Preparation of Ti3AlC2 by mechanically activated sintering with Sn aids

The mechanically activated sintering process was adapted to synthesize Ti₃AlC₂ using 3Ti/Al/2C/0.05Sn powder mixtures. The result showed that the powders containing TiC, Ti₃AlC₂ and Ti₂AlC were obtained by mechanical alloying (MA) 3Ti/Al/2C powders. Addition of appropriate Sn reduced the content of Ti₂AlC and enhanced the synthesis of Ti₃AlC₂ significantly. The powders with highest content of Ti₃AlC₂ were obtained by MA 3Ti/Al/2C/0.05Sn powders. Through pressureless sintering the mechanical alloyed powders at 900–1100 °C for 2 h, the high purity Ti₃AlC₂ material with fine organization was produced.     

Improved high-Q microwave dielectric resonator using ZnO-doped La(Co1/2Ti1/2)O3 ceramics

The microwave dielectric properties and the microstructures of ZnO-doped La(Co_1/2Ti_1/2)O₃ ceramics prepared by conventional solid-state route have been studied. Doped with ZnO (up to 0.75 wt%) can effectively promote the densification of La(Co_1/2Ti_1/2)O₃ ceramics with low sintering temperature. At 1320 °C, La(Co_1/2Ti_1/2)O₃ ceramics with 0.75 wt% ZnO addition possesses a dielectric constant (_r) of 30.2, a Q × f value of 73,000 GHz (at 8 GHz) and a temperature coefficient of resonant frequency (τ_f) of −35 ppm/°C.     

Densification, microstructural evolution, and dielectric properties of hexagonal Ba(Ti1−xMnx)O3 ceramics sintered with fluxes

Recently, doped hexagonal BaTiO₃ (6h-BaTiO₃) ceramics have been reported as potential candidates used in microwave dielectric resonators. However, similar to other common microwave ceramics, doped 6h-BaTiO₃ ceramics require a high sintering temperature, greater than 1300 °C. In this study, the effect of sintering aids, including Bi₂O₃, B₂O₃, BaSiO₃, Li₂CO₃, CuO, V₂O₅, 5ZnO·2B₂O₃, and 5ZnO·2SiO₂, on the densification, microstructural evolution, and microwave properties of the 6h-Ba(Ti_0.85Mn_0.15)O₃ ceramics was examined. Results indicate that among the fluxes studied, Bi₂O₃, B₂O₃, and Li₂CO₃ could effectively reduce the sintering temperature of 6h-Ba(Ti_0.85Mn_0.15)O₃ ceramics through liquid phase sintering, while retaining the hexagonal structure and the microwave dielectric properties. The best results were obtained for the 6h-Ba(Ti_0.85Mn_0.15)O₃ with the additions of 5 wt% Bi₂O₃ sintered at 900 °C (_r: 54.7, Qf_r: 1323, and τ_f:183.3 ppm/°C), 10 wt% B₂O₃ sintered at 1100 °C (_r: 54.4, Qf_r: 3448, and τ_f: 254.5 ppm/°C), and 5 wt% Li₂CO₃ sintered at 950 °C (_r: 43.7, Qf_r: 2501, and τ_f: −29.8 ppm/°C).     

Ti3AlC2掺杂SPS法制备Ti2AlC/TiAl复合材料的研究

通过2TiC-Ti-1.2Al体系的原位热压反应制备了Ti₃AlC₂陶瓷,然后以59.2Ti-30.8Al-10Ti₃AlC₂(wt%)为反应体系,采用放电等离子烧结技术制备出Ti₂AlC/TiAl基复合材料。借助XRD、SEM分析了产物的相组成和微观结构,并测量了其室温力学性能。结果表明：原位热压烧结产物由Ti₃AlC₂和TiC相组成,Ti₃AlC₂呈典型的层状结构,TiC颗粒分布在其间。SPS法制备的Ti₂AlC/TiAl基复合材料主要由TiAl、Ti₃Al和Ti₂AlC相组成,Ti₂AlC增强相主要分布于基体晶界处,表现为晶界/晶内强化作用。力学性能测试表明：Ti₂AlC/TiAl基复合材料的密度、维氏硬度、断裂韧性和抗弯强度分别为3.85 g/cm₃、5.37 GPa、7.17 MPa?m_1/2和494.85 MPa。     

Investigation of the microwave dielectric properties of Ca1−xMgxLa4Ti5O17 ceramics for application in coplanar patch antenna

