Fabrication of Calcite Foam by Inverse Ceramic Foam Method

2012 ◽  
Vol 529-530 ◽  
pp. 153-156 ◽  
Author(s):  
Tram Nguyen Xuan Thanh ◽  
Michito Maruta ◽  
Kanji Tsuru ◽  
Alireza Valanezhad ◽  
Shigeki Matsuya ◽  
...  

We have previously reported that calcite foam that had interconnected porous structure could be prepared by ceramic foam method and it transformed to carbonate apatite (CO3Ap). In the ceramic foam method, polyurethane sponge was used as a template. The polyurethane sponge was immersed in the ceramics slurry, and the strut of the polyurethane foam was covered by ceramic powder. After that it was dried and sintered at high temperature. Calcite foams produced by this approach were comprised of a three-dimensional (3D) interconnected porous structure that facilitated cell penetration. However, all foams have a common limitation: the inherent lack of mechanical strength associated with high porosity. Therefore, in this study, an inverse ceramic foam method was studied; multi polyurethane coating method using polyurethane foam as a template. In this study, the compressive strength was improved by an inverse replication allowed for decreasing porosity while at the same time maintaining the interconnectivity. The burnable synthetic resin coating layer was introduced onto struts of polyurethane foam to make the triangular struts become more round and thick, consequently producing large round capillary within the foam structure fulfilling the requirement for osteoblast colonization. In particular, polyurethane foam was dipped orderly into two monomers, followed by centrifugation to remove excess liquids inside foam. After resin curing, a layer of synthetic resin was coated strut of foam. Calcium hydroxide Ca (OH)2 slurry was then infiltrated into resin coated-polyurethane foam. By firing at 600°C in O2-CO2 stream, polyurethane template was burnt off and Ca (OH)2 was converted into calcite. Negative replicated calcite foam was fabricated and characterized micro-structurally with interconnectivity and improved mechanical strength. The results obtained in this study suggested that this method dramatically improved the mechanical strength of the calcite foam without sacrificing the interconnected structure, and this means that the calcite foam obtained in this method could be precursors for the 3D interconnected porous CO3Ap foam.

2014 ◽  
Vol 891-892 ◽  
pp. 1559-1564 ◽  
Author(s):  
Tram Nguyen Xuan Thanh ◽  
Michito Maruta ◽  
Kanji Tsuru ◽  
Shigeki Matsuya ◽  
Kunio Ishikawa

In this study, three - dimensional porous carbonate apatite (CO3Ap) materials with the chemical compositions and structures similar to cancellous bone were produced via phosphorization of porous calcite precursor in hydrothermal condition. In order to make porous calcite precursor, negative replication of polyurethane foam that named as inverse ceramic foam method was conducted. When the polyurethane template occupied within the ceramic solid walls disappeared due to burning at high temperature, interconnected hollow pathways were produced. Polyurethane foam was used as a porogen - template firstly was coated layer by layer with synthetic resin to modify morphology and enlarge thickness of struts so as to expand porous area for satisficing cellular bioactivities. Calcium hydroxide (Ca(OH)2) slurry was then infiltrated into resin coated-polyurethane foam. Heat treatment in atmosphere of oxygen and carbon dioxide gases was carried out to eliminate polyurethane template and induce carbonation process. Ca(OH)2 was converted to calcite with the internal porous channel architecture simulating polyurethane foam struts network. That interconnected porous calcite was subsequently transformed to CO3Ap with remaining the same macroporous structure through hydrothermal treatment in phosphate solution. The porous CO3Ap materials were implanted in the tibia of Japanese male rabbits and removed after a period of 3 months. The bone formation response of the three - dimensional porous carbonate apatite in vivo has been preliminary studied using micro-computed tomography (µ-CT) scanner. The results showed that the porous implant materials have sufficient mechanical strength to provide structural support during bone remodeling and successfully bond with host bone.


2016 ◽  
Vol 696 ◽  
pp. 23-26
Author(s):  
Nguyen Xuan Thanh Tram ◽  
Michito Maruta ◽  
Kanji Tsuru ◽  
Shigeki Matsuya ◽  
Kunio Ishikawa

We have established a processing method to fabricate three - dimensional porous carbonate apatite (CO3Ap) with interconnected porous structure and improved mechanical strength. Briefly, porous CO3Ap materials were produced via phosphorization of porous calcite precursor in hydrothermal condition. In order to make porous calcite precursor, negative replication of modified polyurethane foam template was conducted. In this study, an in vivo behavior of that porous CO3Ap was evaluated. The interconnected porous CO3Ap material was implanted in the tibia of Japanese male rabbits and removed after a period of 6 months. Micro-computed tomography (μ-CT) scanner and histological analysis were used to characterize the bone formation response of the porous CO3Ap. The results suggest that porous CO3Ap with enhanced mechanical strength was not only osteoconductive but also bioresorbable therefore it could be used as bone substitute material.


Nanoscale ◽  
2017 ◽  
Vol 9 (34) ◽  
pp. 12601-12608 ◽  
Author(s):  
Han-Yu Li ◽  
Lang Liu ◽  
Zhi-Wei Zhang ◽  
Shu-Shen Wang ◽  
Yao Yu ◽  
...  

Three-dimensional functionalized graphene monoliths (3DFGMs) have attracted intensive attention as energy storage materials due to their unique interconnected porous structure, good electrical conductivity, excellent mechanical strength, and pseudocapacitive characteristic.


2005 ◽  
Vol 284-286 ◽  
pp. 373-376 ◽  
Author(s):  
Ishikawa Kunio ◽  
Koh-ichi Udoh ◽  
Hanae Wakae ◽  
Melvin L. Munar ◽  
Shigeki Matsuya ◽  
...  

