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1.
Three dimensional electrospun carbon nanofiber (CNF)/hydroxyapatite (HAp) composites were biomimetically synthesized in simulated body fluid (SBF). The CNFs with diameter of ∼250 nm were first fabricated from electrospun polyacrylonitrile precursor nanofibers by stabilization at 280 °C for 2 h, followed by carbonization at 1200 °C. The morphology, structure and water contact angle (WCA) of the CNFs and CNF/HAp composites were characterized. The pristine CNFs were hydrophobic with a WCA of 139.6°, resulting in the HAp growth only on the very outer layer fibers of the CNF mat. Treatment in NaOH aq. solutions introduced carboxylic groups onto the CNFs surfaces, and hence making the CNFs hydrophilic. In the SBF, the surface activated CNFs bonded with Ca2+ to form nuclei, which then easily induced the growth of HAp crystals on the CNFs throughout the CNF mat. The fracture strength of the CNF/HAp composite with a CNF content of 41.3% reached 67.3 MPa. Such CNF/HAp composites with strong interfacial bondings and high mechanical strength can be potentially useful in the field of bone tissue engineering.  相似文献   

2.
《Ceramics International》2017,43(10):7594-7599
The effects of two-step sintering (TSS) on the mechanical properties and hydrothermal ageing resistance of yttria-stabilized tetragonal zirconia polycrystals (Y-TZP) were investigated. In TSS, the first step involved heating the samples up to 1400 °C at a heating rate of 10 °C/min and holding the samples at this temperature for 1 min. The second step involved sintering by cooling the samples down to 1200 °C and holding the samples at this temperature for various holding times (t) ranging from 0 to 30 h before cooling to room temperature. Moreover, TSS promoted densification with increasing holding time without sacrificing the mechanical properties of the sintered body and causing abnormal grain growth. The average grain size was found not to be affected by the long holding times, and the final microstructure composed of a uniformly distributed tetragonal grain having sizes ranging from 0.24 to 0.26 µm. The beneficial effect of TSS in suppressing the hydrothermal ageing of Y-TZP has been revealed in the present work. In particular, samples sintered at t=20 and 30 h exhibited excellent resistance to low-temperature degradation when exposed to superheated steam at 180 °C, attributed mainly to the enhance densification of the sintered bodies.  相似文献   

3.
《Ceramics International》2016,42(16):18053-18057
LZAS glass-ceramic composites toughened by 5, 10, 15 and 20 vol% 3-mol%-Y2O3-tetragonal-ZrO2-polycrystal (3Y-TZP) were prepared via pressureless sintering. Sinterability of composites was investigated in the temperature range of 520–720 °C using soaking time of 30 min. The sintered specimens were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) methods. The results revealed that during sintering 3Y-TZP particles agglomerated between the glass powders and were not dissolved by glass-matrix. Mechanical properties of the sintered samples such as bending strength, Vickers micro-hardness and fracture toughness were also investigated. Measurements showed that the relative density of the samples decreased with increasing 3Y-TZP content. The composite containing 15 vol% 3Y-TZP has a best mechanical properties and it would be the optimum composition. It can be confirmed that crack deflection and transformation toughening are the dominant mechanisms for improving mechanical properties of the composites.  相似文献   

4.
In this study, 3 mol% yttria-stabilized tetragonal zirconia polycrystal (3Y-TZP)/Al2O3/graphene nanoplatelets (GNPs) medical ceramic materials for manufacturing surgical scalpels were sintered in vacuum in an SPS–625HF furnace. The mechanical performances and microstructures of the composites were investigated, and the influence mechanisms of the sintering temperature and amount of added GNPs were studied. During the sintering process at 1400°C and 30 MPa for 5 min, the added GNPs enhanced the mechanical properties of the 3Y-TZP/Al2O3 composites. The results showed that the composite with .1 wt.% GNPs had 6.4% (910 ± 11 MPa) higher flexural strength than 3Y-TZP/Al2O3. The composite with .4 wt.% GNPs had 38.7% (12.95 ± .22 MPa m1/2) greater fracture toughness than 3Y-TZP/Al2O3. The main toughening mechanisms of 3Y-TZP/Al2O3/GNPs were crack bridging, crack deflection, crack branching, GNPs bridging, transgranular fracture structures, and phase transformation of t-ZrO1.95. The two-stage densification displacement curve appeared at the optimal sintering temperature of the materials, and the 3Y-TZP/Al2O3/GNPs composites with a two-stage densification displacement curve had excellent mechanical properties. The added GNPs can inhibit the grain growth during the sintering process, thereby refining the zirconia grains. With the increase in GNPs content, the grain size and flexural strength of the composites decreased gradually. However, higher content of GNPs was beneficial to improve the relative density and thermal diffusivity of 3Y-TZP/Al2O3/GNPs composite material.  相似文献   

