On the development of an apatitic calcium phosphate bone cement

Development of an apatitic calcium phosphate bone cement is reported. 100 μ Particles of tetracalcium phosphate (TTCP) and dicalcium phosphate dihydrate (DCPD) were mixed in equimolar ratio to form the cement powder. The wetting medium used was distilled water with Na₂HPO₄ as accelerator to manipulate the setting time. The cement powder, on wetting with the medium, formed a workable putty. The setting times of the putty were measured using a Vicat type apparatus and the compressive strength was determined with a Universal Testing Machine. The nature of the precipitated cement was analyzed through X-ray diffraction (XRD), fourier transform infrared spectrometry (FTIR) and energy dispersive electron microprobe (EDAX). The results showed the phase to be apatitic with a calcium-to-phosphorous ratio close to that of hydroxyapatite. The microstructure analysis using scanning electron microscopy (SEM) showed hydroxyapatite nano-crystallite growth over particulate matrix surface. The structure has an apparent porosity of ∼ 52%. There were no appreciable dimensional or thermal changes during setting. The cement passed the in vitro toxicological screening (cytotoxicity and haemolysis) tests. Optimization of the cement was done by manipulating the accelerator concentration so that the setting time, hardening time and the compressive strength had clinically relevant values.     

磷酸三钙/海藻酸钙复合平板膜的制备及其力学性能

本文提供了一种制备磷酸三钙/海藻酸钙（TCP/CA）复合平板膜的方法,以提高CA水凝胶的强度,并使其力学性能容易测试。在水溶液中将TCP与海藻酸钠复合,制备了TCP/CA复合平板膜,采用红外光谱和扫描电子显微镜对其进行表征,研究了不同TCP含量的TCP/CA复合平板膜的溶胀性能与复合平板膜在湿态和干态下的力学性能。结果表明：随着TCP含量的增加,TCP/CA复合平板膜在生理盐水中的溶胀率逐渐降低;TCP/CA复合平板膜在干态和湿态下的极限应力值均随着TCP含量的增加呈现先增加后减小的趋势;干态下的极限应力、模量和断裂能要明显大于湿态下的。该TCP/CA复合平板膜制备方法简单、厚度可控、易批量生产,在控制释放和组织工程领域有潜在的应用前景。     

In vivo estimation of calcium phosphate cements containing chondroitin sulfate in subcutis

Calcium phosphate cements using an equimolar mixture of tetracalcium phosphate and dicalcium phosphate dihydrate (TeDCPD) for the powder phase were experimentally developed for use in endodontic treatment. The fundamental cement is comprised of TeDCPD kneaded with modified McIlvain's buffer solution containing calboxymethyl cellulose sodium salt (CEM-1). In the liquid phase of the modified one (CEM-2), chondroitin sulfate (CS) was added in place of the salt. The final concentration of CS in CEM-2 is 1%. Another one (CEM-3) contained 2% CS finally in place of the salt. X-ray diffract meter (XRD) was used to examine the crystalline phases of the cements. The tissue compatibility of the cements was examined histologically in the subcutaneous tissue using rats. The XRD results showed no dibasic calcium phosphate phase to be traced in CS containing two cements after 1 day of kneading. There were more multinucleated giant cells appearing around CEM-1 than around CEM-2 or CEM-3 after 4 weeks. Fibroblasts, collagen fibers and small vessels infiltrated into the internal porous structure of CEM-3. Excluding CEM-3, two cements were encapsulated with a dense fibrous connective tissue layer. We conclude that CS, in the experimentally developed cement, contributed to biocompatibility and bioactivity of the cement.     

Fabrication of toughened Cf/SiC whisker composites and their mechanical properties

In this paper, dense short carbon fiber reinforced silicon carbide matrix composites had been fabricated by hot-pressed (HP) sintering using Al₂O₃ and La₂O₃ as sintering additives. The results showed that the combination of Al₂O₃ and La₂O₃ system was effective to promote densification of short cut carbon fiber reinforced silicon carbide composites (Cf/SiC). The whisker structure of silicon carbide was formed during the annealed treatment at 2023 K for 1 h. However, it was noted that this structure was not observed in the as-received HP material. The mechanism of forming whisker structure was not clear, but this kind of whisker structure was helpful to improve mechanical properties. The combination of grain bridging, crack deflection and whisker debonding would improve the fracture toughness of the Cf/SiC composites.     

