Effect of residual carbon on the phase transformation and microstructure evolution of alumina-mullite fibers prepared by sol-gel method

Sol-gel method, as one of the most effective methods, has been widely used in producing high-property ceramics. In this method, the pyrolysis of precursor significantly influences the following microstructure evolution and properties of ceramic materials. In this work, the effect of residual carbon, influenced by the pyrolysis atmosphere, on the phase transition and microstructure evolution of the alumina-mullite fibers was investigated. It was revealed that the phase transition path of the preheated fibers with 0.53 wt% residual carbon was amorphous phase → aluminosilicate → tetragonal mullite → orthorhombic mullite + θ-Al₂O₃. The phase transition path of the preheated fibers with 10.51 wt% residual carbon became amorphous phase → γ-Al₂O₃ → orthorhombic mullite + α-Al₂O₃ + θ-Al₂O₃. In addition, the residual carbon contributes to improve the densification of alumina-mullite fibers and refine the fiber grain size. The effect of residual carbon on the formation of mullite coarse grains was further discussed.     

Investigation of microstructure and properties in short carbon fiber reinforced silica-based ceramic cores via atmosphere sintering

Short carbon fiber (C_sf) reinforced silica-based ceramic cores for investment casting were prepared by an injection molding approach and sintered in air and N₂ atmospheres, respectively. SEM and XRD results present that there are some in-situ formed silicon carbides (SiC) in sintered samples. Moreover, as for the ceramic cores sintered in N₂ atmosphere, the peaks in XRD patterns related to the cristobalite increase with an increment in C_sf content, which may be attributed to the adhesion interface provided by the C_sf and the decreased crystallization free energy. Interestingly, the sample sintered in N₂ exhibits a higher flexural strength about 16.2 MPa, which is 155 % times than that of the samples sintered in air. This is originated from an obvious composite coating consisting of fused silica, SiC and cristobalite on the C_sf. In addition, the sintering necks can further enhance the interfacial bonding strength between the fibers and ceramic cores matrix.     

Pressureless reaction sintering of yttrium aluminium garnet (YAG) from powder precursor in the hydroxyhydrogel form

Pressureless reaction sintering of YAG was carried out by using a precursor powder in the hydroxyhydrogel form synthesized by flash polycondensation technique. Reactive silica additive was used to modify Al-O-Y network where Si⁴⁺ was incorporated in the solvated form. The sintering experiments were carried out with the processed powder up to 1650 °C under ambient ambience. Densification indicated effective sintering with well-formed microstructure. Phase identification by XRD indicated only YAG in the sintered specimen.     

The effect of yttrium nitrate addition on the densification behaviour of Y2O3 ceramics during the cold sintering process

The densification behaviour and phase development of Y₂O₃ ceramics were investigated as a function of yttrium nitrate (Y(NO₃)₃·6H₂O) solution addition during the cold sintering process at 200 °C. Second phases such as Y₄O(OH)₉NO₃ and Y(OH)₃ were observed after the cold sintering process. The amount of Y₄O(OH)₉NO₃ increased with increasing amount of yttrium nitrate, while the amount of Y(OH)₃ decreased. The second phases were transformed to fine sized Y₂O₃ (∼30 nm) particles smaller than those of the raw powder (<400 μm) by sintering at 600 °C. The fine sized Y₂O₃ particles were located in the voids between the larger Y₂O₃ particles, thus increasing the packing density and enhancing the densification of the Y₂O₃ ceramics after the final sintering process.     

Effects of yttrium additions on the microstructure and charge transport properties of indium tin oxide semiconductors

The effects of yttrium (Y) additions (x=0, 0.05, 0.1, and 0.2) on the microstructure, chemical structure, and electrical properties of Y_xInSnO_y (YITO) thin films, prepared using a sol-gel process were examined. The transmission electron microscopy (TEM) observations showed that the undoped InSnO (ITO) film consisted of an amorphous structure with local crystalline domains on the film surface, whereas the Y additions (x=0.05, 0.1, and 0.2) to ITO suppressed the formation of the crystalline phase. X-ray photoelectron spectroscopy (XPS) analysis showed that the Y content decreased the concentration of oxygen vacancies owing to the strong incorporation of Y with oxygen. As a result of the Y incorporation, the carrier concentration of ITO films decreased. The saturation mobility (μ_sat), the on-off ratios (I_on/off), and the sub-threshold swing (S.S) of YITO films were 1.1 cm² V⁻¹ s⁻¹, ~10⁶, and ~0.5 V decade⁻¹, respectively, which are comparable with 1.7 cm² V⁻¹ s⁻¹, ~10⁵, and ~1.17 V decade⁻¹ of ITO film. Additionally, the initial threshold voltage (V_TH) was positive shift with increased of Y addition and V_TH shift (ΔV_TH) under the positive bias stress (PBS) results decreased by Y addition.     