5.
The structure-controlled hydroxyapatite/zirconia (HAp/ZrO2) composites were fabricated. At first, cylindrical hydroxyapatite (HAp) samples were prepared by the extrusion process, and then the extruded HAp cylindrical samples were coated with 3 mol% of Y2O3 partially stabilized ZrO2 slurry, dried and aligned unidirectionally to form a composite bulk. The volume fraction of ZrO2 in the HAp/ZrO2 composite was estimated to be about 23 vol%. Bulk density and bending strength of the composites increased with sintering temperature. Fracture energy of HAp/ZrO2 composite sintered at 1350 °C was approximately 1.6 times higher than that of monolithic HAp. Although the bending strength of HAp/ZrO2 composite prepared in this study was relatively low, it exhibited high fracture energy than HAp monolithic and a non-brittle fracture behavior was obtained without using fiber as the reinforcement.  相似文献   

6.
A major challenge for tissue engineers is the design of scaffolds with appropriate physical and mechanical properties. The present research discusses the formation of ceramic scaffolding in tissue engineering. Hydroxyapatite (HAp) powder was made from bovine bone by thermal treatment at 900?°C; 40, 50 and 60%wt porous HAp was then produced using the polyurethane sponge replication method. Scaffolds were coated with poly-3-hydroxybutyrate (P3HB) for 30?s and 1?min in order to increase the scaffold??s mechanical properties. XRD, SEM and FT-IR were used to study phase structure, morphology and agent groups, respectively. In XRD and FT-IR data, established hydrogen bands between polymer and ceramic matrix confirm that the scaffold is formed as a composite. The scaffold obtained with 50%wt HAp and a 30?s coating was 90% porous, with an average diameter of 100?C400???m, and demonstrated a compressive strength and modulus of 1.46 and 21.27?MPa, respectively. Based on these results, this scaffold is optimised for the aforementioned properties and can be utilised in bone tissue engineering.  相似文献   

7.
Various amounts of TiSi2 (30, 40, and 50 wt.%) were added to 3 mol% yttria stabilized tetragonal zirconia polycrystals (3Y-TZP) to fabricate 3Y-TZP/TiSi2 composites by vacuum sintering. The effects of the TiSi2 added amount, as well as the sintering temperature on the microstructure, mechanical, and electrical characteristics of the 3Y-TZP/TiSi2 composites were examined. The sintered samples consisted of three phases: tetragonal (t-ZrO2), TiSi2, and reaction product Ti5Si3. The maximum bending strength and relative density of the composites, reaching 501.20 MPa and 98.59% respectively, were achieved at a TiSi2 content of 30 wt.% and sintering temperature of 1500°C. The resistivity of 3Y-TZP/TiSi2 composites showed a nonlinear decrease with increasing TiSi2 content. These results indicated that 3Y-TZP/TiSi2 composites had a typical percolation threshold phenomenon due to the different TiSi2 content and a conductivity model of 3Y-TZP/TiSi2 composites at room temperature was founded on the generalized effective medium equation. The resistivity of the composites could optionally adjust between 102 and 10−4Ω·cm with 30–50 wt.% TiSi2 under room temperature. Overall, the 3Y-TZP/TiSi2 composites show great potential for applications in the heat-not-burn tobacco field.  相似文献   

