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.

Effect of Silk Fibroin on the Properties of Calcium Phosphate Cement

2011 ◽  
Vol 175-176 ◽  
pp. 100-104 ◽  
Author(s):  
Biao Wang ◽  
Rui Juan Xie ◽  
Qiong Wan ◽  
Yang Wang ◽  
Yang Yang Huang
Keyword(s):  
Calcium Phosphate ◽  
Silk Fibroin ◽  
Calcium Phosphate Cement ◽  
Setting Time ◽  
Testing Machine ◽  
X Ray Diffraction ◽  
Acicular Crystal ◽  
Silk Fibroin Fiber ◽  
Universal Testing ◽  
Distinct Increase

To improve the physicochemical properties of calcium phosphate cement (CPC), silk fibroin (SF) in the different forms were added into CPC. The structure of the composites was studied by X-ray diffraction. The setting time was investigated by ISO Cement Standard Consistency Instrument. Scanning Electron Microscope was used to observe the surface morphology. Mechanical properties of samples were tested by Instron Universal Testing Machine. The results indicated that acicular crystal of hydroxyapatite (HA) was formed in the hardening body of both CPC with SF and the pure CPC. Addition of SF had no significant effect on the structure of SF/CPC composite. The setting time of CPC with SF was significantly shorter than that of the pure CPC (30.3 mins). The setting time of CPC by adding silk fibroin powder I (SFP) and silk fibroin fiber (SFF) was greatly shortened, which was only 11.7 minutes. The setting time of CPC with SFP decreased approximately by 1/3, while the setting time of the CPC with SFF decreased nearly by 1/2. With the adding of SF, the compressive strength of CPC increased significantly. There was a distinct increase in the work-of-compressive of CPC with the adding of SFF.

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.

Physicochemical and Mechanical Properties of Composite of Chitosan Microspheres/Calcium Phosphate Cement

2007 ◽  
Vol 336-338 ◽  
pp. 1654-1657
Author(s):  
Rui Liu ◽  
Li Min Dong ◽  
Qing Feng Zan ◽  
Chen Wang ◽  
Jie Mo Tian
Keyword(s):  
Mechanical Properties ◽  
Compressive Strength ◽  
Calcium Phosphate ◽  
Bone Cement ◽  
Setting Time ◽  
Chemical Properties ◽  
Phase Evolution ◽  
Chitosan Microspheres ◽  
Setting Times ◽  
Calcium Phosphate Bone Cement

The aim of this work is to improve the mechanical properties of calcium phosphate bone cement (CPC) by appending chitosan microspheres to CPC base. That chitosan degrades rapidly than bone cement has been proved by previous investigations. Porous CPC has low compressive strength because of the pores in it weakening the structure. Additive chitosan microspheres can improve the mechanical properties by bearing the compress with the CPC base and produce pores after degradation. This study investigates the effect of chitosan microspheres on the setting time, mechanical properties, phase evolution and morphology of CPC. The additive proportion of chitosan microspheres ranges from 0 wt% to 30 wt%. Compared with original CPC, the modified CPC has higher compressive strength, without significantly affecting the chemical properties. The phase composition of the CPC is tested by XRD. The microstructures of CPC are observed using SEM. The final setting times range from 5~15 minutes and can be modulated by using different liquid and powder (L/P) ratio.

Characterization of α/β-TCP Based Injectable Calcium Phosphate Cement as a Potential Bone Substitute

2012 ◽  
Vol 529-530 ◽  
pp. 157-160 ◽  
Author(s):  
Kemal Sariibrahimoglu ◽  
Joop G.C. Wolke ◽  
Sander C.G. Leeuwenburgh ◽  
John A. Jansen
Keyword(s):  
Compressive Strength ◽  
Calcium Phosphate ◽  
Setting Time ◽  
Surrounding Tissue ◽  
Calcium Phosphate Cements ◽  
Apatite Cement ◽  
Tcp Phase

Calcium phosphate cements (CPCs) can be a suitable scaffold material for bone tissue engineering because of their osteoconductivity and perfect fit with the surrounding tissue when injected in situ. However, the main disadvantage of hydroxyapatite (HA) forming CPC is its slow degradation rate, which hinders complete bone regeneration. A new approach is to use hydraulic apatite cement with mainly α/β-tricalciumphosphate (TCP) instead of α-TCP. After hydrolysis the α/β-TCP transforms in a partially non-absorbable HA and a completely resorbable β-TCP phase. Therefore, α-TCP material was thermally treated at several temperatures and times resulting in different α/β-TCP ratios. In this experiment, we developed and evaluated injectable biphasic calcium phosphate cements (BCPC) in vitro. Biphasic α/β-TCP powder was produced by heating α-TCP ranging from 1000-11250°C. Setting time and compressive strength of the CPCs were analyzed after soaking in PBS for 6 weeks. Results demonstrated that the phase composition can be controlled by the sintering temperature. Heat treatment of α-TCP, resulted in 100%, 75% and 25% of α-to β-TCP transformation, respectively. Incorporation of these sintered BCP powder into the cement formulation increased the setting time of the CPC paste. Compressive strength decreased with increasing β-TCP content. In this study, biphasic CPCs were produced and characterized in vitro. This injectable biphasic CPC presented comparable properties to an apatitic CPC.

