Effect of MgO particle size on the microstructure, mechanical properties and wear performance of ZTA-MgO ceramic cutting inserts

The mechanical properties, microstructure and wear performance of zirconia-toughened alumina (ZTA) cutting inserts with Magnesia (MgO) in different particle sizes as additives was investigated. The MgO particle sizes were varied from 80 nm to 7000 nm. The alumina (Al₂O₃), yittria stabilized zirconia (YSZ) and MgO powders were mixed, compacted and sintered at 1600 °C using the solid-state sintering method. The mechanical and physical properties of the samples such as wear resistance, Vickers hardness, fracture toughness, microstructure and density were analyzed. Commercially available stainless steel (316L) was used as the workpiece for the wear resistance study. It was observed that smaller MgO particle sizes induce better wear performance and mechanical properties for the cutting inserts. Wear resistance analysis showed that the cutting insert with nano-sized MgO (particle size 80 nm) had the lowest wear area of 0.019 mm². The same cutting insert also possessed the highest Vickers hardness value of 1740 Hv compared to the other samples. Furthermore, microstructural observations show that the Al₂O₃ grain size depends on the particle size of MgO, and is directly related to its hardness property.     

Synthesis and consolidation of TiN/TiB2 ceramic composites via reactive spark plasma sintering

The simultaneous synthesis and densification of TiN/TiB₂ ceramic composites via reactive spark plasma sintering (RSPS) was investigated. Different component ratios (TiH₂/BN (TiN, B)) and heating rates (112.5-300 °C/min) were used to initiate the chemical reaction for TiN/TiB₂ synthesis. The omit RSPS process was revealed to have three stages, which are described separately. The relationships between the RSPS conditions, the microstructure and the properties of sintered ceramic composites were established. A Vickers hardness of 16-25 GPa and a fracture toughness of 4-6.5 MPa m^1/2 were measured for various compositions. Sintered ceramic composites containing 36 wt% TiB₂ with the highest relative density of 97.4 ± 0.4% and an average grain size of 150-550 nm have been obtained.     

An evaluation of Al2O3-ZrO2 composites produced by coprecipitation method

The objective of this work is to produce Al₂O₃-ZrO₂ composite from nano-sized powders processed by coprecipitation method. Al₂O₃ and mixture of Al₂O₃ + 10 wt.% ZrO₂ precipitated successfully by chemical route from aluminum sulfate and zirconium sulfate were pressed under uniaxial compression of 170 MPa and sintered at 1600 °C for 1 h. SEM investigations revealed that, pure alumina sample has a microstructure with coarse grains which anisotropically grown up to 30-40 μm in size. In alumina-zirconia composite, the structure consists of very fine equiaxed grains of typically 2 μm in which zirconia precipitates were uniformly dispersed. By adding zirconia to alumina, hardness and indentation fracture toughness were increased from 11.6 GPa to 16.8 GPa and from 3.2 MPa m^1/2 to 4.9 MPa m^1/2, respectively. Improvement in fracture toughness was attributed to bridging effects of zirconia particles as well as transformation toughening.     

Bulk WC-Al2O3 composites prepared by spark plasma sintering

WC and WC-Al₂O₃ materials without metallic binder addition were densified by spark plasma sintering in the range of 1800-1900 °C. The densification behavior, phase constitution, microstructure and mechanical properties of pure WC and WC-Al₂O₃ composite were investigated. The addition of Al₂O₃ facilitates sintering and increases the fracture toughness of the composites to a certain extent. An interesting phenomenon is found that a proper content of Al₂O₃ additive helps to limit the formation of W₂C phase in sintered WC materials. The pure WC specimen possesses a hardness (HV₁₀) of 25.71 GPa, fracture toughness of 4.54 MPa·m^1/2, and transverse fracture strength of 862 MPa, while those of WC-6.8 vol.% Al₂O₃ composites are 24.48 GPa, 6.01 MPa·m^1/2, and 1245 MPa respectively. The higher fracture toughness and transverse fracture strength of WC-6.8 vol.% Al₂O₃ are thought to result from the reduction of W₂C phase, the crack-bridging by Al₂O₃ particles and the local change in fracture mode from intergranular to transgranular.     

