Microstructure and Oxidation Behavior of ZrB_(2)-SiC Ceramics Fabricated by Tape Casting and Reactive Melt Infiltration

ZrB_(2)-based ceramics typically necessitate high temperature and pressure for sintering,whereas ZrB_(2)-SiC ceramics can be fabricated at 1500℃using the process of reactive melt infiltration with Si.In comparison to the conventional preparation method,reactive synthesis allows for the more facile production of ultra-high temperature ceramics with fine particle size and homogeneous composition.In this work,ZrSi_(2),B4C,and C were used as raw materials to prepare ZrB_(2)-SiC via combination of tape casting and reactive melt infiltration herein referred to as ZBC ceramics.Control sample of ZrB_(2)-SiC was also prepared using ZrB_(2) and SiC as raw materials through an identical process designated as ZS ceramics.Microscopic analysis of both ceramic groups revealed smaller and more uniformly distributed particles of the ZrB_(2) phase in ZBC ceramics compared to the larger particles in ZS ceramics.Both sets of ceramics underwent cyclic oxidation testing in the air at 1600℃for a cumulative duration of 5 cycles,each cycle lasting 2 h.Analysis of the oxidation behavior showed that both ZBC ceramics and ZS ceramics developed a glassy SiO_(2)-ZrO_(2) oxide layer on their surfaces during the oxidation.This layer severed as a barrier against oxygen.In ZBC ceramics,ZrO_(2) is finely distributed in SiO_(2),whereas in ZS ceramics,larger ZrO_(2) particles coexist with glassy SiO_(2).The surface oxide layer of ZBC ceramics maintains a dense structure because the well-dispersed ZrO_(2) increases the viscosity of glassy SiO_(2),preventing its crystallization during the cooling.Conversely,some SiO_(2) in the oxide layer of ZS ceramics may crystallize and form a eutectic with ZrO_(2),leading to the formation of ZrSiO_(4).This leads to cracking of the oxide layer due to differences in thermal expansion coefficients,weakening its barrier effect.An analysis of the oxidation resistance shows that ZBC ceramics exhibit less increase in oxide layer thickness and mass compared to ZS ceramics,suggesting superior oxidation resistance of ZBC ceramics.

Development and application of ferrite materials for low temperature co-fired ceramic technology

Development and application of ferrite materials for low temperature co-fired ceramic （LTCC） technology are dis- cussed, specifically addressing several typical ferrite materials such as M-type barium ferrite, NiCuZn ferrite, YIG ferrite, and lithium ferrite. In order to permit co-firing with a silver internal electrode in LTCC process, the sintering temperature of ferrite materials should be less than 950 ℃. These ferrite materials are research focuses and are applied in many ways in electronics.

The temperature-dependent fracture strength model for ultra-high temperature ceramics

Breaking down the entire structure of a material implies severing all the bonds between its atoms either by applying work or by heat transfer. Because bond-breaking is indifferent to either means, there is a kind of equivalence between heat energy and strain energy. Based on this equivalence, we assume the existence of a constant maximum storage of energy that includes both the strain energy and the corresponding equivalent heat energy. A temperaturedependent fracture strength model is then developed for ultrahigh temperature ceramics （UHTCs）. Model predictions for UHTCs, HfB2, TiC and ZrB2, are presented and compared with the experimental results. These predictions are found to be largely consistent with experimental results.

Fabrication and Thermal Structural Characteristics of Ultra-high Temperature Ceramic Struts in Scramjets

ZrB_2-SiC based ultra-high temperature ceramic（UHTC） struts were firstly proposed and fabricated with the potential application in the combustor of scramjets for fuel injection and flame-holding for their machinability and excellent oxidation/ablation resistance in the extreme harsh environment. The struts were machined with electrospark wire-electrode cutting techniques to form UHTC into the desired shape, and with laser drilling to drill tiny holes providing the channels for fuel injection. The integrated thermal-structural characteristic of the struts was evaluated in high-temperature combustion environment by the propane-oxygen free jet facility, subject to the heat flux of 1.5 MW/m^2 lasting for 300 seconds, and the struts maintained integrity during and after the first experiment. The experiments were repeated for verifying the reusability of the struts. Fracture occurred during the second repeated experiment with the crack propagating through the hole. Finite element analysis（FEA） was carried out to study the thermal stress distribution in the UHTC strut. The simulation results show a high thermal stress concentration occurs at the hole which is the crack initiation position. The phenomenon is in good agreement with the experimental results. The study shows that the thermal stress concentration is a practical key issue in the applications of the reusable UHTC strut for fuel injection structure in scramjets.