In this paper, the dielectric properties of Ca_1−xMg_xLa₄Ti₅O₁₇ ceramics at microwave frequency have been studied. The diffraction peaks of Ca_(1−x)Mg_xLa₄Ti₅O₁₇ ceramics nearly unchanged with x increasing from 0 to 0.03. Similar X-ray diffraction peaks of Ca_0.99Mg_0.01La₄Ti₅O₁₇ ceramic were observed at different sintering temperatures. A maximum density of 5.3 g/cm³ can be obtained for Ca_0.99Mg_0.01La₄Ti₅O₁₇ ceramic sintered at 1500 °C for 4 h. A maximum dielectric constant (_r) and quality factor (Q × f) of Ca_0.99Mg_0.01La₄Ti₅O₁₇ ceramic sintered at 1500 °C for 4 h are 56.3 and 12,300 GHz (at 6.4 GHz), respectively. A near-zero temperature coefficient of resonant frequency (τ_f) of −9.6 ppm/°C can be obtained for Ca_0.99Mg_0.01La₄Ti₅O₁₇ ceramic sintered at 1500 °C for 4 h. The measurement results for the aperture-coupled coplanar patch antenna at 2.5 GHz are presented. With this technique, a 3.33% bandwidth (return loss <−10 dB) with a center frequency at approximately 2.5 GHz has been successfully achieved.     

Corrosion behavior of select MAX phases in NaOH, HCl and H2SO4

In this paper we report on the electrochemical corrosion of select MAX phases, namely Ti₂AlC, (Ti,Nb)₂AlC, V₂AlC, V₂GeC, Cr₂AlC, Ti₂AlN, Ti₄AlN₃, Ti₃SiC₂ and Ti₃GeC₂ in 1 M NaOH, 1 M HCl and 1 M H₂SO₄ solutions. Polarization characteristics recorded in 1 M NaOH show that V₂AlC, V₂GeC and Cr₂AlC undergo active dissolution at potentials more positive than the corrosion potential, while Ti₂AlC, (Ti,Nb)₂AlC, Ti₃SiC₂ and Ti₃GeC₂ passivate. In the 1 M HCl solutions, Ti₂AlC, V₂AlC and V₂GeC actively dissolve; Ti₃SiC₂ and Ti₃GeC₂ passivate. Depending on potential, (Ti,Nb)₂AlC and Cr₂AlC showed trans-passive behavior. In 1 M H₂SO₄ solutions, Ti₂AlC, (Ti,Nb)₂AlC, Ti₃SiC₂ and Ti₃GeC₂ passivate, V₂AlC and V₂GeC show active dissolution, while Cr₂AlC exhibits trans-passive behavior. Ti₂AlN and Ti₄AlN₃ were passive in all solutions except in 1 M HCl, where Ti₂AlN showed trans-passive behavior. Given that the corrosion behavior of (Ti,Nb)₂AlC is unlike either Ti or Nb, the behavior of the former cannot be predicted from that of the latter.     

Improving the surface hardness and wear resistance of Ti3SiC2 by boronizing treatment

In order to modify surface properties of Ti₃SiC₂, boronizing was carried out through powder pack cementation in the 1100-1400 °C temperature range. After boronizing treatment, one mixture layer, composed of TiB₂ and β-SiC, forms on the surface of Ti₃SiC₂. The growth of the coating is processed by inward diffusion of boron and obeys a linear rule. The boronizing increases the hardness of Ti₃SiC₂ from 3.7 GPa to a maximal 9.3 GPa and also significantly improves its wear resistance.     

Synthesis of Ti3SiC2 by infiltration of molten Si

High-purity Ti₃SiC₂ compounds have been fabricated by infiltration of molten Si into a precursor, a partially sintered TiC_x (x = 0.67) preform. The Si source and the TiC_x preform were placed side by side on carbon cloth, and the system was heated to 1550 °C. Molten Si infiltrated the preform through the carbon cloth, and a direct reaction between TiC_x and molten Si immediately occurred at the reaction temperature to yield pure Ti₃SiC₂. We could observe phase formation and the microstructure of the bulk products with time, which were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipped with energy-dispersive spectroscopy (EDS). Pure Ti₃SiC₂ compounds were formed on the exterior of the TiC_x preform at 1550 °C when the sintered TiC_x:Si ingot molar ratio was 3:1.4. At 1550 °C, no other minor phases were detected for any of the sintering time ranges.     

