Effects of Liquid-to-Powder Ratio on the Properties of Self-Setting Silk Fibroin/Calcium Phosphate Composites

2012 ◽  
Vol 550-553 ◽  
pp. 1133-1138 ◽  
Author(s):  
Rui Juan Xie ◽  
Yang Yang Huang ◽  
Biao Wang ◽  
Meng Zhang
Keyword(s):  
Compressive Strength ◽  
Calcium Phosphate ◽  
Silk Fibroin ◽  
Significant Influence ◽  
High Purity ◽  
Setting Time ◽  
Obvious Effect ◽  
Tetracalcium Phosphate ◽  
Cooling Method

In this study, the high purity tetracalcium phosphate (TTCP) was prepared conveniently after studying the effect of cooling method on the purity of TTCP. The influence of liquid-to-powder (L/P) ratio on the properties of self-setting silk fibroin/calcium phosphate composites was studied. The results showed that the temperature of the furnace had a significant influence on the purity of TTCP when samples were removed from the furnace. Whether using N2 or not had no obvious effect on the purity of TTCP when the temperature declined from 1500°C to 1300°C. The setting time of composites became longer with the increase of L/P ratio in a range 0.32 - 0.39 ml/g, but all less than 15min. The injectability of the composites improved significantly as the L/P ratio increased. The compressive strength of composites reached maximum at the L/P ratio of 0.34 ml/g. The compressive strength decreased with the increase of L/P ratio greater than 0.34ml/g. The L/P ratio had no significant effect on the structure of the composites and the rod-like crystal of hydroxyapatite appeared in all the hardening-body of composites.

Preparation and Characterization of Silk Fibroin/Calcium Phosphate Composite

2011 ◽  
Vol 332-334 ◽  
pp. 1655-1658
Author(s):  
Biao Wang ◽  
Rui Juan Xie ◽  
Yang Yang Huang
Keyword(s):  
Compressive Strength ◽  
Calcium Phosphate ◽  
Silk Fibroin ◽  
Solid Phase ◽  
Setting Time ◽  
Testing Machine ◽  
X Ray Diffraction ◽  
Acicular Crystal ◽  
Setting Times

In this paper, calcium phosphate cement (CPC) was prepared with tetracalcium phosphate (TTCP)/dicalcium phosphate anhydrous (DCPA) system as solid phase and phosphate buffered solution (PBS) as liquid phase, then silk fibroin (SF) was added into CPC to form silk fibroin/calcium phosphate composite. To study the effect of SF on the properties of composite, different mass fraction of SF was added into the composite. The surface morphology was observed by Scanning Electron Microscope. The setting time was investigated by ISO Cement Standard Consistency Instrument. The structure of the composite was studied by X-ray diffraction and infrared spectroscopy. Mechanical properties of samples were tested by Instron Universal Testing Machine. The results showed that the particles of SF could be seen obviously in the surface of all composite, and acicular crystal of hydroxyapatite (HA) was formed in the hardening body of both the composite and the pure CPC. The acicular crystal of HA derived from composite with SF appeared to be thinner. The setting times of the composites were all between 9 to 15min. Compared to pure CPC, the compressive strength and work-of-compressive of composites were all improved. The compressive strength of the composite with 1% SF increased obviously.

scholarly journals Calcium Phosphate Cement Modified with Silicon Nitride/Tricalcium Phosphate Microgranules

2020 ◽  
Vol 20 (1) ◽  
pp. 56-75
Author(s):  
Lubomir Medvecky ◽  
Radoslava Stulajterova ◽  
Maria Giretova ◽  
Tibor Sopcak ◽  
Maria Faberova ◽  
...  
Keyword(s):  
Compressive Strength ◽  
Silicon Nitride ◽  
Calcium Phosphate ◽  
Tricalcium Phosphate ◽  
Setting Time ◽  
Controlled Drug Release ◽  
Tetracalcium Phosphate ◽  
Composite Cement ◽  
Highly Porous

Abstract Tetracalcium phosphate/monetite biocement was modified with 10 and 30 wt. % addition of highly porous silicon nitride/α-tricalcium phosphate (αTCP) microgranules with various content of αTCP. A composite cement powder mixture was prepared using mechanical homogenization of basic components. The accelerated release of dexamethasone from composite cement was revealed, which indicates their possible utilization for controlled drug release. The wet compressive strength of cements (<17 MPa) was significantly reduced (more than 30%) in comparison with the unmodified cement and both compressive strength and setting time were influenced by the content of αTCP in microgranules. The addition of microgranules caused a 20% decrease in final cement density. Microgranules with a higher fraction of αTCP showed good in vitro SBF bioactivity with precipitation of hydroxyapatite particles. Microstructure analysis of fractured cements demonstrated excellent interconnection between microgranules and cement calcium phosphate matrix, but also showed lower mechanical strength of microgranule cores.

