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At least 847 records · Page 47

A chemical bath deposition route to facet-controlled Ag{sub 3}PO{sub 4} thin films with improved visible light photocatalytic activity

A facile, economic, and reproducible chemical bath deposition (CBD) method is developed for the fabrication of facet-controlled Ag{sub 3}PO{sub 4} thin films with enhanced visible light photocatalytic activity. The fine-control of bath temperature, precursor, complexing agent, substrate, and solution pH is fairly crucial in preparing the facet-selective thin film of Ag{sub 3}PO{sub 4} nanocrystal. The change of precursor from silver nitrate to silver acetate makes possible the tailoring of the crystal shape of Ag{sub 3}PO{sub 4} from cube to rhombic dodecahedron and also the bandgap tuning of the deposited films. The control of [Ag{sup +}]/[phosphate] ratio enables to maximize the loading amount of Ag{sub 3}PO{sub 4} crystals per the unit area of the deposited film. All the fabricated Ag{sub 3}PO{sub 4} thin films show high photocatalytic activity for visible light-induced degradation of organic molecules, which can be optimized by tailoring the crystal shape of the deposited crystals. This CBD method is also useful in preparing the facet-controlled hybrid film of Ag{sub 3}PO{sub 4}–ZnO photocatalyst. The present study clearly demonstrates the usefulness of the present CBD method for fabricating facet-controlled thin films of metal oxosalt and its nanohybrid. - Highlights: • The crystal facet of Ag{sub 3}PO{sub 4} films can be tuned by chemical bath deposition. • The crystal shape of Ag{sub 3}PO{sub 4} is tailorable from cube to rhombic dodecahedron. • Facet-tuned Ag{sub 3}PO{sub 4} film shows enhanced visible light photocatalyst activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A fresnoite-structure-related mixed valent titanium(III/IV) chlorosilicate, Ba{sub 3}Ti{sub 2}Si{sub 4}O{sub 14}Cl: A flux crystal growth route to Ti(III) containing oxides

Single crystals of mixed valent barium titanium(III/IV) chlorosilicate, Ba{sub 3}Ti{sub 2}Si{sub 4}O{sub 14}Cl{sub 0.91}O{sub 0.09}, were grown in a high temperature molten chloride flux involving an in situ reduction step. The fresnoite structure related Ba{sub 3}Ti{sub 2}Si{sub 4}O{sub 14}Cl{sub 0.91}O{sub 0.09} crystallizes in the tetragonal space group P4/mbm with lattice parameters of a=8.6717(2) Å, c=18.6492(5) Å. The title compound exhibits a 3D structure consisting of 2D layers of fused Ti{sub 2}O{sub 9} and Si{sub 4}O{sub 12} groups and 2D layers of fused Ti{sub 2}O{sub 9}Cl{sub 2} and Si{sub 2}O{sub 7} groups that are linked via barium atoms. The in situ reduction of Ti(IV) to Ti(III) is achieved via the addition of metallic Mg to the flux to function as the reducing agent. The temperature dependence of the magnetic susceptibility shows simple paramagnetism above 100 K. There is a discontinuity in the susceptibility data below 100 K, which might be due to a structural change that takes place resulting in charge ordering. - Graphical abstract: The fresnoite structure related novel reduced barium titanium chlorosilicate, Ba{sub 3}Ti{sub 2}Si{sub 4}O{sub 14}Cl{sub 0.91}O{sub 0.09}, were synthesized via flux method. An in situ reduction of Ti(IV) to Ti(III) achieved using Mg metal. The 3D structure consists 2D layers of fused Ti{sub 2}O{sub 9} and Si{sub 4}O{sub 12} and 2D layers of fused Ti{sub 2}O{sub 9}Cl{sub 2} and Si{sub 2}O{sub 7} connected via barium atoms. Compound shows simple paramagnetism above 100 K. - Highlights: • The fresnoite related Ba{sub 3}Ti{sub 2}Si{sub 4}O{sub 14}Cl{sub 0.91}O{sub 0.09} were grown via molten flux method. • The in situ reduction of Ti(IV) to Ti(III) is achieved using metallic Mg. • 2D layers of Ti{sub 2}O{sub 9} and Si{sub 4}O{sub 12} and Ti{sub 2}O{sub 9}Cl{sub 2} and Si{sub 2}O{sub 7} connect via Ba atoms. • The magnetic susceptibility shows simple paramagnetism above 100 K.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

