTiNbO₆ and sufficient emission intensity.     

Development of electrochemical cell with layered composite of the Gd-doped ceria/electronic conductor system for generation of H2–CO fuel through oxidation–reduction of CH4–CO2 mixed gases

This paper shows the recent results on the development of layered composite promoting two types of electrochemical reactions (oxidation and reduction) in one cell. This cell consisted of porous Ni–Gd-doped (GDC) ceria cathode/thin porous GDC electrolyte (50 μm)/porous SrRuO₃–GDC anode. The external electric current was flowed in this cell at the electric field strength of 1.25 and 6.25 V/cm. The mixed gases of CH₄ (30–70%) and CO₂ (70–30%) were fed at the rate of 50 ml/min to the cell heated at 400–800 °C under the electric field. In the cathode, CO₂ was reduced to CO (CO₂ + 2e^? → CO + O^2?) and the formed CO and O^2? ions were transported to the anode through the pores and surface and interior of grains of GDC film. On the other hand, CH₄ was oxidized in the anode to form CO and H₂ through the reaction with diffusing O^2? ions (CH₄ + O^2? → CO + 2H₂ + 2e^?). As a result, H₂–CO mixed fuel was produced from the CH₄–CO₂ mixed gases (CH₄ + CO₂ → 2H₂ + 2CO). This electrochemical reaction proceeded completely at 800 °C and no blockage of gases was measured for long time (>10 h). Only H₂–CO fuel was generated in the wide gas compositions of starting CH₄–CO₂ gases.     

Studies on obtaining of aluminium ammonium calcium phosphates

Aluminium ammonium calcium phosphates were prepared with the use of AlCl₃, CaCO₃, H₃PO₄. The influence of the process parameters (pH 5 ± 3, the molar ratios of Ca²⁺:Al⁺³:PO₄^?3 in the substrates, respectively 0.31:0.62:1; 0.5:0.5:1; 0.72:0.36:1, temperature 40 ± 20 °C) on the phase composition and the product properties was determined. The process parameters that enable to obtain the material with expected physicochemical properties were determined based on the statistical evaluation of the experiments (fractional factorial design at three levels 3^(k?p)27). The phase composition of the obtained samples was studied with the use of XRD analysis. The specific surface area was calculated with the use of S_BET method and the particle size was determined by the laser scanning microscopy. The materials with the molar ratio of Al³⁺/NH₄⁺ and Al³⁺/Ca²⁺ in the range of 0.70–27.93 and 0.47–24.48, respectively, with an absorption oil number of 95–157 g/100 g paraffin oil, the S_BET within 25–118 m²/g, the pore volume within 0.14–0.74 cm³/g and the particle size in the range of 168–285 nm were obtained.     

High resolution electron energy loss spectroscopy of hydrogenated polycrystalline diamond: Assignment of peaks through modifications induced by isotopic exchange

In this work we unambiguously determine the origin of the different peaks which appear in the High Resolution Electron Energy Loss Spectrum (HREELS) of hydrogenated polycrystalline diamond films for an incident electron energy of 5 eV and loss energies extending to 700 meV. High quality diamond films deposited by hot filament chemical vapor deposition from various isotopic gas mixtures: ¹²CH₄ + H₂, ¹²CD₄ + D₂, ¹²CH₄ + D₂, ¹²CD₄ + D₂, ¹³CH₄ + H₂ were characterized. The different vibrational modes, fundamentals and overtones, were directly identified through the modifications of the HREEL spectra induced by the isotopic exchange of H by D and ¹²C by ¹³C Three types of peaks were identified: (1) pure C–C related peaks (a diamond optical phonon at ∼ 155 meV and its overtones at 300, 450 and 600 meV), (2) pure C–H related peaks (C–H bend at ∼ 150 meV and C–H stretch of sp³ carbon at 360 meV), (3) coupling of C–H and C–C peaks (510 meV peak due to coupling of the C–H stretch at 360 meV with either the C–C stretch or the C–H bend at ∼ 155 meV). The overtones at 300, 450 and 600 meV (associated with electron scattering at diamond optical phonons) indicate a well defined hydrogenated diamond surface since they are absent in the HREEL spectrum of low energy ion beam damaged diamond surface.     