Effect of submicron size SiC particles on microstructure and mechanical properties of AZ31B magnesium matrix composites

The magnesium matrix composites reinforced with three volume fractions (3, 5 and 10 vol.%) of submicron-SiC particles (∼0.5 μm) were fabricated by semisolid stirring assisted ultrasonic vibration method. With increasing the volume fraction of the submicron SiC particles (SiCp), the grain size of matrix in the SiCp/AZ31B composites was gradually decreased. Most of the submicron SiC particles exhibited homogeneous distribution in the SiCp/AZ31B composites. The ultimate tensile strength and yield strength of the 10 vol.% SiCp/AZ31B composites were simultaneously improved. The study of interface between the submicron SiCp and the matrix in the SiCp/AZ31B composite suggested that submicron SiCp bonded well with the matrix without interfacial activity.     

Thermal and mechanical properties of porous Y-PSZ/zircon composites

 The thermal and mechanical properties of sintered porous composites of yttria-partially-stabilized-zirconia (Y-PSZ) and zircon (ZrSiO₄) were investigated for a broad range of compositions. Fracture strengths of these composites were significantly improved with the zircon addition (0 to 50wt%). The addition of zircon also improved the thermal shock resistance. Specimens sintered at 1500^oC for 6 h with 15–20% porosity were shown to have superior strength and thermal shock resistance. These findings have been used in the manufacturing of ceramic permanent molds for brass casting. Received: 5 December 1997 / Accepted: 13 December 1997     

Development of a fully injectable calcium phosphate cement for orthopedic and dental applications

A study on the development of a fully injectable calcium phosphate cement for orthopedic and dental applications is presented. The paper describes its characteristic properties including results of biocompatibility studies. A conventional two-component calcium phosphate cement formulation (having a powder part containing dry mixture of acidic and basic calcium phosphate particles and a liquid part containing phosphate solution) is modified with a biocompatible gelling agent, to induce flow properties and cohesion. The quantity of the gelling agent is optimized to get a viscous paste, which is smoothly injectable through an 18-gauge needle, with clinically relevant setting parameters. The new formulation has a setting time of 20 min and a compressive strength of 11 MPa. The X-ray diffraction, Fourier transform infrared spectrometry, and energy dispersive electron microprobe analyses showed the phase to be hydroxyapatite, the basic bone mineral. Scanning electron microscopy revealed a porous structure with particle sizes of a few micrometers. The cement did not show any appreciable dimensional or thermal change during setting. The injectability is estimated by extruding through needle and the cohesive property is assessed by water contact method. The cement passed the in vitro biocompatibility screening (cytotoxicity and haemolysis) tests.     

Indirectly extruded biodegradable Zn-0.05wt%Mg alloy with improved strength and ductility: In vitro and in vivo studies

As compared to permanent orthopedic implants for load-bearing applications, biodegradable orthopedic implants have the advantage of no need for removing after healing, but they suffer from the "trilemma" problem of compromising among sufficiently high mechanical properties, good biocompatibility and proper degradation rate conforming to the growth rate of new bones. In the present work, in vitro and in vivo studies of a Zn-0.05 wt%Mg alloy(namely, Zn-0.05 Mg alloy) were conducted with pure Zn as a control. The Zn-0.05 Mg alloy is composed of a small amount of Mg_2 Zn11 phase embedded in the refined Zn matrix with an average grain size of ～20 μm. The addition of 0.05 wt% Mg into Zn significantly increases the ultimate tensile strength up to 225 MPa and the elongation to fracture to 26%, but has little influence on the in vitro degradation rate. Both Zn and Zn-0.05 Mg alloy exhibit homogeneous in vitro degradation with a rate of about 0.15 mm/year. Based on the cytotoxicity evaluation, Zn and Zn-0.05 Mg alloy do not induce toxicity to L-929 cells, indicating that they have little toxicity to the general functions of the animal. An in vivo biocompatibility study of Zn and Zn-0.05 Mg alloy samples by placing them in a rabbit model for 4.12 and 24 weeks, respectively did not show any inflammatory cells, and demonstrated that new bone tissue formed at the bone/implant interface, suggesting that Zn and Zn-0.05 Mg alloy promote the formation of new bone tissue. The in vivo degradation of Zn and Zn-0.05 Mg alloy does not bring harm to the important organs and their cell structures. More interestingly, Zn and Zn-0.05 Mg alloy exhibit strong antibacterial activity against Escherichia coli and Staphylococcus aureus. The above results clearly demonstrate that the Zn-0.05 Mg alloy could be a potential biodegradable orthopedic implant material.     