Effects of mechanical boundary conditions on thermal shock resistance of ultra-high temperature ceramics

The effects of mechanical boundary conditions, often encountered in thermalstructural engineering, on the thermal shock resistance（TSR） of ultra-high temperature ceramics（UHTCs） are studied by investigating the TSR of a UHTC plate with various types of constraints under the first, second, and third type of thermal boundary conditions. The TSR of UHTCs is strongly dependent on the heat transfer modes and severity of the thermal environments. Constraining the displacement of the lower surface in the thickness direction can significantly decrease the TSR of the UHTC plate, which is subject to the thermal shock at the upper surface. In contrast, the TSR of the UHTC plate with simply supported edges or clamped edges around the lower surface is much better.

Porous Ultra-high Temperature Ceramics for Ultra-high Temperature Thermal Protection System

Ultra-high temperature ceramics(UHTCs)are a family of borides,carbides and nitrides of transition elements such as hafnium,zirconium,tantalum and niobium.They exhibit the highest known melting points,good mechanical strength,good chemical and thermal stability under certain conditions.In last decade,researchers dedicated to characterize porous UHTCs aiming to develop novel thermal insulating materials that could withstand temperatures over 2000℃.In this article,the preparation and characteristics of porous UHTCs were reviewed.Dry processing,colloidal processing and solution processing routes have been used to prepare porous UHTCs with porosities ranging from 5%to 97%and pore sizes ranging from hundreds of nanometers to hundreds of micrometers.The obtained porous UHTCs are chemically and dimensionally stable at temperatures up to 2000℃ during static state high-temperature thermal aging.

Ceramic synthesis of 0.08BiGaO_3–0.90BaTiO_3–0.02LiNbO_3 under high pressure and high temperature

In this paper, the preparation of 0.08BiGaO3–0.90BaTiO3–0.02LiNbO3 is investigated at pressure 3.8 GPa and temperature 1100–1200？C. Experimental results indicate that not only is the sintered rate more effective, but also the sintered temperature is lower under high pressure and high temperature than those of under normal pressure. It is thought that the adscititious pressure plays the key role in this process, which is discussed in detail. The composition and the structure of the as-prepared samples are recorded by XRD patterns. The result shows that the phases of Ba TiO3, BaBiO（2.77）, and Ba2Bi4Ti5O（18） with piezoelectric ceramic performance generate in the sintered samples. Furthermore, the surface morphology characteristics of the typical samples are also investigated using a scanning electron microscope. It indicates that the grain size and surface structure of the samples are closely related to the sintering temperature and sintering time. It is hoped that this study can provide a new train of thought for the preparation of lead-free piezoelectric ceramics with excellent performance.

Realization of Low Temperature Densification of Nickelate Ceramics for MLCC Application

We report an improved method for the preparation of highly dense nickelate ceramics at relatively low temperature. It is found that the introduction of appropriate additives during the ball-milling process facilitates the formation of nickelate phase through solid state reaction. Moreover, although high-purity nickelate powders can only be obtained by calcining the mixture of starting materials at temperature higher than 1100 ℃. The adoption of powders calcined at 1000 ℃, rather than those calcined at higher temperature, is conductive to the low-temperature densification of nickelate ceramics, which is attributed to the small and dispersive particles, and the solid state reaction of the residual starting materials during sintering. Compared with the conventional process, the improved method can reduce the sintering temperature of nickelate ceramics by about 100 ℃ and decrease the grain size of the obtained ceramics, and therefore makes nickelate meet the fabrication requirements of multi-layer ceramic capacitors（MLCC）.

High speed laser cladding as a new approach to prepare ultra-high temperature ceramic coatings

Ultra-high temperature ceramic(UHTC)coatings are used to protect the hot-end components of hypervelocity aerocrafts from thermal ablation.This study provides a new approach to fabricate UHTC coatings with high speed laser cladding(HSLC)technology,and places more emphasis on investigating the formation mechanism,phase compositions,and mechanical properties of HSLC-UHTC coatings.Results show that a well-bonded interface between the coating and the tantalum alloy substrate can be formed.The coating is mainly composed of(Zr,Ta)C ceramic solid solution phase with a content of higher than 90% by volume and Ta(W)metal solid solution phase.At a relatively high powder feeding rate,the ZrC ceramic phase appears in the coating while a dense ZrC UHTC top layer with a thickness of up to~50μm is successfully fabricated.As for the mechanical properties of the HSLC coatings,the fracture toughness of the coating decreases with the increase of powder feeding rate.The increase of carbide solid solution phase can significantly improve the high temperature microhardness(552.7±1.8 HV0.5@1000℃).The innovative design of HSLC ZrC-based coatings on refractory alloys accomplishes continuous transitions on microstructure and properties from the substrate to the UHTC top layer,which is a very promising candidate scheme for thermal protection coating.

