Influence of deposition temperature on microstructure and gas-barrier properties of Al2O3 prepared by plasma-enhanced atomic layer deposition on a polycarbonate substrate

We prepared polymer-based encapsulation films by plasma-enhanced atomic layer deposition (PEALD) of Al₂O₃ film on a polycarbonate (PC) substrate at 80–160 °C to fabricate Al₂O₃/PC barrier films. The thermal and dynamic mechanical properties of the PC substrate, the structural evolution of PEALD Al₂O₃ films, the optical transmission, surface morphology, and gas-barrier properties of Al₂O₃/PC film are all studied in this work as a function of temperature. The glass transition temperature T_g of the PC substrate is about 140 °C, and the coefficient of thermal expansion increases significantly when the temperature exceeds T_g. Increasing the deposition temperature from 80 to 160 °C for Al₂O₃ film deposited over 300 cycles increases the density from 3.24 to 3.45 g cm⁻³, decreases the thickness from 44 to 40 nm, and decreases the O/Al content ratio from 1.525 to 1.406. Al₂O₃/PC films deposited at 80–120 °C have no surface cracks, whereas surface cracks appear in samples deposited near or above 140 °C. Upon increasing the deposition temperature, the water vapor transmission rate (WVTR) and oxygen transmission rate (OTR) of Al₂O₃/PC films decrease significantly at temperatures below T_g, and then increase at temperatures near to or above T_g due to cracks in the films. The optimal deposition temperature is 120 °C, and the minimum WVTR and OTR of Al₂O₃/PC film are 0.00132 g per (m² 24 h) and 0.11 cm³ per (m² 24 h 0.1 MPa), respectively. The gas-barrier properties of the Al₂O₃/PC films are attributed to both the densification of the Al₂O₃ film and the cracks, which are caused by the shrinkage of the PC substrate.

Temperature dependence of the structural evolution of plasma-enhanced atomic layer deposited Al₂O₃ film and the PC substrate.     

Graphene tailored by Fe3O4 nanoparticles: low-adhesive and durable superhydrophobic coatings

This study reports stable superhydrophobic Fe₃O₄/graphene hybrid coatings prepared by spin coating of the Fe₃O₄/graphene/PDMS mixed solution on titanium substrates. By tailoring graphene sheets with Fe₃O₄ nanoparticles, the superhydrophobicity of graphene platelets was largely enhanced with a water contact angle of 164° and sliding angle <2°. Fe₃O₄ nanoparticles interact with FLG sheets via Fe–O–C covalent link, to form a graphene micro-sheet pinned strongly by nano-sized Fe₃O₄. The newly-formed micro/nano-structured sheets interact with each other via strong dipole–dipole attractions among Fe₃O₄ nanoparticles, confirmed by the blue shifts of G band observed in Raman spectra. The strongly interactive micro/nano-structured sheets are responsible for the improvement of both the surface hydrophobicity and the durability towards water impacting. The obtained hybrid coatings possess excellent durability in various environments, such as acidic and basic aqueous solutions, simulating ocean water. And also the coatings can retain their stable superhydrophobicity in Cassie–Baxter state even after annealing at 250 °C or refrigerating at −39 °C for 10 h. We employed an AFM to probe nanoscale adhesion forces to examine further the ability of the as-prepared coatings to resist the initial formation of water layers which reflects the ability to prevent the water spreading. The most superhydrophobic and durable hybrid coating with 1.8 g Fe₃O₄, shows the smallest adhesion force, as expected, indicating this surface possesses the weakest initial water adhesive strength. The resulting low-adhesive superhydrophobic coating shows a good self-cleaning ability. This fabrication of low-adhesive and durable superhydrophobic Fe₃O₄/FLG hybrid coatings advances a better understanding of the physics of wetting and yield a prospective candidate for various practical applications, such as self-cleaning, microfluidic devices, etc.

Strongly interactive graphene micro-sheets tailored by Fe₃O₄ nanoparticles exhibit low-adhesive and durable superhydrophobicity.     

