Preparation of β-Sialon/ZrN bonded corundum composites from zircon by nitridation reaction sintering process

β-Sialon/ZrN bonded corundum composites were synthesized using fused white corundum,alumina micro powder,zircon and carbon black by nitridation reaction sintering process. Phase composition and microstructure of the synthesized composites were investigated by X-ray powder diffraction and scanning electronic microscope,and the formation process of the composites was discussed. The results show that the composites with different compositions can be obtained by controlling the heating temperature and contents of zircon and carbon black. The proper temperature to synthesize the composites is 1773 K.

Preparation of Gd_2O_2S:Pr Scintillation Ceramics by Pressureless Reaction Sintering Method

Fabrication of Gd2O2S：Pr scintillation ceramics by 2Gd2O3.（Gd,Pr）2（SO4）3.mH2O precursor was made Gd2O3, Pr6O11 and H2SO4 as the starting materials pressureless reaction sintering was investigated. The by hydrothermal reaction using commercially available Then single phase Gd2O2SO4：Pr powder was obtained by calcining the precursor at 750℃ for 2 h. The Gd2O2SO4：Pr powder compacts can be sintered to single phase Gd2O2S：Pr ceramics with a relative density of 99% and mean grain size of 30um at 1750℃ for 2 h in flowing hydrogen atmosphere. Densification and microstructural development of the Gd2O2S：Pr ceramics were examined. Luminescence spectra of the Gd2O2S：Pr ceramic under 309 nm UV excitation and X-ray excitation show a green emission at 511 nm as the most prominent peak, which corresponds to the ^3p0-3H4 transition of Pr^3＋ ions.

Thermo-mechanical properties of mullite–zirconia composites derived from reaction sintering of zircon and sillimanite beach sand: Effect of CaO

Mullite–zirconia composites containing 20% zirconia（mass fraction） were prepared by reaction sintering route utilizing Indian coastal zircon flour and sillimanite beach sand. 4%-12% of CaO（mole fraction） with respect to zirconia was used as additive. The effect of additive on densification, microstructure as well as various mechanical and thermo-mechanical properties was studied. Incorporation of CaO reduced the densification temperature of the composites to 1550 ℃ compared to 1600 ℃（for CaO free samples）. CaO formed small amount of liquid phase（calcium aluminosilicate）, which facilitated sintering. Average grain size of the composites decreased up to 4% CaO addition, afterwards grain size increased with further addition of CaO. Samples with 4% CaO exhibited ～225 MPa of flexural strength, ～6 MPa·m^1/2 of fracture toughness and significant improvement in thermal shock resistance. CaO stabilized the tetragonal zirconia phase and thus improved the mechanical properties.

Reaction Sintering of β-sialon/Al_2O_ 3/SiO_2 Mixtures in Flowing Nitrogen at High Temperatures

β-sialon/alumina/silica mixtures were sintered in flowing nitrogen at 1500℃ and 1600℃ respectively. The sintering properties and morphology of samples were investigated by SEM, EDS and XRD. Results show that sintered properties of the samples are influenced by soaking temperatures and compositions. Bulk densities of samples are increased with the increase of the soaking temperature, whereas the apparent porosities are decreased. Mass loss of the sintered samples at 1500℃ is lower than that at 1600℃, but all the mass loss remains approximately constant with the increase of sialon content. From the point of thermodynamic analysis, Complex chemical reactions take place in samples during sintering process and the volatile of SiO (g) is responsible for the mass loss of samples. Compared to cross section microstructure of β-sialon/Al_ 2O_ 3/SiO_ 2 mixtures sintered in coke powder bed consisting of the dense center with well-developed column of sialon phase, the transitional part with needle like grain nitrogen-containing phase and the loose part with short granular Al_2O_3 phase, those of mixtures sintered in flowing nitrogen is made of well-developed sialon in dense center and slightly loose part with sialon debris.