Rapid fabrication of the Ti3SiC2 bonded diamond composite by spark plasma sintering

A mixture of Ti/Si/TiC/diamond powders was employed to fabricate the Ti₃SiC₂ bonded diamond composite using the spark plasma sintering-reactive synthesis method. The addition of diamond does not inhibit the synthesis of Ti₃SiC₂ in the sintered product. In the matrix Ti₃SiC₂ grains developed lamellar morphology with an average length size of 5-10 μm. Ti₃SiC₂ matrix displays good pullout strength with diamond, and the Ti₃SiC₂ bonded diamond material exhibits good wear resistance.     

Effects of TiC and Al4C3 addition on combustion synthesis of Ti2AlC

Preparation of the ternary carbide Ti₂AlC was conducted by combustion synthesis in the mode of self-propagating high-temperature synthesis (SHS) from the elemental powder compacts of Ti:Al:C = 2:1:1, TiC-containing samples with TiC of 6.67–14.3 mol%, and Al₄C₃-containing samples with Al₄C₃ of 1.96–10 mol%. Effects of TiC and Al₄C₃ addition were studied on combustion characteristics and the degree of phase conversion. Due to the growth of laminated Ti₂AlC grains, the reactant compact was subjected to an axial elongation during the SHS process. Because the addition of TiC and Al₄C₃ led to a decrease in the reaction temperature, the flame-front propagation velocity was correspondingly reduced for the TiC- and Al₄C₃-containing samples when compared with the elemental reactants. Based upon the XRD analysis, formation of Ti₂AlC along with a secondary phase TiC was identified in the synthesized products. The grains of Ti₂AlC are typically plate-like with a size of 10–20 μm and several laminated Ti₂AlC grains form a layered structure. The content of Ti₂AlC yielded from the elemental powder compacts is about 85 wt%. The addition of TiC was found to facilitate the formation mechanism and therefore to enhance the extent of Ti₂AlC conversion approaching 90 wt%. As a result of the reduced exothermicity of the reaction, however, the content of Ti₂AlC decreased slightly in the products synthesized from the Al₄C₃-added samples.     

New dielectric material system of La(Mg1/2Ti1/2)O3–Ca0.6La0.8/3TiO3 for microwave applications

The microstructure and microwave dielectric properties of xLa(Mg_1/2Ti_1/2)O₃–(1 − x)Ca_0.6La_0.8/3TiO₃ ceramics system with ZnO additions (0.5 wt.%) investigated by the conventional solid-state route have been studied. Doping with ZnO (0.5 wt.%) can effectively promote the densification and the dielectric properties of xLa(Mg_1/2Ti_1/2)O₃–(1 − x)Ca_0.6La_0.8/3TiO₃ ceramics. 0.6La(Mg_1/2Ti_1/2)O₃–0.4Ca_0.6La_0.8/3TiO₃ ceramics with 0.5 wt.% ZnO addition possess a dielectric constant (_r) of 43.6, a Q × f value of 48,000 (at 8 GHz) and a temperature coefficient of resonant frequency (τ_f) of −1 ppm/°C sintering at 1475 °C. As the content of La(Mg_1/2Ti_1/2)O₃ increases, the highest Q × f value of 62,900 (GHz) for x = 0.8 is achieved at the sintering temperature 1475 °C. A parallel-coupled line band-pass filter is designed and simulated using the proposed dielectric to study its performance.     

Enhanced superconducting properties of bulk MgB2 prepared by in situ Powder-In-Sealed-Tube method

A systematic study on the superconducting properties of polycrystalline MgB₂ synthesized by in situ Powder-In-Sealed-Tube technique is carried out at different temperatures (750–900 °C). Both XRD and SEM results show well-crystallized MgB₂ grains in all the samples and grain size is found to be increasing with the sintering temperature. Sharp superconducting transitions are observed for all samples, irrespective of sintering temperatures, which implies the high degree phase purity and homogeneity of MgB₂ formed, while J_C(H) plot gives sample dependent critical current density. The samples heat treated at relatively low temperatures show enhanced flux pinning and hence improved J_C(H) performance. The reduced grain size and hence increased density of grain boundary pinning centers of MgB₂ bulks synthesized at low temperature are mainly responsible for the enhanced flux pinning and J_C.     

