Papers by Author: Xu Dong Li

Abstract: Zirconia toughened alumina (ZTA) nano-ceramic composite has excellent mechanical properties. Preparation of ZTA was conducted in the present study with an attempt to use as dental ceramics. On the basis of the study on the effect of the die pressing forces on the density and Vickers hardness of the sintered ZTA, additive aids TiO2, MgO, SiO2 and CaO were introduced in order to reduce the sintering temperature of ZTA nano-ceramic composite with good densification. Scanning electron microscopy was employed to evaluate the microstructural morphology. Phase composition was confirmed by using X-ray diffraction. Thermal analysis was further used to study the structural change. The results indicated that the ZTA product sintered at 1450°C had dense and uniform microstructure due to the combinative effect of additive aids, including the formation of an intermediate compound. This study suggested that such ZTA nano-ceramics had potential applications as dental prosthetic materials.

Abstract: L9 (34) orthogonal array design was employed to optimize experimental conditions for the preparation of the composite using in situ synthesis method and to analyze the relationships between experimental parameters and mechanical property of the composites. Bending strength of the composite was considered as a target property of the composites. Hydroxyapatite content in the composite, synthesis temperature and pH were chosen as main parameters. As a result of this study, bending strength of the composite appeared in peak with the increase of the hydroxyapatite content of the composites and synthesis pH, while with the increase of temperature, bending strength decreased. Optimum experimental conditions for the synthesis of the composites with higher bending strength were determined. The bending strength of the composites was 90 MPa at the optimal synthesis conditions.

Abstract: The aim of this study was to optimize sintering aids and processing parameters for zirconia toughened alumina (ZTA) nano-ceramics with optimal properties as dental ceramics. Additive agents (TiO2, MgO, SiO2), dry pressing forces and sintering temperatures are very important for preparation of structural ceramics. In the present study, density and Vickers hardness measurement, SEM, and XRD analysis were employed to investigate the effects of these on the final products. The relevant results showed that higher pressing force led to an increase in the density and Vickers hardness of the sintered ceramics. Among the four groups of sintered nanoceramics with different ratios of alumina and zirconia, and combinations of additive agents, the best densification was achieved in the sample from Group 2# containing 1.05wt% MgO after sintered at 1450°C, as indicated by SEM observation. XRD analysis confirmed the formation of MgAl2O4 as an intermediate compound. The existence of TiO2 in the additive agents was in favor of the acquisition of high densification. The measured values for the density and Vickers hardness indicated that the sintered ZTA nano-ceramics would be a potential material for dental prosthetic applications.

Abstract: Synthesis of hydroxyapatite (HA) in organic solutions has received extensive attention in recent years with an attempt to obtain HA of a nanometer level. In this preliminary study, we demonstrated that organic-HA nanocomposites could also be achieved with one step method via in situ mineralization and subsequent crosslinking of organic species. This design was realized through in situ synthesis of hydroxyapatite in poly(vinyl alcohol) and acrylic acid aqueous solution as an organic template. The aforementioned organic-inorganic nanocomposites were analyzed by using X-ray diffraction, Fourier-transform infrared spectroscopy, scanning electrical microscopy, thermal analysis. The comparative structural measurements were also conducted with the synthesized HA with absence of the organic template. The results indicated that the existence of organic species effectively inhibits the growth of calcium phosphate and that relatively pure HA can be obtained in sintered composite products. The present study provides a direct and versatile route for fabrication of nanocomposite biomaterials.

Abstract: Collagen (Col) and chitosan (Chi) are both natural polymers and have received extensive investigation in recent years in the field of tissue engineering, but there are few reports on the introduction of hydroxyapatite (HA) into the Col-Ch system. In this study, based on the miscibility of these two polymers under proper condition, hydroxyapatite (HA) was synthesis in the Col-Chi system by in-situ co-precipitate method to give rise to a novel nanocomposite. The structural characterization of such Col-Ch-HA nano-materials was carried out by using FT-IR, XRD, SEM and TGA analyses with main components and Col-Chi samples used for comparison. It was found that there exist interactions between Col and Chi molecules. The nucleation and growth of inorganic phase occurs in the Col-Chi system and final products are uniform dispersion of nano-sized HA in the Col-Chi network without obvious phase separation. This novel nanocomposite would be a promising material for bone tissue engineering.