A study on the viscosity reduction mechanism of high-filled silicone potting adhesive by the formation of Al2O3 clusters

Heat dissipation has become a key problem for highly integrated and miniaturized electronic components. High thermal conductivity, good flowability and low coefficient of linear thermal expansion (CLTE) are indispensable performance parameters in the field of electronic potting composite materials. In this study, spherical alumina (Al₂O₃) was surface modified by γ-(2,3-epoxypropoxy) propyltrimethoxy silane (KH560) and γ-aminopropyltriethoxy silane (KH550) and labelled as Al₂O₃-epoxy and Al₂O₃–NH₂, respectively. Al₂O₃-epoxy and Al₂O₃–NH₂ powders were equally filled in vinyl silicone oil to prepare a high Al₂O₃ loading (89 wt%) precursor of silicone potting adhesive. The viscosity of the precursor rapidly decreased with increasing reaction time of Al₂O₃-epoxy and Al₂O₃–NH₂ at 140 °C. The viscosity reduction mechanism may be due to the formation of some Al₂O₃ clusters by the reaction of Al₂O₃-epoxy with Al₂O₃–NH₂, which results in some vinyl silicone oil segments being held in the channel of particles through capillary phenomenon, leading to the friction among Al₂O₃ clusters decreasing considerably. Laser particle size analysis and scanning electron microscopy (SEM) results confirmed the existence of Al₂O₃ clusters. Energy dispersive spectroscopy (EDS) and dynamic viscoelasticity experiments revealed that some segments of vinyl silicone oils were held by Al₂O₃ clusters. When Al₂O₃-epoxy and Al₂O₃–NH₂ reacted for 4 h, the thermal conductivity, CLTE and volume electrical resistivity of the silicone potting adhesive reached 2.73 W m⁻¹ k⁻¹, 75.8 ppm/°C and 4.6 × 10¹³ Ω cm, respectively. A new strategy for preparing electronic potting materials with high thermal conductivity, good flowability and low CLTE is presented.

Surface-modified Al₂O₃-epoxy reacts with Al₂O₃–NH₂ to form clusters that reduce the viscosity of electronic potting composites.     

Water assisted atomic layer deposition of yttrium oxide using tris(N,N′-diisopropyl-2-dimethylamido-guanidinato) yttrium(iii): process development,film characterization and functional properties

We report a new atomic layer deposition (ALD) process for yttrium oxide (Y₂O₃) thin films using tris(N,N′-diisopropyl-2-dimethylamido-guanidinato) yttrium(iii) [Y(DPDMG)₃] which possesses an optimal reactivity towards water that enabled the growth of high quality thin films. Saturative behavior of the precursor and a constant growth rate of 1.1 Å per cycle confirm the characteristic self-limiting ALD growth in a temperature range from 175 °C to 250 °C. The polycrystalline films in the cubic phase are uniform and smooth with a root mean squared (RMS) roughness of 0.55 nm, while the O/Y ratio of 2.0 reveal oxygen rich layers with low carbon contaminations of around 2 at%. Optical properties determined via UV/Vis measurements revealed the direct optical band gap of 5.56 eV. The valuable intrinsic properties such as a high dielectric constant make Y₂O₃ a promising candidate in microelectronic applications. Thus the electrical characteristics of the ALD grown layers embedded in a metal insulator semiconductor (MIS) capacitor structure were determined which resulted in a dielectric permittivity of 11, low leakage current density (≈10⁻⁷ A cm⁻² at 2 MV cm⁻¹) and high electrical breakdown fields (4.0–7.5 MV cm⁻¹). These promising results demonstrate the potential of the new and simple Y₂O₃ ALD process for gate oxide applications.

A new water assisted atomic layer deposition (ALD) process was developed using the yttrium tris-guanidinate precursor which resulted in device quality thin films.     