MgO:Dy{sup 3+} nanophosphor: Self ignition route, characterization and its photoluminescence properties

For the first time series of MgO phosphors doped with different concentrations of Dy{sup 3+} (1–9 mol%) were prepared by solution combustion method using glycine as a fuel. The final products were well characterized by powder X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. The powder X-ray diffraction patterns of the as-formed product show single cubic phase. The crystallite size estimated using Scherrer's method was found to be in the range 5–15 nm and the same was confirmed by transmission electron microscopy result. Photoluminescence properties of Dy{sup 3+} (1–9 mol%) doped MgO for near ultra violet excitation (325 nm) was studied in order to investigate the possibility of its use in white light emitting diode applications. The emission spectra consists of intra 4f transitions of Dy{sup 3+}, namely {sup 4}F{sub 9/2} → {sup 6}H{sub 15/2} (483 nm), and {sup 4}F{sub 9/2} → {sup 6}H{sub 13/2} (573 nm). Further, the emission at 573 nm shows strong yellow emission and can be applied to the yellow emission of phosphor for the application for near ultraviolet excitation. The intensity of yellow emission was attributed to intrinsic defects, especially oxygen-vacancies, which could assist the energy transfer from the MgO host to the Dy{sup 3+} ions. The Commission International De I-Eclairage chromaticity co-ordinates were calculated from emission spectra, the values (x,y) were very close to the National Television System Committee standard value of white emission. Therefore, the present phosphor was highly useful for display applications. - Graphical Abstract: PL emission spectra and CIE diagram of MgO:Dy{sup 3+} nanophosphor. - Highlights: • MgO:Dy{sup 3+} prepared by simple and low cost LCS method at low temperature (400 °C). • Characteristic emission peaks of Dy{sup 3+} ion at ∼ 483 and 573 nm are recorded. • CIE co-ordinate values located in the white region. • Present phosphor was quite useful for display applications.

36 MATERIALS SCIENCE↗

A new route for the synthesis of submicron-sized LaB{sub 6}

Submicron crystalline LaB{sub 6} has been successfully synthesized by a solid-state reaction of La{sub 2}O{sub 3} with NaBH{sub 4} at 1200 °C. The effects of reaction temperature on the crystal structure, grain size and morphology were investigated by X-ray diffraction, scanning electron microscope and transmission electron microscope. It is found that when the reaction temperature is in the range of 1000–1100 °C, there are ultrafine nanoparticles and nanocrystals that coexist. When the reaction temperature elevated to 1200 °C, the grain morphology transformed from ultrafine nanoparticle to submicron crystals completely. High resolution transmission electron microscope images fully confirm the formation of LaB{sub 6} cubic structure. - Highlights: • Single-phased LaB{sub 6} have been synthesized by a solid-state reaction in a continuous evacuating process. • The reaction temperature has a important effect on the phase composition. • The grain size increase from nano-size to submicron with increasing reaction temperature.

36 MATERIALS SCIENCE↗

Utilizing maleic acid as a novel fuel for synthesis of PbFe{sub 12}O{sub 19} nanoceramics via sol–gel auto-combustion route

PbFe{sub 12}O{sub 19} nanostructures were prepared in an aqueous solution by the sol–gel auto-combustion method using Pb(NO{sub 3}){sub 2} and Fe(NO{sub 3}){sub 3} as starting materials and various carboxylic acids, including oxalic acid, malonic acid, succinic acid and maleic acid as fuel and reducing and capping agents. The as-synthesized products were characterized by X- ray diffraction, scanning electron microscopy, and X-ray energy dispersive spectroscopy. The effect of carboxylic acid type, Pb{sup +} {sup 2} to carboxylic acid molar ratio, and calcination temperature was investigated on the morphology of the products and several experiments were carried out to obtain the optimal reaction conditions. It was found that the phase and the morphology of the products are influenced by the investigated parameters. Furthermore, vibrating sample magnetometer (VSM) was used to study the magnetic properties of PbFe{sub 12}O{sub 19} samples. - Graphical abstract: Display Omitted - Highlights: • PbFe{sub 12}O{sub 19} nanoceramics were synthesized from Fe(NO{sub 3}){sub 3} and Pb(NO{sub 3}){sub 2} via the sol–gel auto combustion method. • The maleic acid can be instead of common capping agent and fuel in auto-combustion sol–gel. • The synthesized PbFe{sub 12}O{sub 19} is a hard magnetic material. • The specific saturation magnetization and coercivity are 27 emu/g and 1900 Oe, respectively.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Additive manufacturing as a processing route for steel-aluminum bimetallic structures