Synthesis of O’-SiAlON-BN Composite by Reaction Sintering

By using micron α-SisN4, SiO2, Al2O3 and h-BN as starting materials, O＇ -SiAION-BN （ Si2-z AlzO1 ＋z N2-z, z= 0. 3） composite was synthesized by reaction sintering. According to theoretical proportion ratio： n（ SiO2）/n（ α-Si3N4） = 1, the effects of two sintering aid composites, Y2O3 ＋ B2O3 and Y2O3 ＋ TiO2 at 1700℃ for 2h, were studied. The results indicate that Y2 O3 ＋ TiO2 as sintering aid can accelerate reaction sintering of O＇ -SiAION-BN more effectively than Y2O3 ＋ B2O3, and the relative density of the composites declined with the increase of BN addition （10%, 20% and 30% respectively）; XRD analysis found that excessive β-Si3N4 existed in the O＇ -SiAION-BN composite. Therefore, in order to get more pure O＇ -SiAION and BN phases in the composites ore SiO2 is needed. When Y2O3 ＋ TiO2 was used as sintering aid and addition of BN was 10%, the result of cross experiment on condition of A- n（SiO2）/n（α-Si3N4） was 1.05, 1.1 and 1.2; B-- addition of sintering aid was 2%, 4% and 6% ; C-- firing temperature was 1600℃, 1650℃ and 1700℃ ; D--soaking time was 1h, 2h and 3h, shows that the sintering properties were influenced by factors of firing temperature, soaking time, addition of sintering aid and n（ SiO2 ）/n（α-SisN4） in order of importance. In addition, the technical parameter A s B 3 C s D3 can achieve the highest relative density. Besides, using Pattern Recognition method, the optimized parameter range to form pure O＇ -SiAION and BN without β-Si3N4 remained was determined as Y 〉 1024X^2 - 230. 400X ＋ 11.088 （ X = 0. 9999A -0. 0006C - 0. 0163D, Y = 0. 0163A ＋ 0. 009B -0. 0014C ＋0. 9999D）.

Preparation and sintering properties of zirconia-mullite-corundum composites using fly ash and zircon

Zirconia-mullite-corundum composites were successfully prepared from fly ash,zircon and alumina powder by a reaction sintering process.The phase and microstructure evolutions of the composite synthesized at desired temperatures of 1 400,1 500 and 1 600°C for 4 h were characterized by X-ray diffractometry and scanning electronic microscopy,respectively.The influences of sintering temperature on shrinkage ratio,apparent porosity and bulk density of the synthesized composite were investigated.The formation process of the composites was discussed in detail.The results show that the zirconia-mullite-corundum composites with good sintering properties can be prepared at 1 600°C for 4 h.Zirconia particles can be homogeneously distributed in mullite matrix,and the zirconia particles are around 5μm.The formation process of zirconia-mullite-corundum composites consists of decomposition of zircon and mullitization process.

Reaction Mechanism and Microstructure Evolution of Reaction Sintered h-BN

Hexagonal boron nitride ceramic（h-BN） based on the nitridation of B powders was obtained by reaction sintering method. The effects of sintering temperature on the mechanical properties and microstructure of the resultant products were investigated and the reaction mechanism was discussed. Results showed that the reaction between B and N2 occurred vigorously at temperatures ranging from 1 000 ℃ to 1 300 ℃, which resulted in the generation of t-BN. When the temperature exceeded 1 450 ℃, transformation from t-BN to h-BN began to occur. As the sintering temperature increased, the spherical particles of t-BN gradually transformed into fine sheet particles of h-BN. These particles subsequently displayed a compact arrangement to achieve a more uniform microstructure, thereby increasing the strength.

Microstructure and mechanical properties of reaction-bonded B_(4)C–SiC composites

Reaction-bonded B_(4)C–SiC composites are highly promising materials for numerous advanced technological applications.However,their microstructure evolution mechanism remains unclear.Herein,B_(4)C–SiC composites were fabricated through the Si-melt infiltration process.The influences of the sintering time and the B_(4)C content on the mechanical properties,microstructure,and phase evolution were investigated.X-ray diffraction results showed the presence of SiC,boron silicon,boron silicon carbide,and boron carbide.Scanning electron microscopy results showed that with the increase in the boron carbide content,the Si content decreased and the unreacted B_(4)C amount increased when the sintering temperature reached 1650°C and the sintering time reached 1 h.The unreacted B_(4)C diminished with increasing sintering time and temperature when B_(4)C content was lower than 35wt%.Further microstructure analysis showed a transition area between B_(4)C and Si,with the C content marginally higher than in the Si area.This indicates that after the silicon infiltration,the diffusion mechanism was the primary sintering mechanism of the composites.As the diffusion process progressed,the hardness increased.The maximum values of the Vickers hardness,flexural strength,and fracture toughness of the reaction-bonded B_(4)C–SiC ceramic composite with 12wt%B_(4)C content sintered at 1600°C for 0.5 h were about HV 2400,330 MPa,and 5.2 MPa·m^(0.5),respectively.