Properties of Powder Composite Polyhydroxybutyrate–Chitosan-Calcium Phosphate System

2017 ◽  
Vol 17 (1) ◽  
pp. 1-9
Author(s):  
L. Medvecky ◽  
R. Stulajterova ◽  
M. Giretova ◽  
M. Faberova
Keyword(s):  
Compressive Strength ◽  
Calcium Phosphate ◽  
Thin Layer ◽  
Composite System ◽  
Calcium Phosphates ◽  
Setting Time ◽  
Transformation Rate ◽  
Tetracalcium Phosphate ◽  
Hardening Process ◽  
Phosphate System

Abstract Prepared powder polyhydroxybutyrate – chitosan - calcium phosphate composite system with 10 wt % of biopolymer component can be utilized as biocement which is characterized by the prolonged setting time and achieves wash out resistance after 5 minutes of setting. The origin powder tetracalcium phosphate/nanomonetite agglomerates were coated with the thin layer of biopolymer which decelerates both the transformation rate of calcium phosphates and hardening process of composites. The porosity of hardened composite was around 62% and the compressive strength (8 MPa) was close to trabecular bone. No cytotoxicity of composite resulted from live/dead staining of osteoblasts cultured on substrates.

Effect of Calcium Sulfate Hemihydrate on Structure and Properties of Silk Fibroin/Calcium Phosphate Composites

2012 ◽  
Vol 550-553 ◽  
pp. 1139-1143 ◽  
Author(s):  
Meng Zhang ◽  
Rui Juan Xie ◽  
Yang Yang Huang
Keyword(s):  
Compressive Strength ◽  
Calcium Phosphate ◽  
Silk Fibroin ◽  
Calcium Sulfate ◽  
Setting Time ◽  
Structure And Properties ◽  
Rapid Degradation ◽  
Setting Reaction ◽  
Natural Bone ◽  
Calcium Sulfate Hemihydrate

In this paper, calcium sulfate hemihydrate (CSH) was added into silk fibroin/calcium phosphate (SF/CP) composites. The macropores formed by the SF was connected by micropores formed from rapid degradation of CSH, so that the structure of the composites is more close to the natural bone. The results indicated that the range of pore sizes around 30 - 308 microns were formed in the composites by SF. Compared to SF/CP composites without CSH, the injectability decreased, but the rate were both above 90%; the setting time increased, but were both less than 16min; the porosity increased. When the proportion of CSH was greater than 10%, the morphology of the product of setting reaction, i.e. the hydroxyapatite (HA) crystals, was influenced. When the proportion of CSH was less than 10%, the HA crystals appeared to be needle-like and plate-like crystals. When the proportion of CSH was greater than 10%, HA crystals were needle-like. The added amount of CSH had significant effects on compressive strength and work-of-compressive. The compressive strength and work-of-compressive decreased with increasing of CSH content in the composites.

Primary Study of an Injectable In Situ Composite of Collagen/Calcium Phosphate Porous Scaffold for Bone Substitute

2006 ◽  
Vol 309-311 ◽  
pp. 857-860 ◽  
Author(s):  
Q. Yao ◽  
Dong Xiao Li ◽  
K.W. Liu ◽  
Bo Zhang ◽  
H. Li ◽  
...  
Keyword(s):  
Compressive Strength ◽  
Calcium Phosphate ◽  
Ph Value ◽  
Porous Scaffold ◽  
Setting Time ◽  
Primary Study ◽  
In Situ Composite ◽  
Setting Process ◽  
Main Material

This study was to develop an injectable biocompatible and porous calcium phosphate collagen composite cement scaffold by in situ setting. TTCP was prepared as main material of the CPC powder, and the collagen solution was added into the phosphoric acid directly to form the liquid phase. The injectable time (tI), setting time (tS) and setting temperature (TS), along with the PH value were recorded during the setting process. The compressive strength, morphology and porosity were tested. With the increase of collagen, this novel CPC get a tI of 5mins to 8mins, tS of 20mins to 30mins, compressive strength from 1.5MPa to 4MPa, and the porosity from 40% to 60%. This study gave a possibility to form a porous scaffold of collagen/CPC composite with the nature of injectability and setting in situ.