Densification and mechanical properties of cBN–TiN–TiB2 composites prepared by spark plasma sintering of SiO2-coated cBN powder

cBN–TiN–TiB₂ composites were fabricated by spark plasma sintering at 1773–1973 K using cubic boron nitride (cBN) and SiO₂-coated cBN (cBN(SiO₂)) powders. The effect of SiO₂ coating, cBN content and sintering temperature on the phase composition, densification and mechanical properties of the composites was investigated. SiO₂ coating on cBN powder retarded the phase transformation of cBN in the composites up to 1873 K and facilitated viscous sintering that promoted the densification of the composites. Sintering at 1873 K, without the SiO₂ coating, caused the relative density and Vickers hardness of the composite to linearly decrease from 96.2% to 79.8% and from 25.3 to 4.4 GPa, respectively, whereas the cBN(SiO₂)–TiN–TiB₂ composites maintained high relative density (91.0–96.2%) and Vickers hardness (17.9–21.0 GPa) up to 50 vol% cBN. The cBN(SiO₂)–TiN–TiB₂ composites had high thermal conductivity (60 W m⁻¹ K⁻¹ at room temperature) comparable to the TiN–TiB₂ binary composite.     

Synergic effect of cation doping and phase composition on the photocatalytic performance of TiO2 under visible light

The synergic effect of cation doping and phase composition for the further improvement of the photocatalytic activity of TiO₂ under visible light is reported for the first time. Fe^3 + and Sn^4 + co-doped TiO₂ with optimized phase composition were synthesized through a simple soft-chemical solution method. The visible-light-driven photocatalytic activity of Fe^3 + and Sn^4 + co-doped TiO₂ was 5 times of that of Evonik P25 TiO₂ using degradation of methylene blue as model reaction. The synthesized photocatalysts were characterized by powder X-ray diffraction, UV–Vis diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, ¹¹⁹Sn Mössbauer spectroscopy, and X-ray absorption fine structure spectroscopy. It is indicated that Sn^4 + doping can facilitate the phase transition from anatase to rutile. The different ratios of anatase and rutile can be achieved by tuning the amount of Sn^4 + doped into the lattice. Furthermore, the doping of Sn^4 + into TiO₂ lattice can stabilize the phase composition when Fe^3 + is co-doped. In the Fe^3 + and Sn^4 + co-doped TiO₂, Sn^4 + is mainly used to tune and stabilize the phase composition of TiO₂ and Fe^3 + acts as a doping cation to narrow the band gap of TiO₂. Both band gap and phase composition of TiO₂ can be tuned effectively by the simultaneous introduction of Fe^3 + and Sn^4 +. The synergic effect of optimized phase composition (anatase/rutile = 25/75) and narrowed band gap should be the two main reasons for the promoted photocatalytic activity of TiO₂ under visible light.     

Synthesis of 2-D nanostructured BiVO4:Ag hybrid as an efficient electrode material for supercapacitors

2-D BiVO₄ nanosheets with monoclinic phase were synthesized at room temperature, and incorporated with Ag to form BiVO₄:Ag hybrid materials. The experiments demonstrated that doping Ag has largely increased the electrochemical performances of supercapacitor. Furthermore, the specific capacitance can reach up to 109 F g^–1 at 1 A g^–1 (the undoped one is of 27 F g^–1); energy density has enhanced to 15.2 Wh kg^–1 compared with the pristine one without Ag (3.8 Wh kg^–1). Therefore, doping Ag into bismuth-based compound provides us an alternative approach for the synthesis of 2-D nanostructured hybrid as an efficient electrode material for supercapacitors     