Here we present results on the fabrication of steel-aluminum bi-metallic structures using directed energy deposition additive manufacturing. The challenges associated with the fabrication of a sharp transition from steel to aluminum are uncovered using ex-situ characterization techniques and thermo-mechanical modeling of the deposition process. It was found that the fabrication of a sharp steel-aluminum transition is challenging with extensive cracking observed at the interface. The cracking was attributed to the combined effect of residual stress development due to thermal expansion coefficient mismatch and the presence of ordered intermetallics with low ductility at the interface. Using a coupled thermodynamic and thermo-mechanical modeling approach, potential pathways to enable the fabrication of steel-aluminum bi-metallic structures using additive manufacturing are proposed. The results presented here can lay the foundation for future work on the fabrication of bi-metallic steel-aluminum structures using directed energy deposition.

36 MATERIALS SCIENCE↗

Bioactive glass-ceramic coatings prepared by pulsed laser deposition from RKKP targets (sol-gel vs melt-processing route)

Highlights: Black-Right-Pointing-Pointer Bioactive glass-ceramic coatings for bone tissue repair and regeneration. Black-Right-Pointing-Pointer Pulsed Lased Deposition allowed congruent transfer of target composition to coating. Black-Right-Pointing-Pointer Target was prepared by sol-gel process suitable for compositional tailoring. Black-Right-Pointing-Pointer Titanium, widely used for orthopaedics and dental implants, was used as substrate. Black-Right-Pointing-Pointer The physico-chemical properties of the prepared coatings are reported. -- Abstract: The deposition of innovative glass-ceramic composition (i.e. RKKP) coatings by Pulsed Lased Deposition (PLD) technique is reported. RKKP was synthesised following two methodologies: melt-processing and sol-gel, the latter being particularly suitable to tailor the compositional range. The PLD advantage with respect to other deposition techniques is the congruent transfer of the target composition to the coating. The physico-chemical properties of films were investigated by Scanning Electron and Atomic Force Microscopies, Fourier Transform Infrared Spectroscopy, Angular and Energy Dispersive X-ray Diffraction, and Vickers microhardness. The deposition performed at 12 J/cm{sup 2} and 500 Degree-Sign C allows to prepare crystalline films with the composition that replicates rather well that of the initial targets. The 0.6 {mu}m thin melt-processing RKKP films, possessing the hardness of 25 GPa, and the 4.3 {mu}m thick sol-gel films with the hardness of 17 GPa were obtained.

36 MATERIALS SCIENCE↗

A simple route to disperse silver nanoparticles on the surfaces of silica nanofibers with excellent photocatalytic properties

Graphical abstract: The SiO{sub 2}/Ag composite nanofibers have been prepared by electrospinning and thermal decomposition of hybrid nanofibers, which exhibit a good catalytic property in reducing the methyl orange dye. Highlights: ► Hydrochloric acid was used as the catalyst of tetraethyl orthosilicate. ► Silver nanoparticles are obtained by pyrolysis of silver chloride. ► PVP–silica hybrid can disperse silver chloride and thus preventing the aggregation of silver nanoparticles. ► The catalytic activity of SiO{sub 2}/Ag composite nanofibers is much larger than that of SiO{sub 2} nanofibers. -- Abstract: In this work, monodispersed silver nanoparticles decorated SiO{sub 2} nanofibers were synthesized by electrospinning method, followed by thermal treatment at 600 °C. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermo-gravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS) were used to characterize the composite nanofibers. Accordingly, the detailed formation mechanism of SiO{sub 2}/Ag composite nanofibers was discussed. Furthermore, an excellent catalytic activity of SiO{sub 2}/Ag composite fibers was observed by a degradation reaction of methyl orange (MO) dye.