Conductivity of a new pyrophosphate Sn0.9Sc0.1(P2O7)1−δ prepared by an aqueous solution method

New pyrophosphate Sn_0.9Sc_0.1(P₂O₇)_1−δ was prepared by an aqueous solution method. The structure and conductivity of Sn_0.9Sc_0.1(P₂O₇)_1−δ have been investigated. XRD analysis indicates that Sn_0.9Sc_0.1(P₂O₇)_1−δ exhibits a 3 × 3 × 3 super structure. It was found that Sn_0.9Sc_0.1(P₂O₇)_1−δ prepared by an aqueous method is not conductive. The total conductivity of Sn_0.9Sc_0.1(P₂O₇)_1−δ in open air is 2.35 × 10⁻⁶ and 2.82 × 10⁻⁹ S/cm at 900 and 400 °C respectively. In wet air, the total conductivity is about two orders of magnitude higher (8.1 × 10⁻⁷ S/cm at 400 °C) than in open air indicating some proton conduction. SnP₂O₇ and Sn_0.92In_0.08(P₂O₇)_1−δ prepared by an acidic method were reported fairly conductive but prepared by similar solution methods are not conductive. Therefore, the conductivity of SnP₂O₇-based materials might be related to the synthetic history. The possible conduction mechanism of SnP₂O₇-based materials has been discussed in detail.     

Combustion synthesis of Ti3Si1−xAlxC2 solid solutions from TiC-, SiC-, and Al4C3-containing powder compacts

Preparation of the Ti₃Si_1−xAl_xC₂ solid solution with x = 0.2-0.8 was investigated by self-propagating high-temperature synthesis (SHS) using TiC-, SiC-, and Al₄C₃-containing powder compacts. Due to the variation of reaction exothermicity with sample stoichiometry, the combustion temperature and reaction front velocity decreased with increasing Al content of Ti₃Si_1−xAl_xC₂ for the TiC- and Al₄C₃-added samples, but increased for the samples with SiC. In contrast to the formation of Ti₃(Si,Al)C₂ as the dominant phase for the TiC- and SiC-added samples, TiC was identified as the major constituent in the final products of samples adopting Al₄C₃. In addition, the evolution of Ti₃(Si,Al)C₂ was improved by increasing the Al content of the TiC- and SiC-added powder compacts, but deteriorated considerably upon the increase of Al₄C₃ in the Al₄C₃-containing sample.     

Thermo-physical and thermal cycling properties of plasma-sprayed BaLa2Ti3O10 coating as potential thermal barrier materials

Increased turbine inlet temperature in advanced turbines has promoted the development of thermal barrier coating (TBC) materials with high-temperature capability. In this paper, BaLa₂Ti₃O₁₀ (BLT) was produced by solid-state reaction of BaCO₃, TiO₂ and La₂O₃ at 1500 °C for 48 h. BLT showed phase stability between room temperature and 1400 °C. BLT revealed a linearly increasing thermal expansion coefficient with increasing temperature up to 1200 °C and the coefficients of thermal expansion (CTEs) are in the range of 1 × 10^− 5–12.5 × 10^− 6 K^− 1, which are comparable to those of 7YSZ. BLT coatings with stoichiometric composition were produced by atmospheric plasma spraying. The coating contained segmentation cracks and had a porosity of around 13%. The microhardness for the BLT coating is 3.9–4.5 GPa. The thermo-physical properties of the sprayed coating were investigated. The thermal conductivity at 1200 °C is about 0.7 W/mK, exhibiting a very promising potential in improving the thermal insulation property of TBC. Thermal cycling result showed that the BLT TBC had a lifetime of more than 1100 cycles of about 200 h at 1100 °C. The failure of the coating occurred by cracking at the thermally grown oxide (TGO) layer due to severe oxidation of bond coat. Based on the above merits, BLT could be considered as a promising material for TBC applications.     

Effect of sintering on microstructure and mechanical properties of nano-TiO2 dispersed Al65Cu20Ti15 amorphous/nanocrystalline matrix composite

Mechanically alloyed Al₆₅Cu₂₀Ti₁₅ amorphous alloy powder with or without 10 wt% nano-TiO₂ dispersion was consolidated by isothermal spark plasma sintering in the range 200–500 °C with pressure up to 50 MPa. Selected samples were separately cold compacted with 50 MPa pressure and sintered at 500 °C using controlled atmosphere resistance and microwave heating furnaces. Phase and microstructural evolution at appropriate stages of mechanical alloying/blending and sintering was monitored by X-ray diffraction and scanning and transmission electron microscopy. Measurement and comparison of relevant properties (density/porosity, microhardness and yield strength) of the sintered compacts suggest that spark plasma sintering is the most appropriate technique for developing nano-TiO₂ dispersed amorphous/nanocrystalline Al₆₅Cu₂₀Ti₁₅ matrix composite for structural application.     