8.
《Ceramics International》2023,49(6):9523-9533
In order to solve the problems (i.e. low infiltration efficiency, cracks, interface separation and poor mechanical properties) in the process of wood-derived C–SiC composites, the thermal modification of fir at low temperatures (300 °C ~ 350 °C) combined with sol-gel infiltration was used to successfully produce biomorphic ceramics. The prepared materials were comprehensively characterized and exhibited improved interfacial bonding between C and SiC and mechanical properties. The weight gain per unit volume (0.123 g/cm3) of SiO2 gel in the fir thermally modified at 300 °C is 167.4%, higher than that (0.046 g/cm3) of the unmodified fir. A well-bonded interface was formed between the SiO2 gel and the pore wall of the fir thermally modified at 300 °C. With the increase of modification temperature from 300 °C to 350 °C, the distance between SiO2 gel and the pore wall increases, and a gap (1–3 μm) is observed between SiO2 gel and the pore wall of the fir carbonized at 600 °C. The C–SiC composites sintered at 1400 °C exhibited the highest compressive strength and bending strength of 40.8 ± 5.8 MPa and 11.7 ± 2.1 MPa, respectively, owing to the well-bonded interface between C of fir thermally modified at 300 °C and SiC. However, the composites sintered at 1600 °C for 120 min exhibited the lowest compressive strength and bending strength of 28.1 ± 13.4 MPa and 5.7 ± 1.6 MPa, respectively, which are 31.1% and 51.3% lower than those sintered at 1400 °C for 120 min, respectively. This might result from the porous structure formed by the excessive consumption of fir-derived carbon during the reaction between C and SiO2 at 1600 °C for 120 min. Therefore, thermal modification in the preparation of biomorphic C–SiC composites can promote slurry infiltration and the formation of a well-bonded interface between C and SiC, thus improving the mechanical properties of the composites.  相似文献   

9.
《Ceramics International》2022,48(1):674-683
In order to protect carbon fibers (CF) from oxidation damage during sintering process, rod-like Mg-doped nano-hydroxyapatite (Mg-nHA) with an increased thermal decomposition temperature and reduced sintering temperature was synthesized by hydrothermal method. The synthesized bone-like Mg-nHA with similar composition and morphology to bone apatite was used as the matrix to prepare CF reinforced Mg-nHA composites (CF/Mg-nHA) at a low temperature of 700 °C by pressureless sintering. The increase of temperature slightly influenced the growth of Mg-nHA prepared by hydrothermal method from 160 °C to 200 °C. The Mg-nHA were short and rod-like in structure with a length of approximate 100 nm. When doping 1% magnesium, the decomposition temperature of Mg-nHA increased by 100 °C compared with that of nHA. This can protect CF from oxidation damage which is often encountered when sintering CF reinforced hydroxyapatite composites at high temperature and enhance reinforcing effects of CF. The bending strength of CF/Mg-nHA with 1 wt% CF was 8.51 MPa, which increased by 19.5% compared with Mg-nHA. Alternatively, the rod-like Mg-nHA was prepared on the surface of CF by electrochemical deposition and Mg-nHA coated CF was used to reinforce Mg-nHA, the coefficient of thermal expansion mismatch between CF and HA matrix could be mitigated. The compressive strength of Mg-nHA coated CF reinforced Mg-nHA (CF/Mg-nHA/Mg-nHA) composites with 0.5% CF sintered at 800 °C were 41.3 ± 1.56 MPa, which was attributed to the improved strengthening effect of CF and the good interface between CF and Mg-nHA matrix.  相似文献   