36 MATERIALS SCIENCE↗

Inspired superhydrophobic surfaces by a double-metal-assisted chemical etching route

Graphical abstract: A double-metal-assisted chemical etching method is employed to fabricate superhydrophobic surfaces, showing a good superhydrophobicity with the contact angle of about 170°, and the sliding angle of about 0°. Meanwhile, the potential formation mechanism about it is also presented. Highlights: ► A double-metal-assisted chemical etching method is employed to fabricate superhydrophobic surfaces. ► The obtained surfaces show good superhydrophobicity with a high contact angle and low sliding angle. ► The color of the etched substrate dark brown or black and it is so-called black silicon. -- Abstract: Silicon substrates treated by metal-assisted chemical etching have been studied for many years since they could be employed in a variety of electronic and optical devices such as integrated circuits, photovoltaics, sensors and detectors. However, to the best of our knowledge, the chemical etching treatment on the same silicon substrate with the assistance of two or more kinds of metals has not been reported. In this paper, we mainly focus on the etching time and finally obtain a series of superhydrophobic silicon surfaces with novel etching structures through two successive etching processes of Cu-assisted and Ag-assisted chemical etching. It is shown that large-scale homogeneous but locally irregular wire-like structures are obtained, and the superhydrophobic surfaces with low hysteresis are prepared after the modifications with low surface energy materials. It is worth noting that the final silicon substrates not only possess high static contact angle and low hysteresis angle, but also show a black color, indicating that the superhydrophobic silicon substrate has an extremely low reflectance in a certain range of wavelengths. In our future work, we will go a step further to discuss the effect of temperature, the size of Cu nanoparticles and solution concentration on the final topography and superhydrophobicity.

36 MATERIALS SCIENCE↗

An investigation on the influence of milling time and calcination temperature on the characterization of nano cerium oxide powder synthesized by mechanochemical route

Highlights: ► Synthesis of nanosized CeO{sub 2} was carried out using mechanochemical reactions plus sequential calcinations procedure. ► The effect of milling time and calcinations procedure on crystallite size and surface area of the as-synthesized powders was investigated. ► The extended milling times were exposed to result in the smaller crystallite size, and hence higher surface area for the as-synthesized powder. ► Higher calcinations temperatures, on the other hand, led to the as-synthesized powder with a larger crystallite size and therefore, lower surface area. ► Activation energy for nanocrystallite growth was calculated during the calcinations procedure and the aforementioned crystallite growth was found to be conducted in the light of interfacial reactions. -- Abstract: The synthesis of nano-sized CeO{sub 2} powder was investigated via mechanochemical reactions between hydrate cerium chloride and sodium hydroxide as the starting materials. The process was followed by a subsequent calcination procedure. Characterization of as-synthesized powder was performed using X-ray diffraction, FTIR spectroscopy, Brunner–Emmett–Teller (BET) nitrogen gas absorption, scanning electron microscopy (SEM) and particle size analyzer (PSA). The precursors were milled for different milling times and then were subjected to different heat treatment procedure at variable temperatures from 100 to 700 °C. According to the results, milling time and calcination temperatures induce paramountal effects on crystallite size and surface area of as-synthesized powders. In addition, the average activation energy for the growth of nanocrystals during calcination was determined to be about 12.53 kJ/mol, suggesting the influence of interfacial reactions on the crystallite growth during the calcination procedure.