Preparation and heat-insulating properties of Al2O3–ZrO2(Y2O3) hollow fibers derived from cogon using an orthogonal experimental design

Bionic design is efficient to develop high-performance lightweight refractories with sophisticated structures such as hollow ceramic fibers. Here, we report a four-stage procedure for the preparation of Al₂O₃–ZrO₂(Y₂O₃) hollow fibers using the template of cogon—a natural grass. Subsequently, to optimize the thermal performance of the fibers, four sets of preparation parameters, namely, x(Al₂O₃), solute mass ratio of the mixture, dry temperature, and sintering temperature were investigated. Through an orthogonal design, the optimal condition of each parameter was obtained as follows: x(Al₂O₃) was 0.70, solute mass ratio of the mixture was 15 wt%, dry temperature was 80 °C, and sintering temperature was 1100 °C. Overall, Al₂O₃–ZrO₂(Y₂O₃) hollow fibers show relatively low thermal conductivity (0.1038 W m⁻¹ K⁻¹ at 1000 °C), high porosity (95.0%), and low density (0.05–0.10 g cm⁻³). The multiphase compositions and morphology of Al₂O₃–ZrO₂(Y₂O₃) hollow fibers, which may contribute to their thermal properties, were also discussed.

Lightweight Al₂O₃–ZrO₂(Y₂O₃) hollow fibers with low thermal conductivity were prepared by a natural template—cogon grass.     

Influence of Al2O3 nanoparticle doping on depolarization temperature,and electrical and energy harvesting properties of lead-free 0.94(Bi0.5Na0.5)TiO3–0.06BaTiO3 ceramics

In this research article, the effects of Al₂O₃ nanoparticles (0–1.0 mol%) on the phase formation, microstructure, dielectric, ferroelectric, piezoelectric, electric field-induced strain and energy harvesting properties of the 0.94(Bi_0.5Na_0.5)TiO₃–0.06BaTiO₃ (BNT–6BT) ceramic were investigated. All ceramics have been synthesized by a conventional mixed oxide method. The XRD and Raman spectra showed coexisting rhombohedral and tetragonal phases throughout the entire compositional range. An increase of the grain size, T_F–R, T_m, ε_max and δ_A values was noticeable when Al₂O₃ was added. Depolarization temperature (T_d), which was determined by the thermally stimulated depolarization current (TSDC), tended to increase with Al₂O₃ content. The good ferroelectric properties (P_r = 32.64 μC cm⁻², E_c = 30.59 kV cm⁻¹) and large low-field d₃₃ (205 pC N⁻¹) values were observed for the 0.1 mol% Al₂O₃ ceramic. The small Al₂O₃ additive improved the electric field-induced strain (S_max and ). The 1.0 mol% Al₂O₃ ceramic had a large piezoelectric voltage coefficient (g₃₃ = 32.6 × 10⁻³ Vm N⁻¹) and good dielectric properties (ε_r,max = 6542, T_d = 93 °C, T_F–R = 108 °C, T_m = 324 °C and δ_A = 164 K). The highest off-resonance figure of merit (FoM) for energy harvesting of 6.36 pm² N⁻¹ was also observed for the 1.0 mol% Al₂O₃ ceramic, which is suggesting that this ceramic has potential to be one of the promising lead-free piezoelectric candidates for further use in energy harvesting applications.

In this research article, the effects of Al₂O₃ nanoparticles (0–1.0 mol%) on the phase, microstructure, dielectric, ferroelectric, piezoelectric, electric field-induced strain and energy harvesting of the BNT–6BT ceramic were investigated.     

Atomic layer deposition of dielectric Y2O3 thin films from a homoleptic yttrium formamidinate precursor and water