Effect of residual excess carbon on the densification of ultra-fine HfC powder

The residual carbon content of ultra-fine hafnium carbide (HfC) powder was controlled by the optimization of the synthesis process, and the effect of residual carbon on the densification of HfC powder was analyzed. The amount of residual carbon in the HfC powder could be reduced by the de-agglomeration of HfO₂ powder before the carbo-thermal reduction (CTR) process. The average particle size of HfO₂ powder decreased from 230 to 130 nm after the de-agglomeration treatment. Ultra-fine (d₅₀: 110 nm) and highly pure (metal basis purity: >99.9 % except for Zr) HfC powder was obtained after the CTR at 1600 °C for 1 h using the C/Hf mixing ratio of 3.3. In contrast, the C/Hf ratio increased to 3.6 without the de-agglomeration treatment, indicating that a large amount of excess carbon was required for the complete reduction of the agglomerated HfO₂ particles. HfC ceramics with high relative density (>98 %) were obtained after spark plasma sintering at 2000 °C under 80 MPa pressure when using the HfC powder with low excess carbon content. In contrast, the densification did not complete at a higher temperature (2300 °C) and pressure (100 MPa) when the HfC powder contained a large amount of residual carbon. The results clearly indicated that residual carbon suppressed the densification of HfC powder in case the carbide powder had low oxygen content, and the residual carbon content could be controlled by the optimization of the synthesis process. The average grain size and Vickers hardness of the sintered specimen were 6.7(±0.7) μm and 19.6 GPa, respectively.     

Effect of Ca2+ and Mg2+ ions on the sintering and spectroscopic properties of cr-doped yttrium aluminum garnet ceramics

In this work, we investigated the effects of Ca²⁺ and Mg²⁺ ions and annealing temperature on the spectroscopic parameters of chromium-doped yttrium aluminum garnet ceramics (Cr:YAG). Samples were obtained with either a separate or a simultaneous addition of calcium and magnesium oxides. To achieve this, aqueous suspensions were prepared using Y₂O₃, Al₂O₃, Cr₂O₃, MgO, and CaO high-purity powders as raw materials. The obtained suspensions were freeze-granulated, pressed into pellets, debinded, and subjected to reactive sintering in vacuum at 1715°C for 6 h. Each material was annealed in air with temperatures between 1300 and 1700°C. Samples were also compared to Cr:YAG ceramics with the addition of silica as a sintering aid. All the materials obtained were then exposed to 445 nm excitation, and emission spectra in the visible and infrared wavelengths were recorded. The results showed that the emission spectra of Cr:YAG ceramics varied according to the annealing conditions: as-sintered samples exhibited strong emissions of around 680 nm and, after air annealing, of around 1400 nm. This phenomenon is attributed to the Cr³⁺→Cr⁴⁺ transition. Samples doped solely with MgO exhibited the highest emission intensity in the infrared region. Thus, Mg²⁺ ions provided the best conversion efficiency of chromium ions.     

Influence of sintering atmosphere on the phase,microstructure, and lithium-ion conductivity of the Al-doped Li7La3Zr2O12 solid electrolyte

Al-doped Li₇La₃Zr₂O₁₂ (Al–LLZO) solid electrolytes were sintered at 1150 ^°C for 8 h in atmosphere of oxygen, argon and air (named as Al–LLZO–O₂, Al–LLZO–Ar and Al–LLZO–Air, respectively). All the Al–LLZO samples exhibited a single cubic garnet-type structure. The sample of Al–LLZO–O₂ possessed the highest relative density (95.60%) and the largest average grain size among the three Al–LLZO samples. Furthermore, owing to its high relative density and small number of grain boundaries, Al–LLZO–O₂ demonstrated a higher lithium-ion conductivity than Al–LLZO–Ar and Al–LLZO–Air.     