Synthesis and crystal structure of a new calcium borate, CaB6O10

A new calcium borate, CaB₆O₁₀, has been prepared by solid-state reactions at temperature below 750 °C. The single-crystal X-ray structural analysis showed that CaB₆O₁₀ crystallizes in the monoclinic space group P2₁/c with a = 9.799(1) Å, b = 8.705(1) Å, c = 9.067(1) Å, β = 116.65(1)°, Z = 4. It represents a new structure type in which two [B₃O₇]⁵⁻ triborate groups are bridged by one oxygen atom to form a [B₆O₁₃]⁸⁻ group that is further condensed into a 3D network, with the shorthand notation 6: ∞³[2 × (3:2Δ + T)]. The 3D network affords intersecting open channels running parallel to three crystallographically axis directions, where Ca²⁺ cations reside. The IR spectrum further confirms the presence of both BO₃ and BO₄ groups.     

Low temperature sintering and properties of CaO–B2O3–SiO2 system glass ceramics for LTCC applications

The P₂O₅ + ZnO, ZrO₂ + TiO₂, B₂O₃ and a low-melting-point CaO–B₂O₃–SiO₂ glass (LG) are selected as the sintering additives, and the effect of their additions on the microwave dielectric properties, mechanical properties and microstructures of CaO–B₂O₃–SiO₂ system glass ceramics is investigated. It is found that the sintering temperature of pure CBS glass is higher than 950 °C and the sintering range is about 10 °C. With the above additions, the glass ceramics can be sintered between 820 °C and 900 °C. The dielectric properties of the samples are dependent on the additions, densification and microstructures of sintered bodies. The major phases of this material are CaSiO₃, CaB₂O₄ and SiO₂. With 10 wt% B₂O₃ and LG glass additions, the CBS glass ceramics have better mechanical properties, but worse dielectric properties. The _r values of 6.51 and 7.07, the tan δ values of 0.0029 and 0.0019 at 10 GHz, are obtained for the CBS glass ceramics sintered at 860 °C with 2 wt% P₂O₅ + 2 wt% ZnO and 2 wt% ZrO₂ + 2 wt% TiO₂ additions, respectively. This material is suitable to be used as the LTCC material for the application in wireless communications.     

Role of nano-WC addition on microstructural,mechanical and thermal characteristics of TiC–SiCw composites

In this research, various amounts of nano-sized tungsten carbide (WC_n: 0, 1.5, and 3 wt%) were added to TiC-10 vol% SiC_w system. All samples were sintered at 1900 °C under an external pressure of 40 MPa for 7 min by spark plasma sintering (SPS) procedure. Microstructural, thermodynamical, and XRD evaluations revealed the formation of non-stoichiometric TiC_x, in-situ TiC, SiC, and WSi₂. The carbon exited the TiC lattice owing to the formation of non-stoichiometric TiC_x precipitated at the grain boundaries. Although introducing 1.5 wt% WC_n enhanced the relative density of TiC-SiC_w (98.7%) by around 0.7%, further addition of this sintering aid had a destructive impact. The addition of WC_n decreased both hardness and flexural strength of the specimens, and the poorest values (11.6 GPa and 368 MPa, respectively) were recorded for TiC-10 vol% SiC_w-3 wt% WC_n. The highest thermal conductivity (24.3 W/m.K) was obtained by the addition of 1.5 wt% WC_n.     

Synthesis of Ti3SiC2 bulks by infiltration method

T₃SiC₂ bulks have been synthesized by infiltrating Si liquid into porous precursor pellets composed of solid TiC and Ti powders. Silicon pellets were placed at the bottom of the precursor pellets as the liquid source. The starting compositions can be represented by the formula 2TiC + Ti + xSi, where x = 1.0, 1.2, 1.5 and 1.8, respectively. The phase formation and microstructure of the bulks were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipped with energy-dispersive spectroscopy (EDS) system. The results demonstrated that the TiC/Ti precursor pellet could only react with Si completely when the x value is 1.8. Impurities SiC, Ti-Si binary compounds and Ti₈C₅ appeared along the silicon diffusion direction. It is found that the compositions of impurities strongly depended on the Si-concentration. Reaction mechanism of this Ti₃SiC₂ infiltration synthesis has also been discussed based on the Si-concentration changes on the diffusion path.