We report the application of tris(N,N′-diisopropyl-formamidinato)yttrium(iii) [Y(DPfAMD)₃] as a promising precursor in a water-assisted thermal atomic layer deposition (ALD) process for the fabrication of high quality Y₂O₃ thin films in a wide temperature range of 150 °C to 325 °C. This precursor exhibits distinct advantages such as improved chemical and thermal stability over the existing Y₂O₃ ALD precursors including the homoleptic and closely related yttrium tris-amidinate [Y(DPAMD)₃] and tris-guanidinate [Y(DPDMG)₃], leading to excellent thin film characteristics. Smooth, homogeneous, and polycrystalline (fcc) Y₂O₃ thin films were deposited at 300 °C with a growth rate of 1.36 Å per cycle. At this temperature, contamination levels of C and N were under the detectable limits of nuclear reaction analysis (NRA), while X-ray photoelectron spectroscopy (XPS) measurements confirmed the high purity and stoichiometry of the thin films. From the electrical characterization of metal–insulator–semiconductor (MIS) devices, a permittivity of 13.9 at 1 MHz could be obtained, while the electric breakdown field is in the range of 4.2 and 6.1 MV cm⁻¹. Furthermore, an interface trap density of 1.25 × 10¹¹ cm⁻² and low leakage current density around 10⁻⁷ A cm⁻² at 2 MV cm⁻¹ are determined, which satisfies the requirements of gate oxides for complementary metal-oxide-semiconductor (CMOS) based applications.

In this work, the application of tris(N,N′-diisopropyl-formamidinato)yttrium(iii) [Y(DPfAMD)₃] as a precursor in a water-assisted thermal atomic layer deposition (ALD) process for the fabrication of device quality Y₂O₃ thin films is demonstrated.     

High-temperature chlorination of PbO and CdO induced by interaction with NaCl and Si/Al matrix

Municipal solid-waste incineration leads to emission of lead (Pb) and cadmium (Cd), which vaporize in furnace and condense in flue. NaCl in waste has been proven to enhance volatilization of Pb and Cd at high temperatures via chlorination of oxides to chlorides; however, this process was not well-understood so far due to its complexity. This study decoupled the indirect chlorination process and direct chlorination process so that these two processes were investigated separately. A horizontal tube furnace was used to heat the mixtures of NaCl and Si/Al matrix for indirect chlorination and the mixtures of NaCl, PbO/CdO and Si/Al matrix for direct chlorination. A set of dynamic sampling devices was designed and used to obtain dynamic data during temperature rising. The indirect chlorination process was initiated above 800 °C in O₂ + H₂O atmosphere and O₂ atmosphere and above 1000 °C in N₂ atmosphere. Al₂O₃ exhibited higher activity than SiO₂ to react with NaCl, releasing HCl or Cl₂. In the Cl release reaction, NaCl was in the gas phase. The direct chlorination process was initiated at 650–700 °C when the Si/Al matrix contained SiO₂ only and at around 800 °C when the Si/Al matrix contained Al₂O₃ only or both SiO₂ and Al₂O₃. SiO₂ exhibited higher activity than Al₂O₃ in direct chlorination. The pre-reaction between PbO/CdO and Si/Al matrices was considered as the necessary condition for direct chlorination. During chlorination in O₂ + H₂O atmosphere, indirect chlorination and direct chlorination occurred simultaneously, and the latter dominated the volatilization of Pb and Cd.

The chlorination process by NaCl was decoupled as indirect chlorination and direct chlorination, which were investigated separately.     

Enhanced physical properties of γ-Al2O3–rGO hybrids prepared by solvothermal and hot-press processing

In this study, a solvothermal method was employed for the first time to fabricate hybrids composed of cross-linked γ-Al₂O₃ nanorods and reduced graphite oxide (rGO) platelets. After calcination and hot-press processing, monoliths of Al₂O₃–rGO hybrids were obtained with improved physical properties. It was found that the oxygen-containing groups on graphene oxide were beneficial for the adsorption of aluminum isopropoxide, leading to a uniform dispersion of rGO with Al₂O₃, which was obtained by hydrolysis of aluminum isopropoxide during the solvothermal reaction. The hybrid, which was subsequently calcinated for 3 h showed electrical conductivity of 6.7 × 10¹ S m⁻¹ together with 90% higher mechanical tensile strength and 80% higher thermal conductivity as compared to the bare Al₂O₃. In addition, the dielectric constant of the hybrid was 12 times higher than that of the bare Al₂O₃. In this study, the highest values of electrical conductivity (8.2 × 10¹ S m⁻¹), thermal conductivity (2.53 W m⁻¹ K⁻¹), dielectric constant (10⁴) and Young''s modulus (3.7 GPa) were obtained for the alumina–rGO hybrid calcinated for 1 h. XRD characterization showed that an increase in calcination temperature and further hot-press processing at 900 °C led to enhanced crystallinity in the γ-Al₂O₃ nanorods in the hybrid, resulting in enhanced physical properties in the hybrids.