Properties and fast low-temperature consolidation of nanocrystalline Ni-ZrO2 composites by high-frequency induction heated sintering

Nanopowders of Ni and ZrO₂ (11 nm and 90 nm, respectively) were synthesized from NiO and Zr by high energy ball milling. A highly dense nanostructured 2Ni-ZrO₂ composite was consolidated at low temperature by high-frequency induction heat sintering within 2 min of the mechanical synthesis of the powders (Ni-ZrO₂) with horizontal milled NiO + Zr powders under 500 MPa pressure. This process allows very quick densification to near theoretical density and prohibits grain growth in nano-structured materials. The grain sizes of Ni and ZrO₂ in the composite were calculated. Finally, the average hardness and fracture toughness values of nanostructured 2Ni-ZrO₂ composites were investigated.     

On the wide range of mechanical properties of ZTA and ATZ based dental ceramic composites by varying the Al2O3 and ZrO2 content

In this work the influence of pressureless sintering on the Vickers hardness and fracture toughness of ZrO₂ reinforced with Al₂O₃ particles (ATZ) and Al₂O₃ reinforced with ZrO₂ particles (ZTA) has been investigated. The ceramic composites were produced by means of uniaxial compacting at 50 MPa and the green compacts were heated to 1250 °C using a heating rate of 10 °C min⁻¹, then to 1500 °C at 6 °C min⁻¹ and maintained at this temperature during 2 h. After sintering, relative density over 94%, hardness values between 9.5 and 21.9 GPa, and fracture toughness as high as 3.6 MPa m^1/2 were obtained. The presence of TZ-3Y particles on the grain boundaries suggests that they inhibit notably the alumina grain growth. The grain sizes of pure Al₂O₃ and TZ-3Y as well as Al₂O₃ and TZ-3Y in the 20 wt% Al₂O₃+80 wt% TZ-3Y composite were 1.27 ± 0.51 μm, 0.57 ± 0.12 μm, 0.65 ± 0.19 μm and 0.41 ± 0.14 μm, respectively. The 20 wt% Al₂O₃ + 80 wt% ZrO₂ + 3 mol% Y₂O₃ (TZ-3Y) composite showed a hardness of 16.05 GPa and the maximum fracture toughness (7.44 MPa m^1/2) with an average grain size of 0.53 ± 0.17 μm. On the other side, the submicron grain size and residual porosity seem to be responsible for the high hardness and fracture toughness obtained. The reported values were higher than those obtained by other authors and are in concordance with international standards that could be suitable for dental applications.     

Compressive strength, hardness and fracture toughness of Al2O3 whiskers reinforced ZTA and ATZ nanocomposites: Weibull analysis

The aim of this investigation was to study the variability in compressive strength, fracture toughness and microhardness applying the well-known Weibull statistics and to be able to provide a wide spectrum of mechanical properties in Al₂O₃ whisker reinforced alumina toughened zirconia (ATZ) and zirconia toughened alumina (ZTA) nanocomposites for possible dental applications. Uniaxial compression tests at room temperature of samples 6.35 ± 0.03 mm in diameter and 12.50 ± 0.63 mm in length and Vickers hardness measurements on polished surfaces were carried out. The indentation fracture toughness (K_IC) was derived from the average crack length. Weibull analysis was performed on the data. The ATZ2 (18.0 wt.% Al₂O₃ + 2.0 wt.%_(w) + 80.0 wt.% ZrO₂ (TZ-3Y)) nanocomposite reported the highest average compressive load of 1200 MPa, the highest value of characteristic strength, σ_o, of 1340 MPa with Weibull modulus of 3.25 and relatively high fracture toughness (4.7 ± 0.7 MPa m^1/2), suggesting that with the wide range of mechanical properties obtained in our work, different dental applications could be offered without lead to premature failure.     