The pH-Dependent Properties of the Biphasic Calcium Phosphate for Bone Cements

2014 ◽  
Vol 21 ◽  
pp. 3-16 ◽  
Author(s):  
Nuan La Ong Srakaew ◽  
Sirirat Tubsungnoen Rattanachan
Keyword(s):  
Compressive Strength ◽  
Liquid Phase ◽  
Calcium Phosphate ◽  
Phase Analysis ◽  
Calcium Phosphate Cement ◽  
Biphasic Calcium Phosphate ◽  
Setting Time ◽  
Bone Cements ◽  
Apatite Formation ◽  
Apatite Cement

Self-setting calcium phosphate cement (CPC) has been used in bone repair and substitution due to their excellent biocompatibility, bioactive as well as simplicity of preparation and use. The inherent brittleness and slow degradation are the major disadvantages for the use of calcium phosphate cements. To improve the degradation for the traditional CPC, the apatite cement formula incorporated with β-tricalcium phosphate (β-TCP) with varying concentration were studied and the effect of the pH value of liquid phase on the properties of this new calcium phosphate cement formula was evaluated. The apatite cements containing β-TCP for 10 and 40 wt.% were mixed into the aqueous solution with different pH values and then aging in absolute humidity at 37°C for 7 days. The setting time and phase analysis of the biphasic calcium phosphate were determined as compared to the apatite cement. For proper medical application, the compressive strength, the phase analysis and the degradation of the CPC samples at pH 7.0 and 7.4 were evaluated after soaking in the simulated body fluid (SBF) at 37°C for 7 days. The results indicated that the properties of the samples such as the setting time, the compressive strength related to the phase analysis of the set cements. The high degradation of the CPC was found in the cement with increasing β-TCP addition due to the phase after setting. Apatite formation with oriented plate-like morphology was also found to be denser on the surface of the biphasic bone cements after soaking in SBF for 7 days. The obtained results indicated that the cement containing β-TCP mixed with the liquid phase at pH 7.4 could be considered as a highly biodegradable and bioactive bone cement, as compared to the traditional CPC.

Biodegradable Bone Cement Using Calcium Phosphate Glass

2006 ◽  
Vol 309-311 ◽  
pp. 861-864 ◽  
Author(s):  
Byung Hyun Lee ◽  
Min Chul Kim ◽  
Kyoung Nam Kim ◽  
Kwang Mahn Kim ◽  
Seong Ho Choi ◽  
...  
Keyword(s):  
Weight Loss ◽  
Compressive Strength ◽  
Calcium Phosphate ◽  
Simulated Body Fluid ◽  
Dissolution Rate ◽  
Phosphate Glass ◽  
Body Fluid ◽  
Setting Time ◽  
Ageing Test ◽  
Dynamic Assay

In preliminary ageing test, the cement using only calcium phosphate glass as power phase cracked with 1 day in simulated body fluid because of high dissolution rate of the cement. We added 30 wt% of either β-TCP or HA to 70 wt% calcium phosphate glass as powder phase to control the dissolution rate of the cement and performed in vitro ageing test in simulated body fluid by dynamic protocol as well as static protocol to confirm the possibility of controlling. Adding either β-TCP or HA to the cement increases the setting time and decreases the compressive strength. In dynamic assay, the pH of extract is maintained over 7. However, pH decreased to around 5 in static assay. Therefore, weight loss by static protocol continuously increased for 14 days, while weight loss by dynamic protocol almost saturated. In XRD patterns of ageing cements, CaO peaks appeared. CaO peak was maximized most lately in dynamic assay of the cement adding HA and within 7 days, the cement adding HA showed higher weight loss. It is indicated that CaO formed in surface of the cement hinder the dissolution of the cement. In addition, compressive strength increased when the CaO peak was maximized.

scholarly journals Polymeric-Calcium Phosphate Cement Composites-Material Properties:In VitroandIn VivoInvestigations

2010 ◽  
Vol 2010 ◽  
pp. 1-14 ◽  
Author(s):  
Rania M. Khashaba ◽  
Mervet M. Moussa ◽  
Donald J. Mettenburg ◽  
Frederick A. Rueggeberg ◽  
Norman B. Chutkan ◽  
...  
Keyword(s):  
Calcium Phosphate ◽  
Calcium Phosphate Cement ◽  
Setting Time ◽  
Cement Composites ◽  
Tetracalcium Phosphate ◽  
Methyl Vinyl Ether ◽  
Orthopedic Applications ◽  
Hydroxyapatite Cement