Fabrication and properties of ZrB2–SiC–BN machinable ceramics

ZrB₂–SiC–BN ceramics were fabricated by hot-pressing under argon at 1800 °C and 23 MPa pressure. The microstructure, mechanical and oxidation resistance properties of the composite were investigated. The flexural strength and fracture toughness of ZrB₂–SiC–BN (40 vol%ZrB₂–25 vol%SiC–35 vol%BN) composite were 378 MPa and 4.1 MPa m^1/2, respectively. The former increased by 34% and the latter decreased by 15% compared to those of the conventional ZrB₂–SiC (80 vol%ZrB₂–20 vol%SiC). Noticeably, the hardness decreased tremendously by about 67% and the machinability improved noticeably compared to the relative property of the ZrB₂–SiC ceramic. The anisothermal and isothermal oxidation behaviors of ZrB₂–SiC–BN composites from 1100 to 1500 °C in air atmosphere showed that the weight gain of the 80 vol%ZrB₂–20 vol%SiC and 43.1 vol%ZrB₂–26.9 vol%SiC–30 vol%BN composites after oxidation at 1500 °C for 5 h were 0.0714 and 0.0268 g/cm², respectively, which indicates that the addition of the BN enhances oxidation resistance of ZrB₂–SiC composite. The improved oxidation resistance is attributed to the formation of ample liquid borosilicate film below 1300 °C and a compact film of zirconium silicate above 1300 °C. The formed borosilicate and zirconium silicate on the surface of ZrB₂–SiC–BN ceramics act as an effective barriers for further diffusion of oxygen into the fresh interface of ZrB₂–SiC–BN.     

Temperature stability and high-Qf of low temperature firing Mg2SiO4–Li2TiO3 microwave dielectric ceramics

In this work, a series of low-temperature-firing (1−x)Mg₂SiO₄–xLi₂TiO₃–8 wt% LiF (x = 35–85 wt%) microwave dielectric ceramics was prepared through conventional solid state reaction. X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analyses showed that the Li₂TiO₃ phase was transformed into cubic phase LiTiO₂ phase and secondary phase Li₂TiSiO₅. Partial substitution of Mg²⁺ ions for Ti³⁺ ions or Li⁺Ti³⁺ ions increased the cell volume of the LiTiO₂ phase. The dense microstructures were obtained in low Li₂TiO₃ content (x ≤ 65 wt%) samples sintered at 900 °C, whereas the small quantity of pores presented in high Li₂TiO₃ content (x ≥ 75 wt%) samples sintered at 900 °C and low Li₂TiO₃ content (x = 45 wt%) sintered at 850 and 950 °C. Samples at x = 45 wt% under sintering at 900 °C for 4 h showed excellent microwave dielectric properties of ε_r = 10.7, high Q × f = 237,400 GHz and near-zero τ_f = − 3.0 ppm/°C. The ceramic also exhibited excellent chemical compatibility with Ag. Thus, the fabricated material could be a possible candidate for low temperature co-fired ceramic (LTCC) applications.     

Synthesis and characterization of magnetic polyHIPEs with humic acid surface modified magnetic iron oxide nanoparticles

Magnetic macroporous polymer monoliths have been prepared using styrene/divinylbenzene (S/DVB) high internal phase emulsions (HIPEs) as templates. Humic acid surface modified iron oxide magnetic nanoparticles (Fe₃O₄@HA) have been used to prepare magnetic emulsion templates. The effect of magnetic particle concentration has been investigated by changing the ratio of Fe₃O₄@HA nanoparticles in the continuous phase. Highly macroporous polymers with magnetic response were obtained by the removal of the internal phase after the curing of emulsions at 80 °C. Fe₃O₄@HA particles were characterized by XRD and FTIR. The porosity, pore morphology and magnetic properties of the macroporous polymers were characterized as a function of the Fe₃O₄@HA concentration by scanning electron microscopy (SEM), Brunauer–Emmet–Teller (BET) molecular adsorption method and vibrating sample magnetometry (VSM), respectively. BET and VSM measurements demonstrated that the specific surface area and the saturation magnetization of the polymer monoliths were changed according to the Fe₃O₄@HA concentration between 8.77–35.08 m² g^?1 and 0.63–11.79 emu g^?1, respectively. Resulting magnetic monoliths were tested on the adsorption of Hg(II) and atomic absorption spectroscopy (AAS) was used to calculate the adsorption capacities. The maximum adsorption capacity of the magnetic monoliths was calculated to be 20.44 mmol g^?1 at pH 4.     