The effect of particle size,sintering temperature and sintering time on the properties of Al–Al2O3 composites,made by powder metallurgy

Al₂O₃ is a major reinforcement in aluminum-based composites, which have been developing rapidly in recent years. The aim of this paper is to investigate the effect of alumina particle size, sintering temperature and sintering time on the properties of Al–Al₂O₃ composite. The average particle size of alumina were 3, 12 and 48 μm. Sintering temperature and time were in the range of 500–600 °C for 30–90 min. A correlation is established between the microstructure and mechanical properties. The investigated properties include density, hardness, microstructure, yield strength, compressive strength and elongation to fracture. It has been concluded that as the particle size of alumina is reduced, the density is increased followed by a fall in density. In addition, at low particle size, the hardness and yield strength and compressive strength and elongation to fracture were higher, compared to coarse particles size of alumina. The variations in properties of Al–Al₂O₃ composite are dependent on both sintering temperature and time. Prolonged sintering times had an adverse effect on the strength of the composite.     

Dielectric and microwave properties of ZrO2 doped CaO-SiO2-B2O3 ceramic matrix composites

The behavior of dielectric and microwave properties against sintering temperature has been carried out on CaO-SiO₂-B₂O₃ ceramic matrix composites with ZrO₂ addition. The results indicated that ZrO₂ addition was advantageous to improve the dielectric and microwave properties. X-ray diffraction (XRD) patterns show that the major crystalline β-CaSiO₃ and a little SiO₂ phase existed at the temperature ranging from 950 °C to 1050 °C. At 0.5 wt% ZrO₂, CaO-SiO₂-B₂O₃ ceramic matrix composites sintered at 1000 °C possess good dielectric properties: ?_r = 5.85, tan δ = 1.59 × 10⁻⁴ (1 MHz) and excellent microwave properties: ?_r = 5.52, Q · f = 28,487 GHz (11.11 GHz). The permittivity of Zr-doped CaO-SiO₂-B₂O₃ ceramic matrix composites exhibited very little temperature dependence, which was less than ±2% over the temperature range of −50 to 150 °C. Moreover, the ZrO₂-doped CaO-SiO₂-B₂O₃ ceramic matrix composites have low permittivity below 5.5 over a wide frequency range from 20 Hz to 1 MHz.     

Investigations on synthesis of ZrB2 and development of new composites with HfB2 and TiSi2

This paper presents the results of experimental investigations carried out on the synthesis of pure ZrB₂ by boron carbide reduction of ZrO₂ and densification with the addition of HfB₂ and TiSi₂. Process parameters and charge composition were optimized to obtain pure ZrB₂ powder. Monolithic ZrB₂ was hot pressed to full density and characterized. Effects of HfB₂ and TiSi₂ addition on densification and properties of ZrB₂ composites were studied. Four compositions namely monolithic ZrB₂, ZrB₂ + 10% TiSi₂, ZrB₂ + 10% TiSi₂ + 10% HfB₂ and ZrB₂ + 10% TiSi₂ + 20% HfB₂ were prepared by hot pressing. Near theoretical density (99.8%) was obtained in the case of monolithic ZrB₂ by hot pressing at 1850 °C and 35 MPa. Addition of 10 wt.% TiSi₂ resulted in an equally high density of 98.9% at a lower temperature (1650 °C) and pressure (20 MPa). Similar densities were obtained for ZrB₂ + HfB₂ mixtures also with TiSi₂ under similar conditions. The hardness of monolithic ZrB₂ was measured as 23.95 GPa which decreased to 19.45 GPa on addition of 10% TiSi₂. With the addition of 10% HfB₂ to this composition, the hardness increased to 23.08 GPa, close to that of monolithic ZrB₂. Increase of HfB₂ content to 20% did not change the hardness value. Fracture toughness of monolithic sample was measured as 3.31 MPa m^1/2, which increased to 6.36 MPa m^1/2 on addition of 10% TiSi₂. With 10% HfB₂ addition the value of K_IC was measured as 6.44 MPa m^1/2, which further improved to 6.59 MPa m^1/2 with higher addition of HfB₂ (20%). Fracture surface of the dense bodies was examined by scanning electron microscope. Intergranular fracture was found to be a predominant mode in all the samples. Crack propagation in composites has shown considerable deflection indicating high fracture toughness. An oxidation study of ZrB₂ composites was carried out at 900 °C in air for 64 h. Specific weight gain vs time plot was obtained and the oxidized surface was examined by XRD and SEM. ZrB₂ composites have shown a much better resistance to oxidation as compared to monolithic ZrB₂. A protective glassy layer was seen on the oxidized surfaces of the composites.     