After calcination and hot-press processing, monoliths of γ-Al₂O₃–rGO hybrids are obtained with improved physical properties.     

Effects of the addition of CeO2 on the steam reforming of ethanol using novel carbon-Al2O3 and carbon-ZrO2 composite-supported Co catalysts

Novel carbon-Al₂O₃ and carbon-ZrO₂ composite-supported Co catalysts were prepared using the sol–gel method with polyethylene glycol (PEG) as a carbon source, and the effects of the addition of CeO₂ to catalysts on the steam reforming of ethanol were investigated. The reactions were carried out in a fixed bed reactor with H₂O/EtOH = 12 (mol/mol) and a temperature range of 300 °C to 600 °C. The catalyst characterization was performed by XRD, nitrogen adsorption and desorption isotherms, TG-DTA, XRF and TEM. Although the carbon-Al₂O₃ composite-supported Co catalysts exhibited a higher conversion of ethanol than the carbon-ZrO₂ composite-supported Co catalysts, the effect of the addition of CeO₂ was hardly observed for catalysts with Al₂O₃. In contrast to the case of catalysts with Al₂O₃, the effect of the addition of CeO₂ to catalysts with ZrO₂ on the conversion and the hydrogen yield was observed, and the hydrogen yield at 600 °C exceeded that of catalysts with Al₂O₃. 16Co42C31.5Ce10.5Zr exhibited the highest hydrogen yield of 89% at 600 °C. Fine Co metal species were observed for the used ZrO₂-based catalysts, while Co₃O₄ peaks were observed for the used Al₂O₃-based catalysts. The development of the carbon nanotube-like structure with a diameter of 50 nm was observed with particles having diameters of 30 nm to 50 nm, suggesting that the carbon deposition might occur so as not to deactivate the catalyst.

For the ideal reaction routes in steam reforming of ethanol catalyzed by Co/CeO₂–ZrO₂, as Al₂O₃ was used instead of ZrO₂, the effect of CeO₂ did not appear, suggesting that the configuration of CeO₂ and cobalt species on ZrO₂ would be important.     

Charge balance control of quantum dot light emitting diodes with atomic layer deposited aluminum oxide interlayers

We developed a 1.0 nm thick aluminum oxide (Al₂O₃) interlayer as an electron blocking layer to reduce leakage current and suppress exciton quenching induced by charge imbalance in inverted quantum dot light emitting diodes (QLEDs). The Al₂O₃ interlayer was deposited by an atomic layer deposition (ALD) process that allows precise thickness control. The Al₂O₃ interlayer lowers the mobility of electrons and reduces Auger recombination which causes the degradation of device performance. A maximum current efficiency of 51.2 cd A⁻¹ and an external quantum efficiency (EQE) of 12.2% were achieved in the inverted QLEDs with the Al₂O₃ interlayer. The Al₂O₃ interlayer increased device efficiency by 1.1 times, increased device lifetime by 6 times, and contributed to reducing efficiency roll-off from 38.6% to 19.6% at a current density up to 150 mA cm⁻². The improvement of device performance by the Al₂O₃ interlayer is attributed to the reduction of electron injection and exciton quenching induced by zinc oxide (ZnO) nanoparticles (NPs). This work demonstrates that the Al₂O₃ interlayer is a promising solution for charge control in QLEDs and that the ALD process is a reliable approach for atomic scale thickness control for QLEDs.

We developed a 1.0 nm thick aluminum oxide (Al₂O₃) interlayer as an electron blocking layer to reduce leakage current and suppress exciton quenching induced by charge imbalance in inverted quantum dot light emitting diodes (QLEDs).     