10.
《Ceramics International》2022,48(21):31289-31298
Bioceramic scaffolds are being widely employed in bone tissue engineering applications for their ability to interact with host tissues without inducing any toxicity. Additionally, bioceramics possess good biocompatibility, osteointegration, osteoinduction, and biodegradation characteristics. Hydroxyapatite (HAP) is one such bioceramic known to exhibit closeness to natural bone in terms of chemical composition. The present reports additive manufacturing of HAP and Multiwalled carbon nanotubes (MWCNTs) reinforced HAP scaffold structures for bone tissue engineering applications using the Robocasting technique. Carboxymethyl Cellulose (CMC) was employed as the polymeric binder in this study to prepare the highly viscous HAP and CNT-HAP slurry ideal for robocasting of the scaffold structures. Different percentages of MWCNT (0.5, 1 and 2 wt%) incorporated into the developed CNT-HAP scaffold structures and were vacuum sintered at 1000 °C for 15 min. Vacuum sintering was found to effectively prevent oxidation of MWCNT which is subjected to decomposition at temperatures above 400 or 500 °C in Oxygen atmosphere as per literature. Further, the retention of MWCNTs in the developed CNT-HAP structures post sintering was confirmed using FESEM imaging. The mechanical characterizations revealed that 0.5CNT-HAP structures exhibited highest compression strength (3.36 ± 0.67 MPa) in comparison to 1CNT-HAP and 2CNT-HAP structures. Also, the in vitro biological characterizations demonstrated that the developed CNT-HAP scaffold structures were cytocompatible and remained stable for about 35 days at 37 °C.  相似文献   

11.
Short Pitch-based carbon fiber-reinforced HfB2 matrix composites containing 20 vol% SiC, with fiber volume fractions in the range of 20–50%, were manufactured by hot-press process. Highly dense composite compacts were obtained at 2100 °C and 20 MPa for 60 min. The flexural strength of the composites was measured at room temperature and 1600 °C. The fracture toughness, thermal and electrical conductivities of the composites were evaluated at room temperature. The effects of fiber volume fractions on these properties were assessed. The flexural strength of the composites depended on the fiber volume fraction. In addition, the flexural strength was significantly greater at 1600 °C than at room temperature. The fracture toughness was improved due to the incorporation of fibers. The thermal and electrical conductivities decreased with the increase of fiber volume fraction, however.  相似文献   

12.
Zirconia-toughened alumina composites containing 0–30 vol% of 3Y-TZP were fabricated by sintering at 1600 °C for 2 h in air. The effect of the 3Y-TZP content on the mechanical properties and microstructure of the alumina ceramics was investigated. The fracture toughness and biaxial flexural strength increased as the 3Y-TZP content increased. The Young's modulus decreased with 3Y-TZP content according to the rule of mixture, while the hardness showed the contrary tendency. The Weibull modulus of the Al2O3 with 20 vol% 3Y-TZP composite is higher than that of alumina. The residual hoop compressive stress developed in ZTA ceramic composites probably accounts for the enhancement of strength and fracture toughness, as well as for the higher tendency of crack deflection. No monoclinic phase and strength degradation were found after low temperature degradation (LTD) testing. The excellent LTD resistance can be explained by the increased constraining force on zirconia embedded in alumina matrix.  相似文献   

13.
Nano-powder composites of 3Y-TZP doped with 8 mol% CuO were processed by spark-plasma sintering (SPS). A 96% dense composite ceramic with an average grain size of 70 nm was obtained by applying the SPS process at 1100 °C and 100 MPa for 1 min. In contrast to normal, pressureless, sintering during SPS reactions between CuO and 3Y-TZP were suppressed, the CuO phase was reduced to metallic Cu, while the 3Y-TZP phase remained almost purely tetragonal. Annealing after SPS results in grain growth and tetragonal to monoclinic zirconia phase transformation. The grain size and monoclinic zirconia phase content are strongly dependent on the annealing temperature. By combining the processing techniques studied in this work, including traditional pressureless sintering, properties of the composite ceramic can be tuned via manipulation of microstructure. Tuning the mechanical properties of dense 8 mol% CuO doped 3Y-TZP composite ceramic by utilising different processing techniques is given as an example.  相似文献   