Synthesis, vacuum sintering and dielectric characterization of zirconia (t-ZrO2) nanopowder

Phase pure zirconium oxide powders have been synthesized using the single step auto-ignition combustion method, the particles were nanometer sized (20 nm) and the size distribution was very narrow (3.4 nm). Systematic structural characterization revealed the t-ZrO₂ and indexed for its tetragonal structure (a = 3.5975 Å and c = 5.1649 Å). Calculated microstrain in most of the plane indicated the presence of compressive stress (65-288 MPa) along various planes of the particles. Observed space group (P4₂/nmc) revealed the presence of cations in the 8e positions (0.75, 0.25, 0.75) and the anions in the 16 h positions (0.25, 0.25, 0.4534). The metal-oxide (Zr-O) band observed at the low wavenumber region further confirmed the phase purity of the as-prepared ZrO₂ nanopowders. Peaks at the binding energy positions 2.042 and 0.525 keV in the energy dispersive X-ray spectrum revealed oxygen deficient zirconia. The particle size estimated by TEM was in good agreement with the results obtained through X-ray line broadening (20.81 nm) measurements. The nanopowders were sintered to above 98% of the theoretical density by using vacuum sintering technique at a relatively low temperature of 1300 °C. Stable tetragonal ZrO₂ experimentally yield the permittivity value of about 28 at 10 MHz.     

Microstructure and mechanical properties of laminated ZrB2-SiC ceramics with ZrO2 interface layers

Laminated ZrB₂-SiC ceramics with ZrO₂ interface layers were successfully prepared by tape casting, laminating and hot pressing. The flexural strength and fracture toughness are 561 ± 20 MPa and 14.4 ± 0.3 MPa m^1/2 for parallel direction, and 432 ± 18 MPa and 5.8 ± 0.3 MPa m^1/2 for perpendicular direction. The fracture toughness for parallel direction is improved significantly compared to monolithic ZrB₂-SiC ceramics. The toughening mechanism was attributed to the deflection and branch of the crack and the new microcracks, which would increase the propagation path and fracture work.     

Fabrication and mechanical properties of ultrafine grained WC-10Co-0.45Cr3C2-0.25VC alloys

The ultrafine grained WC-10Co-0.45Cr₃C₂-0.25VC alloys were fabricated through planetary ball milling and low pressure sintering. The effects of the cobalt particle size, milling speed and sintering temperature on the microstructure, hardness and fracture toughness of the ultrafine grained alloys were investigated using optical microscopy, scanning electron microscopy and mechanical testing. The results showed that the mechanical properties of the low pressure-sintered alloys substantially depend on the milling speed and sintering temperature. At the same time, the hardness and fracture toughness of the samples can be increased from 1703 MPa and 8.90 MN m^−3/2 to 1789 MPa and 11.21 MN m^−3/2, respectively, when the cobalt particle size is reduced from 17 μm to 1.4 μm.     