Oxidation behavior of the TiAlN hard coating in the process of recycling coated hardmetal scrap

Recycling coated hardmetal scraps is becoming increasingly important for tungsten resource recovery. However, the coatings in these materials are one of the biggest problems, especially Al-containing coatings. In this study, discarded TiAlN-coated WC–Co hardmetal tool tips were isothermally oxidized at 900 °C in air, during which the final oxide, phase transition and microstructure evolution were investigated. Milled powders below 0.15 mm were completely oxidized in 180 min, and pieces of coatings were found in the final oxides. White WO₃ was mainly distributed on defect-rich areas of oxide scale surfaces. Furthermore, the final oxide scale was triple-layered, mainly consisting of the WO₃-concentrated outmost layer, the Al₂O₃-concentrated middle layer, and the TiO₂-concentrated inner layer. It is different from the bi-layered Al₂O₃/TiO₂ oxide scale that appeared for a new TiAlN-coated hardmetal during an oxidation resistance test. This was attributed to the defects in hardmetal scraps, which provided a fast pathway for element diffusion and volatilization of WO₃. Consequently, it was impossible to remove Al₂O₃ completely.

The final oxide scale was triple-layered, consisting of a WO₃-rich outmost layer, Al₂O₃-concentrated middle layer and TiO₂-concentrated inner layer.     

Nb-doped and Al2O3 + B2O3-coated granular secondary LiMn2O4 particles as cathode materials for lithium-ion batteries

In this work, to improve the cyclability and high-temperature performance of cubic spinel LiMn₂O₄ (LMO) as cathode materials, Nb⁵⁺-doped LiMn₂O₄ powders coated and uncoated with Al₂O₃ and/or B₂O₃ were synthesized via the modified solid-state reaction method. It was found that Nb⁵⁺-doped and B₂O₃ + Al₂O₃-coated LMO powders comprising 5 μm granular agglomerated fine primary particles smaller than 350 nm in diameter exhibited superior electrochemical properties with initial discharge capacity of 101.68 mA h g⁻¹; we also observed capacity retention of 96.31% after 300 cycles at room temperature (RT) and that of 98% after 50 cycles at 55 °C and 1C rate.

Nb-doped and Al₂O₃ + B₂O₃-coated granular secondary LMO particles enabling superior cycling performance at 25 and 55 °C.     

Fabrication of a ceramic/metal (Al2O3/Al) composite by 3D printing as an advanced refractory with enhanced electrical conductivity

Fused deposition modelling (3D) printing is used extensively in modern fabrication processes. Although the technique was designed for polymer printing, it can now be applied in advanced ceramic research. An alumina/aluminum (Al₂O₃/Al) composite refractory can be fabricated by mixing metallic aluminum in a polymer to form an Al/polymer composite filament. The filament can be printed via a regular thermoplastic material extrusion printer with no machine modification. In this study, Al/polymer composite samples were printed in a crucible shape and sintered at different temperatures to form Al₂O₃/Al composite refractory specimens. The sintered samples were examined via several analytical techniques such as scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, compressive testing, hardness testing, XPS, and Hall measurement. Unlike other ceramic printing techniques that require expensive 3D printing machines and a very high temperature furnace (above 1500 °C) for post processing, this study demonstrates the viability of fabricating refractory items using a cost-effective fused deposition modelling 3D printer and a low temperature furnace (900 °C). The samples did not disintegrate at 1400 °C and were still sufficiently electrically conductive for advanced refractory applications.

An Al₂O₃/Al composite is fabricated by the 3D printing, sintering, and calcination processes that can be used in refractory applications.     