Abstract: Hydroxyapatite/collagen composites were prepared in-situ synthesis. The composites were finally achieved by dehydration including air-drying and freeze-drying methods. FTIR, XPS and DSC were employed to investigate the composites dehydrated by two methods. The air-dried composites had better mechanical properties than those of the composites dried by freeze drying. Air-drying of the composite induced more bond formation and crosslink between collagen fibers and HA crystals compared with freeze-drying of the composite, as indicated by the shifting of amide A and I bands to the lower wavenumber and by the changes in the binding energy of O1s, Ca2p, and P2p, leading to the increase of the peak temperature of the composites. Collagen crosslink and bond formation in the air-dried composites were key factors to increase the bending strength of the composites. The results of this study confirm that in situ synthesis and air-dry method are effective ways to obtain nanoHA/COL composites with high mechanical properties.

Abstract: Poly(vinyl alcohol) (PVA) was introduced during in situ synthesis of hydroxyapatite (HA) in neutral collagen (COL) solution and final PVA-COL-HA nanohybrids were achieved via sequential steps including gelation by fibrillogenesis, freezing-thawing physical crosslinking, removal of unreacted residues and dehydration. This method is expected to endow the pure PVA with good bioactivity and meanwhile the presence of elastic PVA would improve the properties of COL-HA composites. The phase, microstructure and possible molecular interactions of the achieved PVA-COL-HA nanohybrids were analyzed by using X-ray diffraction, Fourier transform infra-red spectroscopy and scanning electron microscopy. The results indicate that the inorganic phase is poorly crystallized apatite with a nanometer size due to the confinement of organic macromolecules which forms a network structure.

Abstract: An organic/inorganic composite hydrogel route was used to prepare collagen-calcium phosphate hybrids with high mechanical strengths, via in-situ mineral synthesis during collagen fibrillogenesis followed by dehydration. An array of characterization techniques including X-ray diffraction and Fourier transform infrared spectroscopy analyses confirmed that the final products are analogous to natural bone. A three-point bending strength of 70 MPa, much higher than the values reported in the literature, was recorded in the present case, due to the three dimensional network structure achieved between inorganic and organic phases. This innovative method provides an efficient route to produce bone grafts with the desirable mechanical properties which are dependent upon the actual inorganic/organic ratio and water content.

Abstract: A composite hydrogel with interpenetrating network structure was prepared via in-situ synthesis of calcium phosphates during the physical-chemical crosslinking of poly(vinyl alcohol) (PVA) and poly(acrylic acid) (PAA). The hydrogel water content was tested. Fourier transform infrared absorption spectrum (FT-IR), X-ray diffraction and scanning electron microscopy were employed to evaluate the characteristics of the composite hydrogel. The results showed that the composite hydrogel had high water content and that the inorganic phase was poorly crystalline calcium phosphates. FT-IR confirmed that the interpenetrating network structure was formed between PVA and PAA. The chemical interactions between inorganic and organic phases were further investigated and discussed. The composite hydrogel with an interpenetrating network achieved using the present novel method could be a promising material for tissue engineering.

Abstract: Good interfacial interaction is crucial for preparation of inorganic-organic materials at a nanometer level. Poly(α-methacrylic acid) (PMAA) was grafted on the PLA surfaces via photooxidization and subsequent UV induced polymerization in an attempt to synthesize nano-hydroxyapatite/poly(lactide) (n-HA/PLA) composites. Grafting of PMAA on the PLA surface was confirmed using FTIR analysis and the size distribution measurement of the grafted-PLA (g-PLA) particles. n-HA/g-PLA composites were in situ synthesized via dropwise addition of Ca2+- and g-PLA containing solution to PO4 3-- solution. The prepared composites were characterized by FTIR, XRD，SEM and TEM means. Analytical results indicated that the g-PLA acts as a template to manipulate the nucleation and growth of n-HA crystals and thereby to control the morphology, size and anisotropy of n-HA crystals and their distribution over the organic phase. Chemical linkages and/or interfacial interactions between the n-HA and the g-PLA in the n-HA/g-PLA composite were further discussed.