Electromagnetic Pump Made in a Hybrid Polymer-Ceramic Technology--Preliminary Results

This paper describes technology of the electromagnetic pump made in a hybrid polymer-ceramic technology. The pumping mechanism is realized with a mutual excitation between an electromagnetic coil and a neodymium magnet bonded to a flexible membrane. A PDMS （poly（dimethylsiloxane）） material was used to manufacture a membrane sufficient for the presented micropump. A fish trap construction is adapted to the ceramic technology. The bonding process of ceramics and polymer, using plasma oxidation method, is described as well. Moreover, a membrane deflection depending on magnet dimensions and applied voltage was measured.

Anisotropic thermal expansion in high-entropy multicomponent AlB_(2)-type diboride solid solutions

High-entropy(HE)ultra-high temperature ceramics have the chance to pave the way for future applications propelling technology advantages in the fields of energy conversion and extreme environmental shielding.Among others,HE diborides stand out owing to their intrinsic anisotropic layered structure and ability to withstand ultra-high temperatures.Herein,we employed in-situ high-resolution synchrotron diffraction over a plethora of multicomponent compositions,with four to seven transition metals,with the intent of understanding the thermal lattice expansion following different composition or synthesis process.As a result,we were able to control the average thermal expansion(TE)from 1.3×10^(−6)to 6.9×10^(−6)K^(−1)depending on the combination of metals,with a variation of in-plane to out-of-plane TE ratio ranging from 1.5 to 2.8.

Ultra-low temperature cofired ceramics based on Li_(2)WO_(4)as perspective substrate materials for terahertz frequencies

With the development of low dielectric permittivity materials having an ultra-low sintering temperature,testing their dielectric properties at terahertz frequencies suitable for 6G communication systems and implementation of the fabricated materials in ultra-low temperature cofired ceramics(ULTCC)were the main goals of the research.Lithium tungstate Li_(2)WO_(4)was synthesized by a solid-state reaction and used for the preparation of green tapes and test structures with cofired internal conductive layers,which are destined for substrates of microwave and submillimeter wave circuits.Sintering behavior,thermal effects,and mass changes of the green tapes during heating were studied using a hot-stage microscope,differential thermal analysis,and thermogravimetry.A single-phase composition was revealed for being undoped and doped with AlF3–CaB_(4)O_(7)ceramics.The impact of frequency,temperature,the addition of AlF3–CaB_(4)O_(7)and CuBi_(2)O_(4)dopants,and sintering temperature was the subject of in-depth characterization of dielectric properties in a terahertz region.A glass-free composition,ultra-low sintering temperature of 590–630℃,low roughness of the green tapes,dense microstructure,compatibility with Ag conductors,low and stable dielectric permittivity of 5.0–5.8 in a broad range of 0.2–2 THz,and low dielectric loss of 0.008–0.01 at 1 THz are the main advantages of the developed ULTCC substrates.

Thermal properties and high-temperature ablation of high-entropy (Ti_(0.25)V_(0.25)Zr_(0.25)Hf_(0.25))B_(2) coating on graphite substrate