Rational synthesis of a nanocrystalline calcium phosphate cement exhibiting rapid conversion to hydroxyapatite

The rational synthesis, comprehensive characterization, and mechanical and micromechanical properties of a calcium phosphate cement are presented. Hydroxyapatite cement biomaterial was synthesized from reactive sub-micrometer-sized dicalcium phosphate dihydrate and tetracalcium phosphate via a dissolution-precipitation reaction using water as the liquid phase. As a result nanostructured, Ca-deficient and carbonated B-type hydroxyapatite is formed. The cement shows good processibility, sets in 22 ± 2 min and entirely transforms to the end product after 6 h of setting reaction, one of the highest conversion rates among previously reported for calcium phosphate cements based on dicalcium and tetracalcium phosphates. The combination of all elucidated physical-chemical traits leads to an essential bioactivity and biocompatibility of the cement, as revealed by in vitro acellular simulated body fluid and cell culture studies.The compressive strength of the produced cement biomaterial was established to be 25 ± 3 MPa. Furthermore, nanoindentation tests were performed directly on the cement to probe its local elasticity and plasticity at sub-micrometer/micrometer level. The measured elastic modulus and hardness were established to be E_s = 23 ± 3.5 and H = 0.7 ± 0.2 GPa, respectively. These values are in close agreement with those reported in literature for trabecular and cortical bones, reflecting good elastic and plastic coherence between synthesized cement biomaterial and human bones.     

Effect of pore structure on mechanical properties of porous TiAl

Based on two sets of TiAl powder, two kinds of porous TiAl were separately fabricated by powder metallurgical route including four stages. The porous TiAl with single pore structure (SPS) was prepared using pre-alloyed TiAl powder prior mechanical ball milling. Another porous TiAl with composite pore structure (CPS) was manufactured depending on composite mixture of Ti/Al elemental powders. The sintering was achieved at much lower temperature for the pre-alloyed power than for the elemental composite mixture. Compressive mechanical tests indicate that much higher mechanical strength can be obtained for SPS than for CPS at the same porosity. It was suggested that the difference of mechanical properties is ascribed to the variety of the compressive deformation process.     

Structure and mechanical properties of the annealed TZAV-30 alloy

The Ti–30Zr–5Al–3V (wt.%, TZAV-30) alloy having good mechanical properties is a potential structural material to apply in the aerospace industry. The microstructure and mechanical properties of ZTAV-30 alloy underwent various annealing heat treatments were investigated. The specimens annealed from 500 to 800 °C are composed of α and β two phases. No compound is detected in specimens annealed in that temperature range. The microstructure of annealed specimens is characterized as a typical basketweave microstructure. Three microstructural parameters, thickness of plate α phase, relative fraction of β phase and aspect ratio of α grains, were measured in those annealed specimens. As the alloy annealed in the range from 500 to 800 °C, the average thickness of plate α grains increases with the increasing annealing temperature from 500 to 700 °C but decreases while annealed at 800 °C. The fraction of retained β phase increases with annealing temperature. And the aspect ratio of plate α grains decreases firstly but increases while the annealing temperature is higher than 700 °C. As the variation of those three microstructural parameters, the strength of examined alloy varies from 1269 to 1355 MPa for tensile strength and from 1101 to 1190 MPa for yield strength, inversely, the elongation changes in the range from 12.7% to 8.4%. The strengthening and toughening mechanism of the TZAV-30 alloy with basketweave microstructure is also discussed in this paper.     

Micro-mechanical properties of calcium sulfoaluminate cement and the correlation with microstructures

To investigate the micro-mechanical properties of calcium sulfoaluminate cement and the correlation with the microstructures, we apply a variety of advanced techniques of microstructural and micro-mechanical characterization, including scanning electron microscopy with backscattered electron and energy-dispersive X-ray spectroscopy detectors, X-ray fluorescence, X-ray diffraction and nanoindentation. For the first time, the micro-mechanical properties of material microstructures present in a calcium sulfoaluminate cement are estimated. In the calcium sulfoaluminate cement used in this research, two type of hydration product microstructures with the differentiable microstructural morphologies, compositions and micro-mechanical properties are identified and investigated. The correlation of the micro-mechanical properties with the microstructures shows that the hydration product microstructure containing more ettringite has lower indentation modulus and hardness than that containing more aluminum hydroxide.     

