Fabrication of Ti2AlC by Spark Plasma Sintcring from Elemental Powders and Thermodynamics Analysis of Ti-M-C System

A ternary-layered carbide Ti2AlC material could be synthesized by spark plasma sintering（SPS） technology using elemental powder mixture of Ti, Al and active carbon. By means of XRD and SEM, phases were identified and microscopically evaluated. The experimental results show that the main phase in the product was fully crystallized Ti2AlC with small particle size when sintered at 1200℃. The synthesis temperature of SPS was 200-400℃ lower than that of hot pressing （HP） or hot isostatic pressing （HIP）. Through thermodynamics calculations, the mechanism of Ti2AlC was studied by calculating changes of Gibbs free energy of reactions.     

Development of Zr/ZrO<Subscript>2</Subscript> high temperature and high pressure sensors for <Emphasis Type="Italic">in-situ</Emphasis> measuring chemical parameters of deep-sea water

In order to in situ measure chemical parameters of deep-sea water and hydrothermal fluids at midocean ridge(MOR), it is necessary to use high temperature and high pressure chemical sensors.Developing new sensors is essential to measure in-situ pH and other chemical parameters(dissolved H2, dissolved H2S) of deep-sea water and hydrothermal fluids in a wide temperature range(2℃―400℃) at MOR vents.The YSZ(Yttria Stabilized Zirconia, 9%Y2O3) ceramic-based(HgO/Hg) chemical sensors possess excellent electrochemic...     

Eleetronie Structures and Bonding Properties of Ti2AlC and Ti3AlC2

The relation among electronic structure, chemical bond and property of Ti2AlC, Ti3AlC2 and doping Si into Ti2AlC was studied by density function and the discrete variation （DFT-DVM） method. After adding Si into Ti2AlC, the interaction between Si and Ti is weaker than that between Al and Ti, and the strengths of ionic and covalent bonds decrease both. The ionic and covalent bonds in Ti3AlC2, especially in Ti-Al, are stronger than those in Ti2AlC. Therefore, in synthesis of Ti2AlC, the addition of Si enhances the Ti3AlC2 content instead of Ti2AlC. The density of state （DOS） shows that there is mixed conductor characteristic in Ti2AlC and Ti3AlC2. The DOS of Ti3AlC2 is much like that of Ti2AlC. Ti2SiAl1-xC has more obvious tendency to form a semiconductor than Ti2AlC, which is seen from the obvious difference of partial DOS between Si and Al 3/7.     

Synthesis of high pure Ti3AlC2 and Ti2AlC powders from TiH2 powders as Ti source by tube furnace

Titanium aluminum carbide (Ti₃AlC₂ and Ti₂AlC) powders were synthesized from TiH₂ powders instead of Ti powders as Ti source by a tube furnace under argon atmosphere without preliminary dehydrogenation. 95 wt% pure Ti₃AlC₂ powders were synthesized from TiH₂/1.1Al/2TiC at 1 450 °C for 120 min. High-purity Ti₂AlC powders were also prepared from 3TiH₂/1.5Al/C and 2TiH₂/1.5Al/TiC powders at 1 400 °C for 120 min. The as-synthesized samples were porous and easy to be ground into powders. Sn or Si additives in starting materials increased the purity of synthesized Ti₃AlC₂ obviously and expanded the temperature range for the synthesis of Ti₃AlC₂. With Si or Sn as additives, high pure Ti₃AlC₂ was synthesized at 1 200 °C for 60 min from TiH₂/x Si/Al/2TiC and TiH₂/x Sn/Al/2TiC (x = 0.1, 0.2), respectively.     

Orientation of Bi<Subscript>3.2</Subscript>La<Subscript>0.8</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> ferroelectric thin films with different annealing schedules

Fatigue-free Bi_3.2La_0.8Ti₃O₁₂ ferroelectric thin films were successfully prepared on p-Si (100) substrates using metalorganic solution deposition process. The orientation and formation of 5-layers thin films were studied under different processing conditions using XRD. Experimental results indicate that increase in annealing time at 700 °C after preannealing for 10 min at 400 °C can remarkably increase (200)-orientation of the films derived from the precursor solutions with two contents of citric acid. Meanwhile, high content of citric acid increases the film thickness and is conducive to the a-orientation of the films with the preannealing, and low concentration of the solution is conducive to the c-orientation of the films without the preannealing.     