Improved microstructure and sintering temperature of bismuth nano-doped GDC powders synthesized by direct sol-gel combustion

To improve the microstructural and electrochemical properties of Gadolinium-doped ceria (GDC) electrolytes, materials co-doped ceria with bismuth oxide (1–5 mol%) have been successfully prepared in a one-step sol-gel combustion synthetic route. Sol-gel combustion facilitates molecular mixing of the precursors and substitution of the large Bi³⁺ cations into the fluorite structure, considerably reducing the sintering temperature. Adding Bi₂O₃ as a dopant increases the GDC densification to above 99.7% and reduces its traditional sintering temperature by 300 °C. Impedance analyses show that the addition of bismuth enhances the conductivity (3.1?10^?2?1.7?10^?1 S·cm^?1 in the temperature range 600–800 °C) and improves the performance of the solid electrolyte in intermediate-temperature solid oxide fuel cells.     

Influence of sintering atmosphere on phase,microstructure and mechanical properties of Li4Si0.7Ti0.3O4 tritium breeding ceramics

Li₄Si_1–xTi_xO₄ ceramic solid solution was considered as a promising tritium breeding material for fusion reactor blanket. In this work, the effects of the sintering atmosphere on the phase composition, microstructure, and mechanical properties of Li₄Si_0.7Ti_0.3O₄ ceramic pebbles were investigated for the first time, aiming to explore the optimal sintering atmosphere for this solid solution. The results show that compared with air and argon atmosphere, the negative pressure of vacuum atmosphere was more favorable for Ti to enter the Li₄SiO₄ crystal structure as a substitute for Si atom to form a solid solution. More importantly, sintering in argon-vacuum atmosphere can ensure the formation of solid solution while fully exerting the liquid phase sintering effect. The crushing load of the Li₄Si_0.7Ti_0.3O₄ ceramic pebbles sintered at 800 °C in argon-vacuum atmosphere reaches 30.3 ± 3.2 N. In general, the appropriate sintering atmosphere was of great significance for obtaining Li₄Si_0.7Ti_0.3O₄ solid solution to meet the performance requirements of tritium breeding blanket.     

Effect of Y2O3 and ZnO co-doping on the densification and properties of magnesium aluminum spinel

The effects of Y₂O₃ and ZnO co-doping on the densification and properties of magnesium aluminum spinel were investigated. The physical phase composition, microstructure, elemental distribution, densification, apparent porosity, particle size distribution and average corrosion depth of the specimens were investigated by XRD, SEM-EDS, Archimedes drainage method, Nano Measurer 1.2 software, and molten salt corrosion tests. The results showed that after co-doping with Y₂O₃ and ZnO, the cations in the sintering aids could dissolve into the spinel structure, forming solid solution ZnAl₂O₄, second phase Y₃Al₅O₁₂ and Al₂Y₄O₉, which inhibited the abnormal grain growth and made the grain distribution more uniform, thus promoting the densification of the samples. The best co-doping amount of Y₂O₃ and ZnO was 1 wt% Y₂O₃-3 wt.% ZnO, the relative density of the sample was 99.3%, the apparent porosity was 0.021%, and the grain size was the most uniform (6.52 μm). After the sample was placed into the aluminum electrolytic molten salt electrolyte for 1 h, and it was found that the sample doped with 1 wt% Y₂O₃-3 wt.% ZnO had the minimum average corrosion depth (131.9 μm) and the best corrosion resistance.     

Processing and properties of porous SiC ceramics prepared by yttrium aluminum garnet infiltration

Oxide bonded porous SiC ceramics were synthesized by infiltrating a liquid precursor of yttrium aluminum garnet into porous powder compact of SiC followed by sintering at 1300‐1500°C in air. Infiltration rate was estimated using weight gain by the liquid precursor sol into porous SiC powder compact as a function of time and was explained by Darcy's and Ficks's laws. The effects of SiC particle sizes and sintering temperatures on the formation of bonding phases, microstructure, SiC oxidation degree, flexural strength, porosity, and pore size distribution of porous SiC ceramics were studied. Various crystalline oxide phases were detected by XRD analysis. Depending on the starting SiC powder sizes and sintering temperatures, the porosity of the final ceramics varied nearly in the range of ~29‐41 vol. % with the variation of average pore diameter between ~5 and 30 μm. Flexural strength varied from 41 to 8 MPa depending on porosity. The effect of corrosion on oxide bond phases was investigated in strong acidic and basic medium at 90°C. The ceramics showed better corrosion resistance in acidic medium compared to basic medium. In basic medium, significant reduction in flexural strength (~42%) was arisen.     