An entropy-stabilized multicomponent ultrahigh-temperature ceramic(UHTC)coating,(Ti_(0.25)V_(0.25)Zr_(0.25)Hf_(0.25))B_(2),on a graphite substrate was in-situ sintered by spark plasma sintering(SPs)from constituent transition metal diboride powders.The(Ti_(0.25)V_(0.25)Zr_(0.25)Hf_(0.25))B_(2) coating had a hardness of 31.2±2.1 GPa and resisted 36.9 GPa of stress before delamination,as observed at the interface.The temperature-dependent thermal properties of the multicomponent diboride(Ti_(0.25)V_(0.25)Zr_(0.25)Hf_(0.25))B_(2) were obtained by molecular dynamics(MD)simulations driven by a machine learning force field(MLFF)trained on density functional theory(DFT)calculations.The thermal conductivity,density,heat capacity,and coefficient of thermal expansion obtained by the MD simulations were used in time-dependent thermal stress finite element model(FEM)simulations.The low thermal conductivity(<6.52 W·m^(-1)·K^(-1))of the multicomponent diboride coupled with its similar coefficient of thermal expansion to that of graphite indicated that stresses of less than 10 GPa were generated at the interface at high temperatures,and therefore,the coating was mechanically resistant to the thermal stress induced during ablation.Ablation experiments at 220℃ showed that the multicomponent diboride coating was resistant to thermal stresses with no visible cracking or delamination.The ablation mechanisms were mechanical denudation and evaporation of B_(2)O_(5) and light V-Ti oxides,which caused a decrease in the mass and thickness of the coating and resulted in mass and linear ablation rates of-0.51 mg·s^(-1) and -1.38μm·s^(-1),respectively,after 60 s.These findings demonstrated the thermal and mechanical stability of multicomponent entropy-stabilized diborides as coatings for carbon materials in engineering components under extreme environments.

Advanced research on the preparation and application of carbide ceramic fibers

Carbide ceramic fibers are of significant importance for application in the high-tech areas of advanced aircraft engines,aerospace vehicles,and the nuclear industry due to their excellent properties,such as high tensile strength and elastic modulus,excellent high-temperature resistance,and oxidation resistance.This paper reviews the preparation and application of different carbide ceramic fibers,including SiC fibers and transition metal carbide(e.g.,ZrC,HfC,and TaC)ceramic fibers.The preparation methods of carbide ceramic fibers are discussed in terms of different fiber diameters,represented by SiC fibers with variable weaving properties and functions due to their differences in diameter.Subsequently,the application of carbide ceramic fibers as high-temperature-resistant structural materials,catalyst carriers,sensors,and supercapacitors are summarized,and strategies for the future development of carbide ceramic fibers are proposed.This review aims to help researchers enhance their understanding of the preparation and utilization of carbide ceramic micro/nanofibers,advancing the development of high-performance carbide ceramic fibers.

Advances in ultra-high temperature ceramics,composites,and coatings

Ultra-high temperature ceramics(UHTCs)are generally referred to the carbides,nitrides,and borides of the transition metals,with the Group IVB compounds(Zr&Hf)and TaC as the main focus.The UHTCs are endowed with ultra-high melting points,excellent mechanical properties,and ablation resistance at elevated temperatures.These unique combinations of properties make them promising materials for extremely environmental structural applications in rocket and hypersonic vehicles,particularly nozzles,leading edges,and engine components,etc.In addition to bulk UHTCs,UHTC coatings and fiber reinforced UHTC composites are extensively developed and applied to avoid the intrinsic brittleness and poor thermal shock resistance of bulk ceramics.Recently,high-entropy UHTCs are developed rapidly and attract a lot of attention as an emerging direction for ultra-high temperature materials.This review presents the state of the art of processing approaches,microstructure design and properties of UHTCs from bulk materials to composites and coatings,as well as the future directions.

Design, Preparation and Properties of Carbon Fiber Reinforced Ultra-High Temperature Ceramic Composites for Aerospace Applications： A Review

Carbon fiber reinforced ultra-high temperature ceramic （UHTC） composites, consisting of carbon fibers embedded in a UHTC-matrix or a C-SiC-UHTC-matrix, are deemed as the most viable class of materials that can overcome the poor fracture toughness and thermal shock resistance of monolithic UHTC ma- terials, and also improve the oxidation resistance and ablation resistance of C/C and C/SiC composites at ultra-high temperatures. In this review, we summarize the different processing routes of the compos- ites based on the UHTC introducing methods, including chemical vapor infiltration/deposition （CVI/D）, precursor infiltration and pyrolysis （PIP）, reactive melt infiltration （RMI）, slurry infiltration （SI）. in-sito reaction, hot pressing （HP）, etc; and the advantages and drawbacks of each method are briefly dis- cussed. The carbon fiber reinforced UHTC composites can be highly tailorable materials in terms of fiber. interface, and matrix. From the perspective of service environmental applications for engine propul- sions anti hypersonic vehicles, the material designs （mainly focusing on the composition, quantity, structure of matrix, as well as the architecture of carbon fibers, UHTCs and pores）, their relevant processing routes and properties （emphasizing on the mechanical and ablation properties） are discussed in this paper. In addition, we propose a material architecture to realize the multi-function through changing the distri- bution of carbon fibers, UHTCs and pores, which will be an important issue for future development of carbon fiber reinforced UHTC composites.