Effects of the original state of sodium-based additives on microstructure,surface characteristics and filtration performance of SiC membranes

Sodium-contained compounds are promising sintering additives for the low-temperature preparation of reaction bonded SiC membranes.Although sodium-based sintering additives in various original states were attempted,their effects on microstructure and surface properties have rarely been studied.In this work,three types of sodium-based additives,including solid-state NaA zeolite residue(NaA)and liquidstate dodecylbenzene sulfonate(SDBS)and water glass(WG),were separately adopted to prepare SiC membranes,and the microstructure,surface characteristics and filtration performance of these SiC membranes were comparatively studied.Results showed that the SiC membranes prepared with liquid-state SDBS and WG(S-SDBS and S-WG)showed lower open porosity yet higher bending strength compared to those prepared with solid-state NaA(S-NaA).The observed differences in bending strength were further interpreted by analyzing the reaction process of each sintering additive and the composition of the bonding phase in the reaction bonded SiC membranes.Meanwhile,the microstructural differentiation was correlated to the original state of the additives.In addition,their surface characteristics and filtration performance for oil-in-water emulsion were examined and correlated to the membrane microstructure.The S-NaA samples showed higher hydrophilicity,lower surface roughness(1.80μm)and higher rejection ratio(99.99%)in O/W emulsion separation than those of S-WG and S-SDBS.This can be attributed to the smaller mean pore size and higher open porosity,resulting from the originally solid-state NaA additives.Therefore,this work revealed the comprehensive effects of original state of sintering additives on the prepared SiC membranes,which could be helpful for the application-oriented fabrication by choosing additives in suitable state.

Effect of Si_3N_4 Addition on the Mechanical Properties, Microstructures, and Wear Resistance of Ti-6Al-4V Alloy

In order to improve the wear resistance of Ti-6Al-4V, different amounts of Si3N4 powder were added into the alloy powder and sintered at 1250℃. Porous titanium alloy with higher wear resistance was successfully fabricated. At sintering temperature, reaction took place and a new hard phase of Ti5Si3 formed. The mechanical properties of the fabricated alloys with different amounts of Si3N4 addition were investigated. The hardness of Ti-6Al-4V, which is the index of wear resistance, was increased by the addition of Si3N4. Amounts of Si3N4 addition have very significant influences on hardness and compressive strength. In present study,titanium alloy with 5 wt pct Si3N4 addition has 62% microhardness and 45% overall bulk hardness increase,respectively. In contrast, it has a 16.4% strength reduction. Wear resistance was evaluated by the weight loss during wear test. A new phase of Ti5Si3 was detected by electron probe microanalyzer （EPMA） and X-ray diffraction （XRD） method. The original Si3N4 decomposed during sintering and transformed into titanium silicide. Porous structure was achieved due to the sintering reaction.

Microstructure and Temperature Distribution in ZnAl_2O_4 Sintered Body by Pulse Electric Current

Microstructure of reaction sintering of ZnAl2O4 at 1500℃ by hot-pressing(HP) and pulse electric current was investigated. The results indicated that the existed cracks in sintered body were caused by structure mismatch. It is the evidence that periodical temperature field existed during pulse electric current sintering of nonconductive materials. The distance between high temperature areas was related to die diameter.

Reactive sintering of B4C-TaB2 ceramics via carbide boronizing:Reaction process, microstructure and mechanical properties

Carbide boronizing is a promising approach to obtain fine grained boron carbide based ceramics with improved mechanical properties. In this work, reaction process, microstructural characteristics and mechanical properties of BxC-TaB2(x = 3.7, 4.9, 7.1) ceramics were comprehensively investigated via this method. Dense BxC-TaB2 ceramics with refined microstructure were obtained from submicro tantalum carbide and boron powder mixtures at 1800℃/50 MPa/5 min by spark plasma sintering. The stoichiometry of boron carbide was determined from lattice parameters and Raman shift. It was found that uniformly distributed TaB2 grains in the BxC matrix is favor of the densification process and restricting grain growth.Besides, planar defects with high density were observed from the as-formed B7.1 C grains and transient stress was considered to contribute to the densification involved with plastic deformation. Microstructural observations indicate the dissolution of oxygen in the TaB2 lattice and most of the B7.1 C/TaB2 phase boundaries were clean. Owing to the highly faulted structure and finer grain size, as-obtained BxC-TaB2 ceramics exhibit high Vickers hardness(33.3–34.4 GPa at 9.8 N) and relatively high flexural strength ranging from 440 to 502 MPa.