14.
Y-TZP, Ce-TZP and Ce-TZP/Al2O3 materials are widely investigated in dentistry. Digital Light Processing (DLP) is considered as a breakthrough technology for the dental field to fine print Y-TZP green parts. High loading photocurable formulations (>45 vol%) with Y-TZP, Ce-TZP commercial powders and Ce-TZP/30 vol% Al2O3 as-synthesized powder suitable to DLP printing were achieved in this study. A low specific surface area (5–13 m2/g) of particles without any pores and 1 wt% to 2 wt% of steric dispersant are required to obtain high loading formulations. The as-synthesized composites provide these properties by increasing the calcination temperature from 800 °C to 1200 °C. The as-prepared ceramic formulations based on the same photocurable resin exhibit a curing behavior suitable to DLP process for Y-TZP formulations (thickness > 50 μm in few seconds with a high conversion rate) in comparison with ceria ceramic. The ceria is a strongly UV absorbing material and a specific formulation is developed to obtain 80% of conversion and a cured thickness of 75 μm in 0.5 s.  相似文献   

15.
《Ceramics International》2016,42(9):11126-11135
Zirconia precursor was precipitated in a HAp particles suspension using two HAp powders of natural origin and a synthetic powder. The first natural HAp was extracted from animal bones by treatment with hot NaOH solution and the second one by treatment under hydrothermal conditions with water.Hydrous zirconia was precipitated in the HAp suspension. Pressureless sintering was performed at 1000–1300 °C and hot pressing at 1050–1300 °C.It was found that zirconia additive promotes decomposition of both HAp of natural origin as well as the synthetic one. The most stable HAp was the one extracted from bovine bones by treatment with water in an autoclave. This reaction leads to the formation of β–TCP and the CaO–ZrO2 solid solution.The hot pressed composites show essentially higher strength and fracture toughness as compared to the pure hydroxyapatite polycrystals.  相似文献   

16.
Pulse electric current sintering (PECS) method was applied to the fabrication of zeolite, hydroxyapatite (HAp) and fluorapatite (FAp) sintered bodies that should be long-term assurance materials for the disposal of radioactive waste. The weight ratio of zeolite and apatite was ca. 3/7. Zeolite powder evenly covered with HAp thin layers prepared by a hydrothermal method and spherical FAp powder by spray dryer were employed for the PECS; the sample was sintered at 900 °C for 10 min at a rate of 50 °C/min under a uniaxial pressure of 50 MPa and then cooled to 600 °C at 5 °C/min in vacuum. The powder X-ray diffractions indicated that the structure of zeolite changed to the amorphous. The zeolite powder was well dispersed in FAp matrix as the results of element mapping analyses by energy dispersive X-ray spectrometer. The observations by a scanning transmission electron microscope indicated that amorphous zeolites were covered with needle-like HAp crystals of which layer completely coupled with sintered FAp grains. The HAp thin layers thus play an important role for improving the affinity between FAp matrix and the zeolite. The microhardness and three-point bending strength of the sintered bodies were also elucidated by a dynamic-ultra microhardness tester and a universal tester, respectively.  相似文献   

17.
《Ceramics International》2020,46(8):11508-11514
Nanopowders of holmium zirconate (Ho2Zr2O7) synthesised through carbon neutral sol-gel method were pressed into pellets and individually sintered for 2 h in a single step sintering (SSS) process from 1100 °C to 1500 °C at 100 °C interval and in a two step sintering (TSS) process at (I) −1500 °C for 5 min followed by (II) - 1300 °C for 96 h. Relative density of each of the sintered pellet was determined using the Archimedes’ technique and the theoretical density was calculated from crystal structure data. Grain size was obtained from SEM micrographs using ImageJ. Pellets processed by TSS have been found to be denser (98 %) with less grain growth (1.29 μm) as compared to the pellets processed using SSS process. Ionic conductivity of Ho2Zr2O7 pellets sintered by two different processes was measured using ac impedance spectroscopy technique over the temperature range of 350 °C–750 °C in the frequency range of 100 mHz–100 MHz for both heating and cooling cycles. The temperature dependence of bulk (2.67⨯10−3 Scm−1) and grain boundary (2.50⨯10−3 Scm−1) conductivities of Ho2Zr2O7 prepared by TSS process are greater than those processed by SSS process suggesting the strong influence of processing conditions and grain size. Results of this study, indicates that the TSS is the preferable route for processing the holmium zirconate as it can be sintered to exceptionally high densities at lower temperature, exhibits less grain growth and enhanced ionic conductivity compared with the samples processed by SSS process. Hence, holmium zirconate can be considered as a promising new oxide ion conducting solid electrolyte for intermediate temperature SOFC applications between 350 °C and 750 °C temperature range.  相似文献   