Microstructure and mechanical properties of hot pressed ZrB2-SiCp-ZrO2 composites

The present paper investigated the microstructure and mechanical properties of ZrB₂-10 vol.%SiC_p-10 vol.%ZrO₂ composites hot pressed at three temperatures. Phase transformability from t-ZrO₂ to m-ZrO₂ during fracture was analyzed through calculating the volume fractions of m-ZrO₂ and t-ZrO₂ on polished and fracture surfaces. The densification temperature was found to have a significant effect on the microstructure, phase transformation and the properties of the composites. When the composite was hot pressed at 1950 °C, the average grain size was 9.5 µm, and the fracture toughness was 4.5 MPa·m^1/2. Comparatively, when the composite was hot pressed at 1750 °C, the average grain size was 3.4 µm, and the fracture toughness increased by ~ 50% to 6.8 MPa·m^1/2.     

Microstructure and mechanical properties of Mg-4.0Zn-0.5Ca alloy

A new kind of Mg-4.0 wt.%Zn-0.5 wt.%Ca alloy is fabricated by casting and hot extrusion for used as a high performance structure material as well as a biomaterial. In the as-cast alloy, the average grain size of the α-Mg is 120-150 µm and the precipitated second phases are distributed uniformly in α-Mg grains. The as-cast Mg-4.0 wt.%Zn-0.5 wt.%Ca alloy shows a good balance between the tensile strength (211 MPa) and ductility (17% in elongation). After hot extrusion at 593 K, the second phase is greatly refined and the average grain size of the α-Mg is reduced to 8-12 μm which is resulted from dynamic re-crystallization during hot extrusion. In this case, it exhibits a high tensile strength (273 MPa) and a high ductility (34% in elongation) at room temperature.     

Microstructure and mechanical properties of the T23 steel after long-term ageing at elevated temperature

The paper presents the results of research on the microstructure and mechanical properties of T23 steel after long-term ageing up to 70 000 h at the temperature of 550 and 600 °C. It has been shown that the main mechanisms of degradation of the T23 steel microstructure were: recovery of the matrix, disintegration of the bainitic microstructure, growth of carbide diameter and precipitation of M6C carbides. These processes were more advanced in the steel aged at higher temperature. The changes in the microstructure resulted in a 10–15% decrease in mechanical properties (YS, TS) and hardness HV10, and a 30–40% decrease in the impact energy kV. A greater fall of impact strength occurred in the steel aged at the lower temperature. This was ascribed to the segregation of phosphorus to grain boundaries, which has a well-known adverse effect on ductility of low-alloy steels.     

Influence of oxygen content on the microstructure and mechanical properties of cold rolled Ti-32.5Nb-6.8Zr-2.7Sn-xO alloys after aging treatment

The influence of oxygen (O) content on the microstructure and mechanical properties of cold rolled Ti-32.5Nb-6.8Zr-2.7Sn-xO (TNZS-xO; x?=?0, 0.3, 0.6; mass%) alloys after aging at temperature range from 350 to 600?°C for 24?h was investigated. Results showed that the cold rolled TNZS-xO alloys possess single β phase. During the aging process, O could not only effectively suppress the precipitation of ω phase but also retard the formation and decomposition of α phase. In addition, the corresponding temperatures of the maximal volume fraction of α phase precipitation and the (α+β)/β transus temperatures of the TNZS-xO alloys were all increased with the increasing of O content. For mechanical properties, it was found that the strength and Young's modulus of the TNZS-xO alloys increased owing to the ω phase and/or α phase precipitation and decreased owing to the α phase decomposition. However, the elongation showed the opposite change tendency with the above mentioned strength. The mechanical properties of TNZS-xO alloys can be controlled over a wide range by subjecting to aging treatment and/or changing their O content. When aged at or below 450?°C, the TNZS-xO alloys exhibit great potential to become a series of new candidates for biomedical applications since they possess high strength (870–1460?MPa), low Young's modulus (45.1–75.6?GPa), high strength-to-modulus ratio (0.018–0.02) and appropriate elongation (7.2%–14.9%), which are superior to those of Ti-6Al–4?V alloy and suitable for the use as bio-implant materials.     