Effects of BN content on the mechanical properties of nanocrystalline 3Y-TZP/Al_(2)O_(3)/BN dental ceramics

3Y-TZP/3wt%Al_(2)O_(3) powder was coated with varying amounts of BN using the urea and borate reaction sintering method,and then multiphase ceramics were prepared by hot pressing sintering.The micro-topography and the compositional analysis of synthesized ceramics were conducted through scanning electron microscopy,transmission electron microscopy and X-ray diffraction.A mechanical tester was used to analyze the Vickers hardness,fracture toughness,and bending strength of the synthesized ceramics.The results showed that the ceramic with a BN content of 12wt%showed the best processability,but had diminished mechanical properties(such as fracture toughness and bending strength).The ceramic with a BN content of 9wt%showed better processability than those with 3wt%and 6wt%BN.However,the fracture toughness was affected by the addition of 9wt%BN,making this ceramic only usable as a base material for a three-unit fixed bridge.In contrast,the ceramics with a BN content of 3wt%or 6wt%fulfilled the criteria for use in multi-unit restoration,but their low processability made them unsuitable for milling after sintering.

Sintering characteristics and microwave dielectric properties of 0.5Ca_(0.6)La_(0.267)TiO_3-0.5Ca(Mg_(1/3)Nb_(2/3))O_3 ceramics prepared by reaction-sintering process

0.5 Ca（0.6La0.267TiO3-0.5 Ca（Mg1/3Nb2/3）O3（5 CLT-5 CMN） ceramics were prepared by a reaction-sintering process and their sintering characteristics, microwave dielectric properties were investigated in detail.Without any calcination stage involved,a mixture of CaCO_3, La_2 O_3, TiO_2, MgO and Nb_2 O_5 was pressed and sintered directly. Pure phase 5 CLT-5 CMN ceramics with high density and dense microstructure can be obtained after sintered at 1400 ℃ for 4 h. Compared with those prepared by the conventional ceramic route, 5 CLT-5 CMN ceramics produced by the reaction-sintering process exhibit slightly higher dielectric constant and Q×f value. Fine microwave dielectric properties of ε_r= 56.4, Q×f= 48,550 GHz and T_f = ＋8.7 ppm/℃ for 5 CLT-5 CMN ceramics sintered at 1400 ℃ for 4 h are obtained, suggesting reactionsintering process is a simple and efficient method to produce pure phase 5 CLT-5 CMN ceramics as a potential candidate for the fabrication of microwave devices.

Thermodynamic Properties of Non-Oxide Composite Refractories

For initiative application of non-oxides in refractories, it is essential to study thermodynamic properties of non-oxides. The stability and stable order of non-ox- ides under oxidized atmosphere are analyzed firstly and then a new process, “converse reaction sintering”, is proposed. The results of study on oxidation mechanism of silicon and aluminum nitrides indicate that the gaseous suboxides can be produced observably when the oxygen partial pressure is lower than “conversion oxygen partial pressure”. The suboxides can be deposited near the surface of composite to become a compact layer. This causes the material possessing a performance of “self-impedient oxidation”. Metal Si and Al are the better additives for increasing the density and width of compact layer and increasing the ability of anti-oxidation and anti-corrosion. The study on Si3 N4-Al2O3, Si3N4-MgO, Si3 N4-SiC systems is also enumerated as examples in the paper. The experimental results show that the converse reaction sintering is able to make high performance composites and metal Si and Al not only can promote the sintering but also increase the density and width of compact layer.

Zero sintering-induced shrinkage of porous oxide ceramics

Porous oxide ceramics are widely used in extreme working conditions owing to their excellent resistance to high temperatures and corrosion.However,sintering is an inevitable process applied to ceramics,from the green body to the final product.The highly complex structures exacerbate the shrinkage-induced ir-regular deformation and crack formation in the sintering process.A pioneering approach is developed in this study to achieve zero shrinkage for porous alumina ceramics during multistep sintering,using a combination of active fillers-ZrAl 3 and Al 75 Si 25.The response surface method is used to optimize the material compositions and sintering process,to achieve shrinkages of less than 0.05%for the entire pro-cess.The sintering expansion mechanism is investigated by analyzing the pyrolysis and microstructures of samples at different temperatures.The combination of ZrAl 3 and Al 75 Si 25 can attain the continuous expansion of the matrix in a wide temperature range of 600-1400°C.Furthermore,typical alumina com-ponents are fabricated and used to verify the effectiveness of the proposed approach.Owing to shrinkage suppression,the profile deviation of the samples is less than 0.1 mm,and the proportion of microcracks is reduced by 97.8%.The suggested approach shows potential applications in near-net,low-defect fabrica-tion of complex fine ceramic components.