Atomic layer deposition and tellurization of Ge–Sb film for phase-change memory applications

We studied the atomic layer deposition (ALD) and the tellurization of Ge–Sb films to prepare conformal crystalline Ge–Sb–Te (GST) films and to achieve void-free gap filling for emerging phase-change memory applications. ALD Ge–Sb film was prepared by alternating exposures to GeCl₂-dioxane and Sb(SiEt₃)₃ precursors at 100 °C. The growth rate was 0.021 nm per cycle, and the composition ratio of Ge to Sb was approximately 2.2. We annealed the ALD Ge–Sb films with a pulsed feeding of di(tert-butyl)tellurium. The ALD Ge–Sb films turned into GST films by the tellurization annealing. When the tellurization temperature was raised to 190 °C or higher temperatures, the Raman peaks corresponding to Ge–Sb bond and amorphous Ge–Ge bond disappeared. The Raman peaks corresponding to Ge–Te and Sb–Te bonds were evolved at 200 °C or higher temperatures, resulting in the phase transition temperature of 123 °C. At 230 °C or higher temperatures, the entire film was fully tellurized to form a GST film having a relatively uniform composition of Ge₃Sb₂Te₆, and the carbon impurities in the as-deposited ALD Ge–Sb film were eliminated. As the tellurization temperature increases, the volume of the ALD film is expanded owing to the incorporation of tellurium, resulting in complete filling of a trench pattern by GST film after the tellurization at 230 °C.

We studied the atomic layer deposition (ALD) and the tellurization of Ge–Sb films to prepare conformal crystalline Ge–Sb–Te (GST) films and to achieve void-free gap filling for emerging phase-change memory applications.     

Effect of sodium silicate on Portland cement/calcium aluminate cement/gypsum rich-water system: strength and microstructure

In this investigation, sodium silicate (SS) was mixed into rich-water (RW) materials consisting of Portland cement, calcium aluminate cement and gypsum for improved mechanical properties. The RW materials containing different amounts of SS were characterized by the compression test, mercury intrusion porosity, scanning electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. The results demonstrated that with the increase of SS additions, the early strength of the RW materials increases, and the long-term strength retrogression of the RW materials can be inhibited when the SS content is above 3%. Pore structures of the RW materials are improved significantly due to the filling effect of the calcium silicate hydration (C–S–H) gel from a reaction between silicate ions and Ca(OH)₂, thus increasing the early strength of the RW materials. For the RW materials containing SS and cured for 0 to 14 days, there are more hexagonal hydrates including CaO·Al₂O₃·10H₂O (CAH₁₀) and 2CaO·Al₂O₃·8H₂O (C₂AH₈), more C–S–H gel and less ettringite crystals, which is of benefit to the strength of the material. The strength retrogression can be attributed to phase conversions from hexagonal hydrates (CAH₁₀ and C₂AH₈) to cubic ones (3CaO·Al₂O₃·6H₂O) with lower intercrystal bonding forces. Furthermore, this phase conversion is inhibited effectively by the chemical reaction of silicate ions and CAH₁₀ (or C₂AH₈), improving the long-term strength of the RW materials.

After the addition of sodium silicate, the strength of the RW material is improved and the strength retrogression is inhibited.     

Study on the wetting interface of Zr–Cu alloys on the SiC ceramic surface

A Zr–Cu alloy, as a new type of filler metal, is proposed for brazing SiC ceramic under special working conditions. The wetting angle of Zr–Cu alloy/SiC ceramic at different temperatures and holding times was investigated by a high-temperature wetting tester. The composition of the wetting interface was tested by XRD, and the interfacial reaction layer was analyzed with SEM and EDS. The results show that the wetting angle decreases sharply with the change in temperature from 1100 °C to 1175 °C and remains unchanged when the temperature is higher than 1175 °C, about 34 ± 1°. The dynamic wetting angle of Zr–Cu/SiC at 1200 °C with the increase in holding time conforms to the law of exponential decay, and the equilibrium wetting angle is 5°. The transition layer with a certain thickness is formed during the spreading process of the Zr–Cu alloy at a high temperature, and the microstructure of the interfacial reaction layer mainly consists of ZrC and Zr₂Si.

A Zr–Cu alloy, as a new type of filler metal, is proposed for brazing SiC ceramic under special working conditions.     