New polymeric calcium phosphate cement composites (CPCs) were developed. Cement powder consisting of 60 wt% tetracalcium phosphate, 30 wt% dicalcium phosphate dihydrate, and 10 wt% tricalcium phosphate was combined with either 35% w/w poly methyl vinyl ether maleic acid or polyacrylic acid to obtain CPC-1 and CPC-2. The setting time and compressive and diametral tensile strength of the CPCs were evaluated and compared with that of a commercial hydroxyapatite cement.In vitrocytotoxicity andin vivobiocompatibility of the two CPCs and hydroxyapatite cement were assessed. The setting time of the cements was 5–15 min. CPC-1 and CPC-2 showed significantly higher compressive and diametral strength values compared to hydroxyapatite cement. CPC-1 and CPC-2 were equivalent to Teflon controls after 1 week. CPC-1, CPC-2, and hydroxyapatite cement elicited a moderate to intense inflammatory reaction at 7 days which decreased over time. CPC-1 and CPC-2 show promise for orthopedic applications.

scholarly journals Injectable Enzymatically Hardened Calcium Phosphate Biocement

2020 ◽  
Vol 11 (4) ◽  
pp. 74
Author(s):  
Lubomir Medvecky ◽  
Radoslava Štulajterová ◽  
Maria Giretova ◽  
Lenka Luptakova ◽  
Tibor Sopčák
Keyword(s):  
Compressive Strength ◽  
Calcium Phosphate ◽  
Setting Time ◽  
Microstructural Analysis ◽  
Chemical Properties ◽  
Gene Expressions ◽  
Cement Pastes ◽  
Anionic Polyelectrolyte ◽  
Simple Possibility

(1) Background: The preparation and characterization of novel fully injectable enzymatically hardened tetracalcium phosphate/monetite cements (CXI cements) using phytic acid/phytase (PHYT/F3P) hardening liquid with a small addition of polyacrylic acid/carboxymethyl cellulose anionic polyelectrolyte (PAA/CMC) and enhanced bioactivity. (2) Methods: Composite cements were prepared by mixing of calcium phosphate powder mixture with hardening liquid containing anionic polyelectrolyte. Phase and microstructural analysis, compressive strength, release of ions and in vitro testing were used for the evaluation of cement properties. (3) Results: The simple possibility to control the setting time of self-setting CXI cements was shown (7–28 min) by the change in P/L ratio or PHYT/F3P reaction time. The wet compressive strength of cements (up to 15 MPa) was close to cancellous bone. The increase in PAA content to 1 wt% caused refinement and change in the morphology of hydroxyapatite particles. Cement pastes had a high resistance to wash-out in a short time after cement mixing. The noncytotoxic character of CX cement extracts was verified. Moreover, PHYT supported the formation of Ca deposits, and the additional synergistic effect of PAA and CMC on enhanced ALP activity was found, along with the strong up-regulation of osteogenic gene expressions for osteopontin, osteocalcin and IGF1 growth factor evaluated by the RT-qPCR analysis in osteogenic αMEM 50% CXI extracts. (4) Conclusions: The fully injectable composite calcium phosphate bicements with anionic polyelectrolyte addition showed good mechanical and physico-chemical properties and enhanced osteogenic bioactivity which is a promising assumption for their application in bone defect regeneration.

Improving the anti-washout property of calcium phosphate cement by introducing konjac glucomannan/κ-carrageenan blend

2019 ◽  
Vol 33 (8) ◽  
pp. 1094-1104 ◽  
Author(s):  
Guowen Qian ◽  
Xingmei Li ◽  
Fupo He ◽  
Jiandong Ye
Keyword(s):  
Compressive Strength ◽  
Calcium Phosphate ◽  
Calcium Phosphate Cement ◽  
Setting Time ◽  
Konjac Glucomannan ◽  
Water Soluble ◽  
Mouse Bone Marrow ◽  
Human Cancellous Bone ◽  
Marrow Mesenchymal Stem Cells

Anti-washout calcium phosphate cement (CPC) was prepared by dissolving water-soluble konjac glucomannan (KGM) and κ-carrageenan (KC) blend in the cement liquid. The anti-washout property, setting time, compressive strength and in vitro cytocompatibility of the CPC modified with KGM/KC blend were evaluated. The results indicated that the CPC pastes modified with KGM/KC blend exhibited excellent anti-washout property. The addition of KGM/KC blend shortened the setting time and increased the injectability of CPC. Although the introduction of KGM/KC blend reduced the compressive strength of CPC, the compressive strength still surpassed that of human cancellous bone. The optimal KGM/KC mass ratio was 2:8, with which the modified cement exhibited the most efficient washout resistance and the highest compressive strength. The introduction of KGM/KC blend obviously promoted the proliferation of mouse bone marrow mesenchymal stem cells. This anti-washout CPC modified by KGM/KC blend with excellent in vitro cytocompatibility will have good prospects for application in bone defect repair.

Sign in / Sign up

Export Citation Format

Share Document