36 MATERIALS SCIENCE↗

Characterization of nanostructured iron selenide thin films grown by chemical route at room temperature

Highlights: ► Nanostructured FeSe thin films were successfully synthesized at room temperature by CBD method. ► The XRD and EDAX characterization confirms nanocrystalline nature of FeSe. ► The SEM and AFM show microporous morphology with nanorods and nanoplates of FeSe. -- Abstract: Iron selenide thin films have been deposited onto glass substrates by using chemical bath deposition technique. Structural characterization of iron selenide thin films was carried out by means of X-ray diffraction and Fourier transforms infrared spectrum. The morphological characterization of FeSe thin film was carried out using scanning electron microscopy and atomic force microscopy, which revealed porous grain morphology of FeSe with some nano rectangular rods and plates grown on it. The as-deposited thin films exhibited optical band gap energy 2.60 eV. The as deposited FeSe thin films are semiconducting in nature with p-type electrical conductivity. The room temperature electrical resistivity is of the order of 1.1 × 10{sup 5} Ω-cm with activation energy 0.26 and 0.95 eV, respectively, in low and high temperature region.

36 MATERIALS SCIENCE↗

A self-propagation high-temperature synthesis and annealing route to synthesis of wave-like boron nitride nanotubes

Highlights: ► Large quantities of wave-like BN nanotubes were synthesized by SHS-annealing method. ► The catalytic boron-containing porous precursor was produced by self-propagation high-temperature synthesis method. ► Three growth models were proposed to explain the growth mechanism of the wave-like BN nanotubes. - Abstract: Large quantities of boron nitride (BN) nanotubes were synthesized by annealing a catalytic boron-containing porous precursor in flowing NH{sub 3} gas at 1180 °C. The porous precursor was prepared by self-propagation high-temperature synthesis (SHS) method at 800 °C using Mg, B{sub 2}O{sub 3} and amorphous boron powder (α-B) as the starting materials. The porous precursor played an important role in large quantities synthesis of BN nanotubes. The as-synthesized product was characterized by X-ray diffractometer (XRD), Fourier transform infrared spectrometer (FTIR), Raman, Scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS), Transmission electron microscopy (TEM) and High-resolution transmission electron microscopy (HRTEM). Characterization results indicated that the BN nanotubes displayed wave-like inner structures with diameters in the range of 50–300 nm and average lengths of more than 10 μm. The possible growth mechanism of the BN nanotubes was also discussed.

36 MATERIALS SCIENCE↗

Simple polyol route to synthesize heptanoic acid coated magnetite (Fe{sub 3}O{sub 4}) nanoparticles

Highlights: ► Heptanoic acid@Fe{sub 3}O{sub 4} nanocomposite has been prepared via simple polyol. ► Heptanoic acid used as both surfactant and solvents. ► Magneto polymer composite with adjustable Ea has a potential usage as functional composites. - Abstract: Magnetite (Fe{sub 3}O{sub 4}) nanoparticles were prepared via polyol method by using FeCl{sub 2} as only source of iron. As-prepared samples were characterized by powder X-ray diffractometer (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analyzer (TGA) and vibrating sample magnetometer (VSM). Crystalline phase was identified as Fe{sub 3}O{sub 4} and the crystallite sizes were calculated as 19.1 ± 1.1 and 22 ± 1.3 nm for uncalcinated and calcinated products from X-ray line profile fitting. The capping of heptanoic acid around Fe{sub 3}O{sub 4} nanoparticles was confirmed by FT-IR spectroscopy, the interaction being via bridging oxygen's of the carboxylate and the nanoparticle surface and also by TG analysis. VSM measurements showed that both samples exhibited typical superparamagnetic behavior at room temperature with different Ms values. The ε′ decreases with increasing frequency for both composites and permeability has almost same values for all temperatures at higher frequencies. As synthesized and calcinated samples conductivity increase linearly with the temperature.

36 MATERIALS SCIENCE↗

A facile mixed-solvothermal route to γ-Bi{sub 2}MoO{sub 6} nanoflakes and their visible-light-responsive photocatalytic activity