18.
《Ceramics International》2016,42(11):13176-13182
Nanocrystalline carbonated HAp powder has been synthesized successfully within 2 h by mechanical alloying the stoichiometric mixture of CaCO3, CaHPO4·2H2O at room temperature under open air. To observe the sintering behavior of HAp the as-milled sample is sintered at different temperatures. The amorphous HAp phase (~14 vol%) in as-synthesized sample transforms completely to crystalline HAp after sintering at 700 °C and after sintering the sample at 800 °C, the crystalline HAp partially transforms to β-TCP phase. Presence of low content of β-TCP phase in HAp powder could be useful in artificial hard tissue applications. Increase in sintering temperature up to 1000 °C results in enhancement of decomposition rate of HAp into β-TCP phase. Microstructure characterization in terms of lattice imperfections and relative phase abundances in non-sintered and all sintered samples are made both by analyzing the respective XRD patterns using Rietveld's structure refinement method as well as TEM images. The growth mechanism of β-TCP from crystalline HAp phase has been proposed based on structure and microstructure characterizations of sintered samples.  相似文献   

19.
《Ceramics International》2017,43(4):3752-3760
The clinical success of implant is governed by implant-surface and bone cell interaction that promote osseointegration and long term stability. Calcium hydroxyapatite (HAp) is a widely used bioceramic material for orthopedic and dental applications, which promotes bone tissue generation. Doped hydroxyapatite using various metallic ions is often reported to enhance this osteoconductive property. The objective of this study was to synthesize zinc doped HAp, to investigate the osteoblast cell response on this doped HAp and find out separately the effect of doping and different surface parameters on cell response. Slip casting technique was used to prepare pure and doped HAp specimens which were sintered at 1100 °C and 1250 °C. Different porosities, pore sizes were generated along with different surface roughness so as to understand the effect of these extrinsic parameters on cell culture. MG63 osteoblast cells were used for a maximum period of two weeks. Metabolic activity, adhesion and proliferation rate study of osteoblast cells on doped HAp showed significantly better response than pure HAp. Effect of doping was found to be more prominent than the effect of surface roughness.  相似文献   

20.
《Ceramics International》2022,48(2):1532-1541
In order to improve the degree of matrix densification of SiCf/SiC composites based on liquid silicon infiltration (LSI) process, the microstructure and mechanical properties of composites according to various pyrolysis temperatures and melt infiltration temperatures were investigated.Comparing the microstructures of SiCf/C carbon preform by a one-step pyrolysis process at 600 °C and two-step pyrolysis process at 600 and 1600 °C, the width of the crack and microcrack formation between the fibers and matrix in the fiber bundle increased during the two-step pyrolysis process. For each pyrolysis process, the density, porosity, and flexural strength of the SiCf/SiC composites manufactured by the LSI process at 1450–1550 °C were measured to evaluate the degree of matrix densification and mechanical properties. As a result, the SiCf/SiC composite that was fabricated by the two-step pyrolysis process and LSI process showed an 18% increase in density, 16%p decrease in porosity, and 150% increase in flexural strength on average compared to the composite fabricated by the one-step pyrolysis process.In addition, among the SiCf/SiC specimens fabricated by the LSI process after the same two-step pyrolysis process, the specimen that underwent the LSI process at 1500 °C showed 30% higher flexural strength on average than those at 1450 or 1550 °C. Furthermore, under the same pyrolysis temperature, the mechanical strength of SiCf/SiC specimens in which the LSI process was performed at 1500 °C was higher than that of the 1550 °C although both porosity and density were almost similar. This is because the mechanical properties of the Tyranno-S grade SiC fibers degraded rapidly with increasing LSI process temperature.  相似文献   

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