Crystal growth control of rod-shaped ε-Fe2O3 nanocrystals

Herein we report crystal growth control of rod-shaped ε-Fe₂O₃ nanocrystals by developing a synthesis based on the sol–gel technique using β-FeO(OH) as a seed in the presence of a barium cation. ε-Fe₂O₃ nanocrystals are obtained over a wide calcination temperature range between 800 °C and 1000 °C. A low calcination temperature (800 °C) provides an almost cubic rectangular-shaped ε-Fe₂O₃ nanocrystal with an aspect ratio of 1.4, whereas a high calcination temperature (1000 °C) provides an elongated rod-shaped ε-Fe₂O₃ nanocrystal with an aspect ratio of 3.3. Such systematic anisotropic growth of ε-Fe₂O₃ is achieved due to the wide calcination temperature in the presence of barium cations. The surface energy and the anisotropic adsorption of barium on the surface of ε-Fe₂O₃ can explain the anisotropic crystal growth of rod-shaped ε-Fe₂O₃ along the crystallographic a-axis. The present work may provide important knowledge about how to control the anisotropic crystal shape of nanomaterials.

Crystal growth control of rod-shaped ε-Fe₂O₃ nanocrystals is achieved by a synthesis based on the sol–gel technique.     

Investigation of annealing effects on the physical properties of Ni0.6Zn0.4Fe1.5Al0.5O4 ferrite

In the present study, the structural, morphological, electrical, and dielectric properties of Ni_0.6Zn_0.4Fe_1.5Al_0.5O₄ annealed at 600 °C, 900 °C, and 1200 °C were investigated. The X-ray diffraction patterns confirmed the presence of the single-phase cubic spinel structure with the Fd$\bar{3}$m space group. The SEM images of Ni_0.6Zn_0.4Fe_1.5Al_0.5O₄ nanoparticles demonstrated that these samples (Ni900 and Ni1200) were nano-sized and that the increase in annealing temperature enhanced the agglomeration rate. It was found that the electrical conductivity of the system improved on increasing the temperature over the whole explored range for the two low annealing temperatures, while this improvement declined after 500 K in the case of the highest annealing temperature. For such a sample, a metallic behavior was seen. The sample annealed at 1200 °C possessed the highest conductivity and the lowest activation energy. The impedance measurements were in good agreement with the conductivity plots and confirmed the emergence of a grain boundary effect with the increase in annealing temperature. For the sample annealed at the highest temperature, Z′ decreased rapidly with frequency. This sample exhibited the lowest defect density than the other samples. Consequently, its electrical conductivity increased. A Nyquist diagram was used to examine the contribution of the grains and grain boundary to conduction and to model each sample by an equivalent electrical circuit. The dielectric behavior of the investigated samples was correlated to the polarization effect.

In the present study, the structural, morphological, electrical, and dielectric properties of Ni_0.6Zn_0.4Fe_1.5Al_0.5O₄ annealed at 600 °C, 900 °C, and 1200 °C were investigated.     

Structure,optical simulation and thermal stability of the HfB2-based high-temperature solar selective absorbing coatings

Transition metal borides are a kind of potential materials for high-temperature solar thermal applications. In this work, a novel SS/HfB₂/Al₂O₃ tandem absorber was prepared, which exhibited high solar spectrum selectivity (α/ε) of 0.920/0.109. The optical constants of the coating were obtained using spectroscopic ellipsometry, and the dispersion model of the HfB₂ layer was modeled with the Tauc–Lorentz dispersion formula. In addition, the reflectance spectrum simulated by the CODE software corroborated well with the experimental results. The thermal stability test indicated that the HfB₂/Al₂O₃ solar absorber coating was thermally stable in vacuum at 600 °C for 2 h. When extending the annealing time to 100 h, the coating could maintain high spectral selectivity after aging at 500 °C irrespective of whether in air or vacuum. All these results indicate that the coating has good solar selectivity and is a promising candidate for high-temperature solar thermal applications.

Transition metal borides are a kind of potential materials for high-temperature solar thermal applications.