Graphical abstract: γ-Bi2MoO6 nanoflakes were successfully synthesized by a mixed-solvothermal process. The visible-light-responsive photocatalytic activities of the obtained γ-Bi2MoO6 nanoflakes were evaluated by photodegradation of Rhodamie B under visible light. The high degradation efficiency of RhB was attributed to the good crystallization and flake-like morphology of γ-Bi2MoO6 nanostructures, which is in accord with the photocurrent result. - Highlights: • γ-Bi{sub 2}MoO{sub 6} nanoflakes were obtained by a mixed-solvothermal process with SDBS as surfactant. • The photocurrent test was taken to characterize the photocatalytic activity. • The nanopowders exhibit high efficient photocatalytic activity under visibile-light irradiation. - Abstract: γ-Bi{sub 2}MoO{sub 6} nanoflakes were successfully synthesized by a mixed-solvothermal process with SDBS involved in the reaction. The as-prepared γ-Bi{sub 2}MoO{sub 6} was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and UV–vis absorption spectroscopy. The effect of different ratio of solvents on the resulting products was investigated. The visible-light-responsive photocatalytic activities of the obtained γ-Bi{sub 2}MoO{sub 6} nanoflakes were evaluated by photodegradation of Rhodamie B under visible light (λ > 400 nm). The high degradation efficiency of RhB was attributed to the good crystallization and flake-like morphology of γ-Bi{sub 2}MoO{sub 6} nanostructures, which is in accord with the photocurrent result.

36 MATERIALS SCIENCE↗

Effect of reductant and PVP on morphology and magnetic property of ultrafine Ni powders prepared via hydrothermal route

Graphical abstract: The ultrafine Ni powders with the shapes including sphere, pearl-string, leaf, fish-bone, hexagonal sheet and silknet were prepared through one-step hydrothermal reduction using different reductants. Their saturation magnetization, remanent magnetization and coercivity sequentially increase, and the coercivity of hexagonal sheet-like Ni powders increases by 25% compared with the Ni bulk counterpart. - Highlights: • The ultrafine Ni powders with various shapes of sphere, fish-bone, hexagonal sheet, etc. • Facile and one-step hydrothermal reduction using three reductants and PVP additive was developed. • Magnetic properties of the ultrafine Ni powders with different shapes were measured. • Compared with bulk Ni material, coercivity of hexagonal sheet Ni increases by 25%. • The formation mechanism of the shapes was suggested. - Abstract: The ultrafine nickel particles with different shapes including sphere, pearl-string, leaf, fish-bone, hexagonal sheet and silknet were prepared through one-step hydrothermal reduction using hydrazine hydrate, sodium hypophosphite and ethylene glycol as reductants, polyvinylpyrrolidone as structure-directing agent. It has been verified with the characterization of X-ray powder diffraction and transmission/scanning electronic microscopy that as-prepared products belong to face-centered cubic structure of nickel microcrystals with high purity and fine dispersity. The magnetic hysteresis loops measured at room temperature reveal that the values of saturation magnetization, remanent magnetization and coercivity rise sequentially from silknet, sphere to hexagonal sheet. In comparison with nickel bulk counterpart, the coercivity of the hexagonal sheet nickel powders increases by 25%.

36 MATERIALS SCIENCE↗

CdSe@ZnS nanocomposites prepared by a mechanochemical route: No release of Cd{sup 2+} ions and negligible in vitro cytotoxicity

Graphical abstract: - Highlights: • CdSe@ZnS nanocomposites were produced by milling. • Negligible cadmium leakage was observed. • No toxicity against living cells was documented. • The material is suitable for biological imaging. - Abstract: CdSe@ZnS nanocomposites have been prepared by a two-step solid state mechanochemical synthesis. CdSe prepared from Cd and Se elements in the first step was mixed with zinc acetate and sodium sulphide in the second step of milling to prepare a CdSe@ZnS nanocomposite. In the third step, the obtained nanocomposite was coated with L-cysteine to prepare a biocompatible system. The crystallite size of the new type of nanocomposite was 20–35 nm for cubic CdSe and 3–8 nm for hexagonal ZnS as calculated from XRD, TEM and SEM data. The synthesised samples show good crystallinity and have been tested for dissolution and cytotoxicity. The dissolution of cadmium from CdSe@ZnS was less than 0.05 μg mL{sup −1}, whereas a value of 0.8 μg mL{sup −1} was measured for CdSe alone. The binding of ZnS with CdSe in the nanocomposite practically eliminated the release of cadmium into solution. As a consequence, a very low cytotoxic activity has been evidenced for CdSe@ZnS. The nanocomposites coated with L-cysteine have a great potential as fluorescent labels in biomedical engineering.

36 MATERIALS SCIENCE↗