Sol–gel derived porous ultra-high temperature ceramics

Ultra-high temperature ceramics(UHTCs)are considered as a family of nonmetallic and inorganic materials that have melting point over 3000℃.Chemically,nearly all UHTCs are borides,carbides,and nitrides of early transition metals(e.g.,Zr,Hf,Nb,Ta).Within the last two decades,except for the great achievements in the densification,microstructure tailoring,and mechanical property improvements of UHTCs,many methods have been established for the preparation of porous UHTCs,aiming to develop high-temperature resistant,sintering resistant,and lightweight materials that will withstand temperatures as high as 2000℃for long periods of time.Amongst the synthesis methods for porous UHTCs,sol–gel methods enable the preparation of porous UHTCs with pore sizes from 1 to 500μm and porosity within the range of 60%–95%at relatively low temperature.In this article,we review the currently available sol–gel methods for the preparation of porous UHTCs.Templating,foaming,and solvent evaporation methods are described and compared in terms of processing–microstructure relations.The properties and high temperature resistance of sol–gel derived porous UHTCs are discussed.Finally,directions to future investigations on the processing and applications of porous UHTCs are proposed.

Elucidating the role of preferential oxidation during ablation:Insights on the design and optimization of multicomponent ultra-high temperature ceramics

Multicomponent ultra-high temperature ceramics(UHTCs)are promising candidates for thermal protection materials(TPMs)used in aerospace field.However,finding out desirable compositions from an enormous number of possible compositions remains challenging.Here,through elucidating the role of preferential oxidation in ablation behavior of multicomponent UHTCs via the thermodynamic analysis and experimental verification,the correlation between the composition and ablation performance of multicomponent UHTCs was revealed from the aspect of thermodynamics.We found that the metal components in UHTCs can be thermodynamically divided into preferentially oxidized component(denoted as MP),which builds up a skeleton in oxide layer,and laggingly oxidized component(denoted as ML),which fills the oxide skeleton.Meanwhile,a thermodynamically driven gradient in the concentration of MP and ML forms in the oxide layer.Based on these findings,a strategy for pre-evaluating the ablation performance of multicomponent UHTCs was developed,which provides a preliminary basis for the composition design of multicomponent UHTCs.

Ablation behaviour of(Hf-Ta-Zr-Nb)C high entropy carbide ceramic at temperatures above 2100℃

The ablation behaviour of(Hf-Ta-Zr-Nb)C high entropy carbide(HEC4)was studied at temperatures above 2100℃using a plasma flame gun in air.The microstructures,phase and chemical compositions of the HEC4 samples were investigated after ablation.The mass ablation rate of the HEC4 samples increased with increasing ablation time from 0.21 mg cm^(−2)s^(−1)for 60 s to 0.45 mg cm^(−2)s^(−1)for 120 s.Com-pared to the mono-and binary carbides with commonly decreased mass and thickness after ablation,the HEC4 samples with the increased mass and thickness after ablation showed good resistance to mechan-ical scouring at such high temperatures and an oxidation controlled ablation mechanism.The ablation processes mainly include the oxidation of the carbide,the phase separation of the oxides,the melting of oxides,and the diffusion of oxygen.A composition gradient in the oxide layer was detected due to the different melting temperatures of the different oxides;Nb-Ta rich oxides formed at the front surface melted and became enriched at the edge of the samples,and the Zr-Hf rich oxides were enriched in the centre of the samples.The oxide layer with complex compositions and phase distributions acted as an effective ablation barrier.

Measurement of wireless pressure sensors fabricated in high temperature co-fired ceramic MEMS technology

High temperature co-fired ceramics(HTCCs) have wide applications with stable mechanical properties,but they have not yet been used to fabricate sensors.By introducing the wireless telemetric sensor system and ceramic structure embedding a pressure-deformable cavity,the designed sensors made from HTCC materials(zirconia and 96% alumina) are fabricated,and their capacities for the pressure measurement are tested using a wireless interrogation method.Using the fabricated sensor,a study is conducted to measure the atmospheric pressure in a sealed vessel.The experimental sensitivity of the device is 2 Hz/Pa of zirconia and 1.08 Hz/Pa of alumina below 0.5 MPa with a readout distance of 2.5 cm.The described sensor technology can be applied for monitoring of atmospheric pressure to evaluate important component parameters in harsh environments.