Microstructures and mechanical,electrical, high-temperature properties of Cu/Ti<Subscript>2</Subscript>AlC FGM fabricated by hot-pressing

The microstructure and the electrical, thermal, friction, and mechanical properties of Cu/Ti₂AlC fabricated by hot-pressing at 900 °C for 1 h were investigated in the present work. Microstructural observations have shown that the plate-like Ti₂AlC grains distribute irregularly in the network of Cu grains, and well-structured, crack-free bonds between the layers. With the increase in the content of Ti₂AlC from layer A to layer D, the electrical resistivity increases from 1.381×10^-7 Ω·m to 1.918 ×10^-7 Ω·m, the hardness increases from about 980.27 MPa to about 2196.01 MPa, and the friction coefficient from above 0.20 reduces to about 0.15. Oxidation rate increases with the increases of temperature. Exfoliation was obviously observed on the surface of oxidation layer A. The surface of layer D was still intact and the spalling and other defects were not found. The mass decreases in the acid solution, and increases in the alkaline solution. The largest corrosion rate is found in 6.5% HNO₃ or 4% NaOH solution.     

Preparation of TiAl/Ti2AlC Composites with Ti/Al/C Powders by In-situ Hot Pressing

TiAl/Ti2AlC composites were prepared by in-situ hot pressing of TilAl/C powders mixtures and sintered at different temperatures were investigated by X- ray diffraction （ XRD ） of samples. The reaction procedure of Ti-Al-C system could be divided into three stnges. Below 900℃ , Ti reacts with Al to form TiAl intermetallics ; above 900 ℃ , C reacts with remain Ti to form TiC triggered by the exothermal reaction of Ti and Al ; TiAl reacts with TiC to produce dense TiAl/Ti2AlC compasites.In the holding stage, ternary Ti2AlC develops to layered polycrystal and composites pyknosis in the meanwhile. The mechanism of synthesis and microstructure was especially discussed.     

Physical, antioxidant and thermal shock properties of Cu/Ti2AlC conductive composites

Cu/Ti₂AlC composites were fabricated by vacuum hot-pressing technique. Phase composition was analyzed by XRD and morphology of fracture was observed by SEM. Physical performance such as density, resistivity, hardness and friction coefficient with different volume fraction of Cu/Ti₂AlC composites were studied. When the content of Ti₂AlC increased from 10% to 70%, the relative density reduced from 99.38% to 90.56% and the resistivity increased significantly. Hardness reached the maximum value when Ti₂AlC was at 60% and friction coefficient declined with the increasing of Ti₂AlC. Cu/Ti₂AlC composites, showing good conductivity properties and friction performance. Oxidation resistance enhanced obviously with the content of Ti₂AlC increasing. Cu-60%Ti₂AlC sample possessed optimum thermal shock resistance, and no cracking was found at 600 °C cycled for 10 times and 900 °C cycled for 1 time.     

Low-temperature sintering and microwave dielectric properties of Ba<Subscript>2</Subscript>Ti<Subscript>3</Subscript>Nb<Subscript>4</Subscript>O<Subscript>18</Subscript> ceramics

The effects of CuO and H3BO3 additions on the low-temperature sintering,microstructure,and microwave dielectric properties of Ba2Ti3Nb4O18 ceramics were investigated.The addition of less amount of CuO (< 1 wt%) considerably facilitated the densification of Ba2Ti3Nb4O18 ceramics.Appropriate addition of H3BO3 (< 3.5 wt%) remarkably improved the microwave dielectric properties of ceramics.The addition of H3BO3 and CuO successfully reduced the sintering temperature of Ba2Ti3Nb4O18 ceramics from 1300 to 1050 ℃.B...     

Phase structure and electrical properties of La<Subscript>2</Subscript>O<Subscript>3</Subscript>-doped BiInO<Subscript>3</Subscript>-PbTiO<Subscript>3</Subscript> ceramics with high curie temperature

The phase structure and electrical properties of pure and La2O3-doped Bi-InO3-PbTiO3 （BI-PT） ceramics were studied respectively. In （1 -x）BI-xPT （x=0.72-0.80） ceramics, the stability of tetragonal phase increased with increasing x, and pure perovskite structure was obtained for x=-0.80 ceramics. The phase transition temperature range was between 575 ℃ and 600 ℃ for x=0.72-0.80 ceramics, higher than that of PT （-490 ℃）. The c/a ratio almost linearly decreased with increasing La2O3 content in x-0.80 ceramics. It is believed that Pb^2＋ vacancies were formed by La^3＋ substituting Pb^2＋ in La2O3-doped BI-PT ceramics. Tc shifted to lower temperature by 30 ℃/mol% La2O3. The maximum dielectric constant 8557 around 559 ℃ was exhibited in 0.5mol%-doped BI-0.80PT ceramics. La2O3-doped ceramics could be poled resulting from decreasing of c/a ratio and improving of dielectric loss and resistivity. The maximum piezoelectric coefficient d33 was 12 pC/N for 2mol%-doped BI-0.80PT ceramics.     