Carbonate apatite form that has three-dimensional fully interconnected pore was prepared based on so-called ceramics form preparation method. First, a-tricalcium phosphate (a-TCP) form was prepared by immersing polyurethane form into a-TCP powder suspension. The form was heated in an electronic furnace for sintering a-TCP as well as for burning out of the polyurethane form. Then hydrothermal treatment was preformed at 200 degrees in the presence of saturated sodium bicarbonate for 24 hours. Although the mechanical strength of the carbonate apatite form was poorer when compared with a-TCP form, we found that the hydrothermal treatment of a -TCP form result in the formation of B-type carbonate apatite form without changing the ideal morphology of a -TCP form.


2008 ◽  
Vol 368-372 ◽  
pp. 920-922
Author(s):  
Hong Li Liu ◽  
Wen Wu Zhong ◽  
Yang Wu Mao

The SiOC foam ceramics were prepared using polyurethane sponge and polysiloxane as raw materials. The effects of the pyrolysis temperature, the concentration of polysiloxane solutions, and the content of SiC nano-powder on compression strength of the SiOC foam ceramics have been investigated respectively. The optimum compression strength of SiOC foam ceramics is obtained at the pyrolysis temperature of 1250°C and the concentration of solution PSO of 0.8 g/ml. Adding SiC nano-powder into PSO can effectively increase compression strength of samples, and the maximum compression strength, 20.8 MPa, is obtained when the content of SiC nano-powder is 5 wt%. Microstructural study reveals that the foam ceramics have an open, uniform and interconnected porous structure with high porosity of 80%.


2019 ◽  
Vol 829 ◽  
pp. 28-33
Author(s):  
Zatira Avriyanti ◽  
Zulia Hasratiningsih ◽  
Arief Cahyanto

Carbonate apatite is one of the most widely studied bioceramic material for its use as bone cement. On the previous study, it has already stated that CO3Ap cement has good osteoconductivity which makes this cement could be replaced by bone. However, the mechanical strength of CO3Ap cement is still low. This low mechanical strength is estimated due to the high porosity and absence of organic components. The aim of this study is to improve the mechanical strength of the CO3Ap cement reinforced by gelatin as an organic component with genipin as a cross-linking agent (Gelapin). The powder phase of vaterite and DCPA at weight ratio 40:60 were mixed with 0.2 mol/L Na2HPO4, 5% (w/v) gelatin, and 20% (v/v) genipin using 0.5 liquid to powder (L/P) ratio. The liquid phase ratios of Na2HPO4 and Gelapin were 50:50, 70:30, and 90:10. For control group, Gelapin were didn’t mixed in the liquid. Diametral tensile strength was improving and statistically significant (p<0.05) on set cement with 50:50 liquid ratio, the average value was 6.02 ± 0.14 MPa whereas the average value of the control group was only 3.10 ± 0.15 MPa. For this instance, gelatin serves a polymer matrix so the carbonate apatite crystallites could be well distributed within it which then gives more flexibility and resistance for the cement. On the other hand, genipin was also successfully cross-linked the gelatin. This study showed that by reinforcing CO3Ap cement using genipin cross-linked gelatin might be a good candidate for a bone substitute material.


2014 ◽  
Vol 910 ◽  
pp. 23-26
Author(s):  
Lie Feng Liang ◽  
Jun Jie Chen ◽  
Yong He ◽  
Dai Yang Li

A new technique to prepare macroporous hydroxyapatite (HA) scaffolds was introduced. Porous HA ceramics were prepared by sol-gel method from chitin dissolved in dimethylacetylamide (DMAc) / lithium chloride (LiCl) solvent, three dimensional stacking with HA gel fibers and pore agent. The blocks dried were heated to optimum sintering temperature of 1280°C. The porous HA ceramics reinforced by homogeneous fibers, with interconnected pores and high porosity and pore-diameter were obtained, whilst improving mechanical strength. Sintered ceramics were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD analysis confirmed that the crystal structure remained HA. SEM showed the samples presented a highly interconnected porous reticulate structure with average pore size ranging from 340μm to 450μm. The porosity was varied from 61% to 83%. The maximum compressive strength of HA ceramic was 3.4MPa.The mechanical strength of samples was improved with addition of homogeneous fibers.


Minerals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 213
Author(s):  
Hamid Ait Said ◽  
Hassan Noukrati ◽  
Hicham Ben Youcef ◽  
Ayoub Bayoussef ◽  
Hassane Oudadesse ◽  
...  

Three-dimensional hydroxyapatite-chitosan (HA-CS) composites were formulated via solid-liquid technic and freeze-drying. The prepared composites had an apatitic nature, which was demonstrated by X-ray diffraction and Infrared spectroscopy analyses. The impact of the solid/liquid (S/L) ratio and the content and the molecular weight of the polymer on the composite mechanical strength was investigated. An increase in the S/L ratio from 0.5 to 1 resulted in an increase in the compressive strength for HA-CSL (CS low molecular weight: CSL) from 0.08 ± 0.02 to 1.95 ± 0.39 MPa and from 0.3 ± 0.06 to 2.40 ± 0.51 MPa for the HA-CSM (CS medium molecular weight: CSM). Moreover, the increase in the amount (1 to 5 wt%) and the molecular weight of the polymer increased the mechanical strength of the composite. The highest compressive strength value (up to 2.40 ± 0.51 MPa) was obtained for HA-CSM (5 wt% of CS) formulated at an S/L of 1. The dissolution tests of the HA-CS composites confirmed their cohesion and mechanical stability in an aqueous solution. Both polymer and apatite are assumed to work together, giving the synergism needed to make effective cylindrical composites, and could serve as a promising candidate for bone repair in the orthopedic field.


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