Effects of infiltration conditions on the densification behavior of carbon/carbon composites prepared by a directional-flow thermal gradient CVI process

Multiple quasi three-dimensioned carbon fibre preforms with disk-like shape were simultaneously densified by a directional flow thermal gradient CVI process. The effects of infiltration conditions, including temperature (ranging from 850 to 1050 °C), temperature gradient (5 and 10 °C/mm), pressure (2.5, 5.0, 7.5 and 9.5 kPa) and the type of carrier gas (N₂ or H₂), on the densification behavior of the resultant carbon/carbon composites were investigated. The results showed that lower temperatures (below 900 °C), a larger temperature gradient and higher pressure are favorable for higher average bulk density and homogeneous infiltration. Carbon/carbon composites disks with an average bulk density of 1.78 g/cm³ were achieved in one CVI cycle at a total pressure of 9.5 kPa. It was also found that adding N₂ carrier gas has no pronounced influence on the densification of the preforms. As compared to N₂, H₂ had positive effects on the densification of the preforms for temperatures above 900 °C, but it had negative effects on the densification when the control temperature was as low as 850 °C.     

The effect of the annealing atmosphere on the properties of Sr2Bi4Ti5O18 ferroelectric thin films

The Sr₂Bi₄Ti₅O₁₈ (SBT-5) ferroelectric thin films were prepared on Pt/Ti/SiO₂/Si substrate using the sol-gel method and annealing in oxygen, air, and nitrogen. Their properties were measured. After annealing in oxygen, the films showed good crystallization and a larger average grain size of approximately 34.05 nm. XPS analysis clearly showed that annealing in oxygen inhibited the generation of oxygen vacancies in the films, which contributed to the melioration of the ferroelectric properties. The remanent polarization was 20.09 μC/cm² and the coercive field was 75 kV/cm. When the electric field was 15 kV/cm, the leakage current density was approximately 3.88 × 10⁻⁷A/cm², while the Ohmic conduction was the dominating leakage mechanism. Because the content of the oxygen vacancy in the samples annealed in oxygen atmosphere was lower, the fixing effect on the domain structure was weaker and the volume effect was not obvious, so the aging degree of the samples was low. The larger relative dielectric constant was 742, while the dielectric loss was 0.037 when the test frequency was 2.0 × 10⁵ Hz.     

Effects of the sintering atmosphere on Nb-based dielectrics

The effects of a forming atmosphere on the stability, the sintering and the dielectric properties of Ba₅Nb₄O₁₅, BaNb₂O₆, ZnNb₂O₆ and Zn₃Nb₂O₈ ceramics were investigated, because of the primary importance of the sintering atmosphere in relation to copper sintering. These Nb-based materials were sintered in air and in Ar/H₂10%. Zn-containing samples are very sensitive to the reductive atmosphere. ZnO volatilises at 800–850 °C and the resulting compound does not exhibit the expected properties. BaNb₂O₆ and Ba₅Nb₄O₁₅ are more stable in term of relative weight loss. Nevertheless, the phase analysis reveals a modification of the BaNb₂O₆ phase, what induces the degradation of the dielectric property stability versus temperature. The properties of Ba₅Nb₄O₁₅ are not modified by a sintering in reductive atmosphere. A relative permittivity of 38.8, a permittivity temperature coefficient of −150 ppm °C⁻¹ and an insulating resistivity of 10^10.9 Ω cm were obtained for this latter.     