Structure and dielectric properties of ZnO and Nb<Subscript>2</Subscript>O<Subscript>5</Subscript> doped BaO-TiO<Subscript>2</Subscript> system microwave ceramics

The microwave dielectric properties and microstructure of BaTi4.3ZnyO9.6＋y ＋0.02 mol% SnO2＋0.01 mol% MnCO3＋x mol% Nb2O5（x=0-0.05, y=0-0.08） system ceramics were studied as a function of the amount of ZnO and Nb2O5 doped. Addition of （y=0-0.05） ZnO and （x=0-0.025） Nb2O5 enhanced the reactivity and decreased the sintering temperature effectively. It also increased the dielectric constant ε r and quality factor Q（=1/tan 8） of the system due to the substitution of Ti^4＋ ions with incorporating Zn^2＋and Nb^5＋ ions, which was analyzed by the reaction ZnO＋Nb2O5＋ 3 TiTxTi →ZnTi＋ 2NbTi＋3TiO2. When the system doped with （y=0.05） ZnO and （x=0.025） Nb205 were sintered at 1 160 ℃ for 6 h, the εr. Qf0 value and rfwere 36.5, 42 000 GHz, and＋1.8 ppm/℃, respectively, at 5 GHz.     

Dielectric properties of Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> ceramics by impedance spectroscopic method

Various lead-free ceramics have been investigated in search for new high-temperature dielectrics. In particular, Bi₄Ti₃O₁₂ is a type of ferroelectric ceramics, which is supposed to replace leadcontaining ceramics for its outstanding dielectric properties in the near future. Ferroelectric ceramics of Bi₄Ti₃O₁₂ made by conventional mixed oxide route have been studied by impedance spectroscopy in a wide range of temperature. X-ray diffraction patterns show that Bi₄Ti₃O₁₂ ceramics are a single-phase of ferroelectric Bi-layered perovskite structure whether it is calcined at 800 °C or after sintering production. This study focused on the effect of the grain size on the electric properties of BIT ceramics. The BIT ceramics with different grain sizes were prepared at different sintering temperatures. Grain becomes coarser with the sintering temperature increasing by 50 °C, relative permittivity and dielectric loss also change a lot. When sintered at 1 100 °C, r values peak can reach 205.40 at a frequency of 100 kHz, the minimum dielectric losses of four different frequencies make no difference, all close to 0.027. The values of E _a range from 0.52 to 0.68 eV. The dielectric properties of the sample sintered at 1 100 °C are relatively better than those of the other samples by analyzing the relationship of the grain, the internal stresses, the homogeneity and the dielectric properties. SEM can better explain the results of the dielectric spectrum at different sintering temperatures. The results show that Bi₄Ti₃O₁₂ ceramics are a kind of dielectrics. Thus, Bi₄Ti₃O₁₂ can be used in high-temperature capacitors and microwave ceramics.     

Flux pinning effect of cubic equiaxed morphology and its Ti stabilizing in Nb<Subscript>3</Subscript>Sn superconductors

Two sets of internal-Sn Nb3Sn superconducting strands were fabricated through RRP method, one with 2 wt% of Ti alloyed in Sn core and the other just pure Sn. Four reaction temperatures of 650℃, 675℃, 700℃ and 725℃ and 128 h duration were applied for A15 phase formation heat treatment after Cu-Sn alloying procedure of 210℃/50 h + 340℃/25 h. For the heat-treated coil samples, transport non-Cu JC was examined through standard 4-probe technique and phase microstructure was observed by means of Field Emission Sc...     

Preparation of Ti3SiC2 with Aluminum by Means of Spark Plasma Sintering

Polycrystalline bulk Ti3SiC2 material with a high purity and density was fabricated by spark plasma sintering from the elemental powder mixture with starting composition of Ti3Si3Si1-xAlxC2 , where x = 0. 05 -0.2. X-ray diffraction patterns and scanning electron microscopy photographs of the fully dense samples show that a proper addition of aluminum promotes the formation, and accelerates the crystal growth rate of Ti3SIC2, conse-quently results in a high purity of the prepared samples. The synthesized Ti3 SiC2 is in plane-shape with a size of about 10- 25μm in the elongated dimension. Solid solution of aluminum decreases the thermal stability of Ti3SiC2, and lowers the temperature of Ti3SiC2 decomposeing to be 1300 ℃ .     