Fabrication of A356 composite reinforced with micro and nano Al2O3 particles by a developed compocasting method and study of its properties

Aluminum/alumina composites are used in automotive and aerospace industries due to their low density and good mechanical strength. In this study, compocasting was used to fabricate aluminum-matrix composite reinforced with micro and nano-alumina particles. Different weight fractions of micro (3, 5 and 7.5 wt.%) and nano (1, 2, 3 and 4 wt.%) alumina particles were injected by argon gas into the semi-solid state A356 aluminum alloy and stirred by a mechanical stirrer with different speeds of 200, 300 and 450 rpm. The microstructure of the composite samples was investigated by Optical and Scanning Electron Microscopy. Also, density and hardness variation of micro and nano composites were measured. The microstructure study results revealed that application of compocasting process led to a transformation of a dendritic to a nondendritic structure of the matrix alloy. The SEM micrographs revealed that Al₂O₃ nano particles were surrounded by silicon eutectic and inclined to move toward inter-dendritic regions. They were dispersed uniformly in the matrix when 1, 2 and 3 wt.% nano Al₂O₃ or 3 and 5 wt.% micro Al₂O₃ was added, while, further increase in Al₂O₃ (4 wt.% nano Al₂O₃ and 7.5 wt.% micro Al₂O₃) led to agglomeration. The density measurements showed that the amount of porosity in the composites increased with increasing weight fraction and speed of stirring and decreasing particle size. The hardness results indicated that the hardness of the composites increased with decreasing size and increasing weight fraction of particles.     

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。     

Effect of Mn content on the microstructure and mechanical properties of Mo2FeB2 based cermets

Five series of Mo₂FeB₂ based cermets with Mn addition between 0 and 10 wt% in 2.5 wt% increments were prepared by reaction sintering process. The effect of Mn content on the microstructure and crystalline phases was investigated by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffraction (XRD). Hardness (HRA) and transverse rupture strength (TRS) were also measured. Mn addition improved the wettability of the Fe binder phase on the Mo₂FeB₂ hard phase, which resulted in a decrease in porosity and Mo₂FeB₂ grain size and an increase in phase uniformity. No Fe–Mn intermetallic compounds or other intermetallic compounds were detected with increasing Mn content. The TRS increased with increasing Mn content until it reached the maximum value at 10.0 wt% Mn addition. The hardness slightly increased with increasing Mn content firstly and then turned to decrease with increasing Mn content. The highest hardness was obtained for cermets with 5.0 wt% Mn addition.     

Sinter and hot isostatic pressing (HIP) of multi-wall carbon nanotubes (MWCNTs) reinforced ZTA nanocomposite: Microstructure and fracture toughness

This work describes the microstructure and fracture toughness of zirconia toughened alumina (ZTA) nanocomposite in which multi-wall carbon nanotubes (MWCNTs) and nanosized ZrO₂ particles were used as reinforcement. The ZTA nanocomposites with additions of 0, 0.005, and 0.01 wt.% MWCNTs and 2 wt.% nanosized ZrO₂ particles were pressureless sintered in an anti-oxidant sagger with graphite powder bed at 1520 °C during 1 h in air and then HIPed at 1475 °C in argon atmosphere 1 h at a pressure of 150 MPa. Relative densities ranging 94–98% were reached. In HIPed composites the hardness and fracture toughness values were increased up to ∼17% and ∼37%, respectively, compared to the “as sintered” composites free of carbon nanotubes. A combined fracture mode, crack deflection, pull-outs of a small amount of carbon nanotubes, and bridging effect were the mechanisms leading to the improvement in fracture toughness.     