Comparative study of mechanical and wear behavior of Cu/WS_2 composites fabricated by spark plasma sintering and hot pressing

The mechanical and wear behavior of copper-tungsten disulfide（Cu/WS_2） composites fabricated by spark plasma sintering（SPS） and hot pressing（HP） was investigated, comparatively. Results indicated that the addition of lubricant WS_2 substantially reduced wear rate of the Cu matrix composites fabricated by SPS,and the optimum content of WS_2 is 20 wt% with regard to the wear behavior. However, it affected a little to the wear rate while dramatically decreased the friction coefficient of the composite fabricated by HP.This difference in friction behavior of the self-lubricating composites fabricated by the two techniques was closely related to their different mechanical properties. Severe interfacial reaction occurred during spark plasma sintering, leading to brittle phase formation at interface.

Porous high entropy(Zr0.2Hf0.2Ti0.2Nb0.2Ta0.2)B2: A novel strategy towards making ultrahigh temperature ceramics thermal insulating

Transition metal diborides based ultrahigh temperature ceramics(UHTCs) are characterized by high melting point, high strength and hardness, and high electrical and thermal conductivity. The high thermal conductivity arises from both electronic and phonon contributions. Thus electronic and phonon contributions must be controlled simultaneously in reducing the thermal conductivity of transition metal diborides. In high entropy(HE) materials, both electrons and phonons are scattered such that the thermal conductivity can significantly be reduced, which opens a new window to design novel insulating materials. Inspired by the high entropy effect, porous HE(Zr0.2Hf0.2Ti0.2Nb0.2Ta0.2)B2 is designed in this work as a new thermal insulting ultrahigh temperature material and is synthesized by an in-situ thermal borocarbon reduction/partial sintering process. The porous HE(Zr0.2Hf0.2Ti0.2Nb0.2Ta0.2)B2 possesses high porosity of 75.67%, pore size of 0.3–1.2 μm, homogeneous microstructure with small grain size of 400–800 nm, which results in low room temperature thermal diffusivity and thermal conductivity of 0.74 mm2 s^-1 and 0.51 W m^-1K^-1, respectively. In addition, it exhibits high compressive strength of3.93 MPa. The combination of these properties indicates that exploring porous high entropy ceramics such as porous HE(Zr0.2Hf0.2Ti0.2Nb0.2Ta0.2)B2 is a novel strategy in making UHTCs thermal insulating.

Recycling of High Ferrous Bauxite Reducing Slag for Synthesis of CaAl_2Si_2O_8-Al_2O_3-CaAl_(12)O_(19) Composite

CaAl2 Si2 O8- Al2 O3- CaAl12 O19） （CAS2- Al2 O3 -CA6 ） composite was synthesized through reaction sintering alumina and bauxite reducing slag. The CAS2-Al2 O3-CA5 composite was mainly composed of α-Al2O3 , CAS2 , and CA6. Gehlenite （Ca2 Al2 SiO7 , C2 AS） phase was effectively transformed to CASe and CA6 through high-temperature reaction sintering under weak oxidizing atmosphere at 1400 ℃for 4 h. SEM （scanning electron microscopy） and EDS （energy dispersive spectroscopy） analysis indicated that black and needle-shaped Al2O3, rhombic or irregular polygonal shaped FeAl2O4 , and glassy phase Ca2 Al2 SiO7 disappeared after the reaction sintering. The light gray and flaky hexagon crystals of CaAl12 O19 （10 μm） and the grainy particles of Al2O3 （2-7 μm） were observed in the CASe-Al2 O3-CA6 composite. The gray crystals of CASe act as the binding phase and are distributed around CA6 and Al2O3. CAS2-Al2O3-CA6 composite exhibits high refractoriness and service temperature, which are 1 650 ℃ and 1 450 ℃, respectively. Reaction sintering of alumina and bauxite reducing slag is a feasible method for the synthesis of CAS2-Al2 O3-CA6 composite.