Friction and wear properties of TiAl and Ti2AlN/TiAl composites at high temperature

The high-temperature friction and wear properties of TiAl alloys and Ti₂AlN/TiAl composites (TTC) in contact with nickel-based superalloy were studied. The results showed that, at 800 and 1 000 °C, the coefficient of the friction (COF) decreased with the increase of sliding velocity and the wear loss of the TTC decreased with the increase of volume fraction of Ti₂AlN. The wear mechanisms of the pairs are adhesive wear and the wear debris mainly comes from the contacting nickel-based superalloy. The intergranular fracture and the cracking of the phase boundary in the lamellar structure are the wear mode of TiAl alloy. The wear mode of TTC is phase boundary fracture and adhesive spalling. The abrasive resistance of TTC is slightly higher than that of TiAl alloy.     

Spark plasma sintering of undoped SnO<Subscript>2</Subscript> ceramics

Various parameters in spark plasma sintering(SPS),such as sintering temperature,holding time,heating rate,and pressure,were adopted to investigate their effects on the densification of pure SnO2 power.The obtained experimental data show that the SPS process enhances densification.The high-density undoped SnO2 ceramics (96.6% of theoretical) was obtained at much lower temperature (1000℃),within a much shorter time,compared to the conventional sintering process.The high-density undoped SnO2 ceramics (96.6% of theoretical) were obtained by SPS,under the condition of temperature:1000℃,pressure:40MPa,heating-rate:200℃/min,and holding time:3min     

Synthesis of ZrAlN coatings with thermal stability at high temperature

Dry machining will result in elevated temperatures at the tool surface (800—1000℃). So, coating materials that can provide protection for cutting tools at these temperatures are of great technological interests. ZrAlN coating is proposed to possess high-temperature stable structural and mechanical properties due to the addition of the alloying element. ZrAlN coatings were grown using a dc reactive magnetron sputtering. The XRD and nano indenter were employed to investigate the effects of reaction gas partial pressure and substrate bias on structural and mechanical properties, as well as high-temperature stability. The ZrAlN coating, when deposited under optimum conditions (-37 V substrate bias and 2×10-5 Pa N2 partial pressure), showed smooth surface with thermal stable hardness. Its internal stress was relaxed from 2.2 to 0.7 GPa after anneal- ing. Formation of Al2O3 and ZrO2 crystalline phases should be related to thermal stability of the coatings.     

Synthesis and structure of NaNbO<Subscript>3</Subscript> ceramic powders in ultrahigh pressure field

The NaNbO3 powders were synthesized and their crystal structure changes were analyzed by ultrahigh pressure up to 6 GPa. The results indicate that the pure NaNbO3 powders can be synthesized at 300℃ under a pressure of 4 GPa, to significantly restrain the Na element volatilization compared with the traditional synthesis method. It is found that the crystal structure of synthesized NaNbO3 changes from low symmetry to high symmetry with the increase of the pressure.     

In-situ TEM Study on Mierostruetural Evolution of Nanostruetured TiO2

The effect of electron beam on the microstructures and phase transformation of nanostructured TiO2 heat treated at various temperatures for different time was studied by in-situ TEM and SAED. Anatase ex-situ heated at 250℃ and 360℃ transformed to rutile while irradiated by the electron beam. With the increasing sizes and distribution of the powders on the amorphous carbon, the process of phase transformation by the electron beam was encumbered. These evolutions may be due to the changes of vacuum atmosphere and the properties of powders.     

Structure and properties of Mg-doped SrBi<Subscript>4</Subscript>Ti<Subscript>4</Subscript>O<Subscript>15</Subscript> Bi-layered compounds

The structure and properties of Mg-doped SrBi4Ti4O15（SBT） were dicussed. Mg substitution into SBT had two possibilities states with the dopant amount variety. Mg cation substituted mostly into Sr^2＋ and the amount proportion was 68.11%.Mg ion will substitute into Ti ion site in perovskite layer when the doping amount increases. Polarization increases sharply when x=0.1 and then decreases becauses of the domain pinning. The Curie temperature of Mg-doped SBT is about 300 ℃ and there is a broad diffuse phase transition near Tc with a flat peak near the Ta of SBT.