Effect of HCl concentration on the sintering behavior of 8 mol% Y2O3 stabilized ZrO2 deposits produced by electrophoretic deposition (EPD)

In this work, we have investigated the effect of HCl concentration and particle packing on the sintering behavior of 8 mol% yttria-stabilized-zirconia (8YSZ) deposits. 8YSZ deposits were fabricated by electrophoretic deposition (EPD). For 8YSZ coatings, it was found that the concentration of HCl in the EPD suspension significantly influences the neck size to grain size ratio. High neck size to grain size ratio (0.8 ± 0.03) was found in the sintered 0.8 HCl coating. The grain growth was observed to depend on the initial particle packing in the green coating. The effect of chloride ions on the grain and neck growth as well as elemental segregation within the 8YSZ is investigated using photoelectron spectroscopy (XPS) which confirmed the presence of chloride ions in green and sintered 8YSZ coatings. This was later confirmed using high-resolution transmission electron microscopy (HRTEM) and thermal analysis techniques. It was found that the presence of chloride ions induced an increase in the oxygen vacancy concentration at the grain boundaries. High oxygen vacancy concentration in the grain boundaries could promote neck growth of 8YSZ.     

Effect of dual liquid phase sintering aids on the densification and microstructure of low temperature sintered alumina ceramics

Alumina ceramics was prepared by pressureless sintering technology in which a CuO–TiO₂–Bi₂O₃ mixture (0–4.0 wt% Bi₂O₃ and 4.0 wt% CuO and TiO₂) was added as dual liquid phase sintering aids. The phase compositions, microstructural feature, and sintering behaviour of the alumina ceramics were analyzed. The results showed that adding 2.5 wt% Bi₂O₃ to alumina ceramics can increase the contribution rate of initial stage of sintering to the sintering process. The relative density of the sample reached 97.63% after sintering at 1200 °C for 90 min. Measurements from differential scanning calorimetry, with the addition of CuO–TiO₂–Bi₂O_3, demonstrated the formation of two liquid phase points, 827.4 and 936.8 °C. Notably, the solid solution temperature of TiO₂ and Al₂O₃ ceramics diminished thanks to the dual liquid phase sintering aids, and at the same time the activation energy required also dropped from 368.96 to 137.31 kJ/mol. Research indicates that the combined action of dual liquid phase sintering and solid-state reaction sintering has promoted the densification of alumina ceramics during the sintering process while at the same time inhibiting the growth of abnormal grains so that a homogeneous microstructure can be formed.     

Effects of Sn4+ doping and oxygen vacancy on magnetic and electrical properties of yttrium iron garnet prepared by sol-gel method

Sn-substituted yttrium iron garnet samples, Y₃Fe_5-xSn_xO₁₂ (x = 0–0.1, step 0.02) were prepared using a citrate sol–gel method and followed by a sintering process. Synchrotron X-ray diffraction (SXRD), X-ray absorption near edge structure (XANES), scanning electron microscope (SEM) and Fourier infrared spectroscopy (FTIR) measurements were used to investigate the structure parameters, valence state of Fe, oxygen vacancies and lattice distortion in the samples. The magnetic properties of the samples were measured with the SQUID and VSM equipments. The Sn substitution and oxygen vacancies cause the transformation of Fe³⁺ to Fe²⁺ which leads to the decrease of Curie temperature and slight increase of saturation magnetization. Temperature dependence of the resistivity in the range of 300–573 K was investigated to elucidate the conduction mechanism in the samples. The resistivity of the sol-gel derived samples was found to be nine orders of magnitudes lower than the value for the bulk sample prepared by flux-grown method. The effects of Fe²⁺ centers, lattice dislocation, porosity and grain boundary on the resistivity are discussed. This study indicates that Sn-substituted yttrium iron garnets are good candidates for sensor elements which operate based on electrical signals.     

Densification behavior and mechanical properties of nano-alumina ceramics prepared by Spark Plasma Sintering with pressure applied at different sintering stages

High densification and fine grain size are the key to achieve excellent mechanical properties of ceramic materials. Pressure-assisted sintering is an effective approach to achieve this goal. However, the pressure at different sintering stages has different effects on the densification behavior of nano-ceramics. In this work, it is found that adjusting the pressure applying regime during Spark Plasma Sintering of nano-alumina ceramics can effectively increase the densification rate and balance the relationship between the densification behaviors of particle coarsening, grain growth and vapor migration. When the pressure is applied at the beginning of the second sintering stage, the high densification and fine grain size microstructures can be both obtained at lower temperatures, leading to the best mechanical properties. This result is of great significance for the preparation of nano-ceramics with excellent mechanical properties.