添加W对ZrB2-SiC复合材料的微观组织、力学性能和氧化行为的影响

通过放电等离子烧结技术制备了添加不同W含量(1%,3%和5%,体积分数,下同)的ZrB₂-SiC复合材料,研究了烧结过程中复合材料的致密化行为,分析了添加W对复合材料微观组织演化、相组成、力学性能和氧化行为的影响。结果表明：W的添加使复合材料的微观组织表现出核壳结构,以ZrB₂晶粒为核,原位形成的(Zr, W)B₂固溶体为壳,有效地促进了复合材料的致密化和晶粒细化。对比不含W的复合材料,含W复合材料的维氏硬度、抗弯曲强度和断裂韧性显著提高,W添加含量在3%时力学性能最优,复合材料表现出最佳的硬度、强度和韧性。随着W添加量从0%增加到5%,复合材料的氧化增重和氧化层厚度逐渐减小。当W添加量为5%时,复合材料的SiC贫化层消失。最后,详细说明了W的添加对复合材料性能的影响机制。     

Effects of sintering additives on microstructure and mechanical properties of TiB2-WC ceramic-metal composite tool materials

TiB₂-WC ceramic-metal composite tool materials were fabricated using Co, Ni and (Ni, Mo) as sintering additives by vacuum hot-pressing technique. The microstructure and mechanical properties of the composite were investigated. The composite was analyzed by the observations of scanning electron microscope (SEM), X-ray diffraction (XRD) and energy dispersive spectrometry (EDS). The microstructure of TiB₂-WC ceramic-metal composites consisted of the fine WC grains and uniform TiB₂ grains. The brittle phase of Ni₃B₄ and a few pores were found in TiB₂-WC-Ni ceramic-metal composite. A lot of pores and brittle phases such as W₂CoB₂ and Co₂B were formed in TiB₂-WC-Co ceramic-metal composite. The liquid phase of Co was consumed by the reaction which led to the formation of the pores and the coarse grains of TiB₂. The pores, brittle phases and coarse grains of TiB₂ were harmful to the improvement of the mechanical properties of the composite. The sintering additive of (Ni, Mo) had a significant effect on the density and the mechanical properties of TiB₂-WC ceramic-metal composite. The formation of intermetallic compound of MoNi₄ inhibited the consumption of liquid phase of (Ni, Mo). The liquid phase of (Ni, Mo) not only inhibited the formation of the pores and the coarse grains of TiB₂ but also strengthened the interface energy between WC and TiB₂ grains. The grain size was fine and the average relative density of TiB₂-WC-(Ni, Mo) ceramic-metal composite reached 99.1%. The flexural strength, fracture toughness and Vickers hardness of TiB₂-WC-(Ni, Mo) ceramic-metal composite were 1307.0 ± 121.4 MPa, 8.19 ± 0.29 MPa m^1/2 and 22.71 ± 0.82 GPa, respectively.     

Electrophoretic enhanced micro arc oxidation of ZrO2-HAp-TiO2 nanostructured porous layers

Micro arc oxidation (MAO) and electrophoretic deposition (EPD) processes were simultaneously employed to grow ZrO₂-HAp-TiO₂ porous layers on titanium substrates under different conditions. Influence of the electrolyte composition and the growth time on surface morphology, topography, phase structure, and stoichiometry of the layers was investigated. The utilized electrolytes consisted of β-glycerophosphate, calcium acetate, sodium phosphate, and micron sized yttria-stabilized zirconia with different concentrations. AFM and SEM evaluations revealed a rough surface with a porous structure with a pores size of 50-750 nm. The pores size increased with the time and the electrolyte concentration. Based on the XRD and XPS results, the layers consisted of anatase, hydroxyapatite, monoclinic ZrO₂, tetragonal ZrO₂, ZrO, CaTiO₃, and α-TCP phases whose fractions were observed to change depending on the synthesis conditions. The average crystalline size of the HAp phase was determined as ∼54 nm. The nano-sized zirconia particles (d = 20-60 nm) were dispersed not only on surface, but also in depth of the layers. Utilizing thicker electrolytes and prolonging the growth time resulted in decomposition of hydroxyapatite as well as tetragonal ZrO₂ to monoclinic ZrO₂. EDX results also showed that the zirconium wt% in the layers increased with the time. EPD-enhanced MAO (EEMAO) technique was expressed as an efficient route to fabricate ZrO₂-HAp-TiO₂ multiphase systems within short times and only in one step.