Effect of pyrolysis temperature on the pore structure evolution of polysiloxane-derived ceramics

Homogeneous silicon oxycarbide (SiOC) ceramic powders were prepared by pyrolysis of cross-linked polysiloxane at different temperatures (1250–1500 °C) under vacuum. The effect of pyrolysis temperature on the pore structure evolution was investigated by means of N₂ adsorption, SEM, XRD, IR and element analysis (EA). Studies showed that predominate mesoporous ceramics with the average pore size in the range of 2–13 nm were obtained after pyrolysis in this temperature range. The pore structure transformation is strongly correlated with the thermolytic decomposition process of the used precursor, such as phase separation and carbothermal reduction. At relatively lower temperature (1250–1350 °C), the ceramics had a relative small specific surface areas (35 m²/g) owing to the low degree of carbothermal reduction. However, as the carbothermal degree had an obvious augment at relative higher temperature (1400–1450 °C), the specific surface areas and total pore volume increased and reached to the maximum of 66 m²/g and 0.214 cm³/g, respectively, and subsequently decreased rapidly after 1500 °C for the reason of partial sintering of the nano-sized SiC derived from polysiloxane.     

Microwave dielectric properties of Mn-doped BaO–(Nd0.7,Sm0.3)2O3–4TiO2 ceramic sintered in a reducing atmosphere

The effect of MnCO₃ doped from 0 to 55 mol% into BaO–(Nd_0.7Sm_0.3)₂O₃–4TiO₂ (BNST) sintered in a reducing atmosphere on the microstructure and electrical properties was studied. Mn³⁺ completely substituted into Ti⁴⁺-sites of BNST to form a solid solution, so there is no second phase until 42 mol% which is the maximum solubility. Mn (<42 mol%)-doped BNST sintered in a reducing atmosphere is in a semi-conducing state because the concentration of free electron is higher than that of the acceptors. On the other hand, when Mn content doped into BNST exceeds a critical value (>43 mol%), the second Mn-rich phase due to excess of Mn³⁺ substituted into Ti⁴⁺-site, corresponding to original BaO–(Nd_0.7Sm_0.3)₂O₃–4TiO₂ (1 1 4) phase, is formed. Mn (>43 mol%)-doped BNST sintered in a reducing atmosphere is in an insulating state because the concentration of the acceptors is higher than that of liberated free electron, so the insulation resistance becomes high and tan δ becomes low. The formation of the second Mn-rich phase affects Q × f factor and temperature coefficient of capacitance (T.C.C.) of BNST significantly.     

Spark plasma sintering of MgAl2O4–YCr0.5Mn0.5O3 composite NTC ceramics

New high temperature negative temperature coefficient (NTC) thermistor ceramics based on a xMgAl₂O₄–(1 − x)YCr_0.5Mn_0.5O₃ (x = 0.1, 0.4, 0.6) composite system have been successfully fabricated through spark plasma sintering (SPS) with a low sintering temperature and a short sintering period. The X-ray diffraction analysis indicates that the SPS-sintered composite ceramics consist of a cubic spinel MgAl₂O₄ phase and an orthorhombic perovskite YCr_0.5Mn_0.5O₃ phase isomorphic to YCrO₃. The SPS-sintered composite ceramics have high relative density ranging from 94.1 to 97.4% of the theoretical density. X-ray photoelectron spectroscopy analysis corroborates the presence of Cr³⁺, Cr⁴⁺, Mn³⁺, and Mn⁴⁺ ions on lattice sites, which may result in the hopping conduction. The obtained ρ₂₅, B_25–150, and B_700–1000 of the SPS-sintered composite NTC thermistors are in the range of 1.53 × 10⁶–9.92 × 10⁹ Ω cm, 3380–5172 K, and 7239–9543 K, respectively. These values can be tuned by adjusting the MgAl₂O₄ concentration.     

Facile preparation and unique H2 adsorption behavior of three-dimensional novel Pt–Ru hollow sphere assemblies

Three-dimensional long range ordered hollow Pt–Ru sphere assemblies were prepared using a sacrificial three-dimensionally ordered macroporous (3DOM) carbon template. Metallic salts, such as a mixture of RuCl₃ with H₂PtCl₆ were infiltrated into the carbon template, and a reduced Pt–Ru phase was produced on the surface of the 3DOM carbon template by a borohydride reduction reaction. The sacrificial template was then burnt off in air at 650 °C. The diameter of the hollow Pt–Ru spheres could be tailored using a different pore size 3DOM carbon template. Assemblies with an outer diameter of 550 nm showed high BET surface area of 584.3 m²/g. In addition, a high hydrogen adsorption stoichiometry (>0.5 H/M) was obtained on the Pt–Ru sphere assemblies, which indicated that most of the metal atoms on the surface were exposed.