Effect of fabrication process on the microstructure and dynamic compressive properties of SiCp/Al composites fabricated by spark plasma sintering

The effect of fabrication process on the microstructure and dynamic properties of SiC_p/Al composites was studied in this paper. Pure Al matrix composites reinforced with 20 vol.% SiC particles were fabricated by spark plasma sintering, and the pre-blended powders were prepared by two different processes. One was to mix the powders in conical flask by using a mechanical stirrer, and the other was the mechanical alloying process by using a planetary ball mill. The sintering temperature was also explored. The conventional split Hopkinson pressure bar was used to test the dynamic properties of these composites. The results show that the sintering temperature significantly affects the consolidation of the composites. The composites, which have not been fully densified, have very loose microstructure and poor mechanical properties. Mechanical alloying process can improve the microstructure and mechanical properties of the composites. These composites are rate dependent, their strengths increase with increasing strain rates.     

Microstructure,mechanical and degradation properties of equal channel angular pressed pure magnesium for biomedical application

Abstract

Magnesium is a biocompatible and biodegradable metal, which has attracted much interest in biomedical engineering. Pure magnesium shows the low strength and plasticity at ambient temperature. Microstructure, mechanical properties and degradation properties of the equal channel angular pressed pure magnesium have been investigated for biomedical application in detail by optical microscopes, mechanical properties testing and corrosion testing. The results have revealed that the processing temperature and routes are important factors that affect the properties of pure Mg by equal channel angular pressing. The two-step equal channel angular pressing processing (one pass at 360°C and three passes at 200°C) has been successfully applied to control the microstructure, mechanical and degradation properties of the pure Mg. Optical microscopy observation has indicated that the grain size of the as cast pure magnesium has been significantly decreased after equal channel angular extrusion, which has mainly contributed to the high tensile strength and good elongation. Equal channel angular pressed pure magnesium has provided moderate corrosion resistance, which has opened a new window for materials design, especially for biomedical.     

Microstructure and mechanical properties of an HfB2 + 30 vol.% SiC composite consolidated by spark plasma sintering

An ultra-high-temperature HfB₂–SiC composite was successfully consolidated by spark plasma sintering. The powder mixture of HfB₂ + 30 vol.% β-SiC was brought to full density without any deliberate addition of sintering aids, and applying the following conditions: 2100 °C peak temperature, 100 °C min⁻¹ heating rate, 2 min dwell time, and 30 MPa applied pressure. The microstructure consisted of regular diboride grains (2 μm mean size) and SiC particulates evenly distributed intergranularly. The only secondary phase was monoclinic HfO₂. The incorporated SiC particulates played a key role in enhancing the sinterability of HfB₂. Flexural strength at 25 °C and 1500 °C in ambient air was 590 ± 50 and 600 ± 15 MPa, respectively. Fracture toughness at room temperature (RT) (3.9 ± 0.3 MPa √m) did not decrease at 1500 °C (4.0 ± 0.1 MPa √m). Grain boundaries depleted of secondary phases were fundamental for the retention of strength and fracture toughness at high temperature. The thermal shock resistance, evaluated through the water-quenching method, was 500 °C.     

Effect of heavy metals and water content on the strength of magnesium phosphate cements

In this paper the mechanical properties of magnesium potassium phosphate cements used for the Stabilization/Solidification (S/S) of galvanic wastes were investigated. Surrogate wastes (metal nitrate dissolutions) were employed containing Cd, Cr(III), Cu, Ni, Pb or Zn at a concentration of 25 g dm⁻³ and different water-to-solid (W/S) ratios (0.3, 0.4, 0.5 and 0.6 dm³ kg⁻¹) have been employed. Cements were prepared by mixing hard burned magnesia of about 70% purity with potassium dihydrogen phosphate. Compressive strength and tensile strength of specimens were determined. In addition the volume of permeable voids was measured. It was found that when comparing pastes that the volume of permeable voids increases and mechanical strength decreases with the increase of water-to-solid ratio (W/S). Nevertheless pastes with the same material proportions containing different metals show different mechanical strength values. The hydration products were analyzed by XRD. With the increase of water content not previously reported hydration compound was detected: bobierrite.