Preparation and Characterization of the Porous Hydroxyapatite/Silk Fibroin Composite Scaffolds with Interconnected Ducts

2008 ◽  
Vol 368-372 ◽  
pp. 1190-1193 ◽  
Author(s):  
Jing Wang ◽  
Mu Qin Li ◽  
Xiang Cai Meng ◽  
Guang Wu Wen
Keyword(s):  
Compressive Strength ◽  
Silk Fibroin ◽  
Freeze Drying ◽  
Composite Scaffold ◽  
Drying Process ◽  
X Ray Diffraction ◽  
Composite Scaffolds ◽  
Porous Hydroxyapatite ◽  
X Ray

Porous hydroxyapatite (HA) bioceramic matrix with interconnected ducts was obtained using a porogen burnout technique at 1200°C. The HA/silk fibroin (SF) composite scaffolds were developed with the SF sponges formed inside the pores and ducts of the bioceramics by first introducing HA/SF slurries into the pores and ducts followed by a freeze-drying process. Phase components and morphology of materials were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. Porosity was measured by Archimedean method. Compressive strength was also measured. The simulated body fluids (SBF) experiments were conducted to evaluate bioactivity. The results show that hydroxyapatite is the main phase compositions after sintering at 1200°C. The porosity of composite scaffolds reaches 70%~80%. The sizes of pores and ducts of HA matrix range from 150μm to 400μm and the pore sizes of SF sponges formed inside the macroporous structure of bioceramics are approximately 100μm,a structure favorable for bone tissue in-growth. The compressive strength of the composite scaffolds is greatly improved in comparison with that of HA matrix. In the SBF tests, a layer of randomly oriented apatite crystals form on the scaffold surface after sample immersion in SBF. The cell culture experiments show that the osteoblast cells are attached and proliferated on the surface of the composite scaffold, which suggest good bioactivity and cellular compatibility of the composite material.

Behavior of Cement Pastes and Mortar Containing Phosphogypsum

2015 ◽  
Vol 668 ◽  
pp. 181-188 ◽  
Author(s):  
Hanan El Nouhy ◽  
Enas Khattab ◽  
Sayieda Zeedan
Keyword(s):  
Compressive Strength ◽  
Setting Time ◽  
Blended Cement ◽  
X Ray Diffraction ◽  
Cement Pastes ◽  
Initial Setting Time ◽  
Second Stage ◽  
Setting Times ◽  
Initial Setting ◽  
Two Stages

The aim of this study is to investigate the effects of phosphogypsum on the properties of both cement pastes and mortars. Normal Portland cement CEM Ι 32,5N, Limestone Blended cement CEM ΙΙ B-L32,5N, and Slag cement CEM ΙΙ A-S32,5N were used. These cements were partially substituted by 0,2,4,6,8,10,and 15% of phosphogypsum. The test program was divided to two stages. In the first stage, tests were conducted according to BSEN 196, namely setting times (initial and final), soundness, and compressive strength (at ages 7 and 28 days). In the second stage, X-ray diffraction (XRD), and scanning electron microscope (SEM) were conducted on selected mixes from first stage. The results show that the three types of cements with the various replacement percentages of phosphogypsum met the limit of initial setting time, as well as, provided soundness of 2 mm. Also, in terms of compressive strength, it was proven, that it is possible to partially replace the three tested types of cements by phosphogypsum by up to 8%and 15% with regard to cement/sand ratio of (1:3) and (1:2) respectively.

Development of Injectable Calcium Phosphate Cement Adding with ZrO2

2007 ◽  
Vol 361-363 ◽  
pp. 347-350
Author(s):  
J.Y. Gong ◽  
Shu Xin Qu ◽  
Q. Cui ◽  
Jie Weng
Keyword(s):  
Compressive Strength ◽  
Calcium Phosphate ◽  
Setting Time ◽  
X Ray Diffraction ◽  
Liquid Component ◽  
X Ray ◽  
Initial Setting Time ◽  
Mass Fractions ◽  
Initial Setting ◽  
Diffraction Peaks

In the present study, ZrO2 was added into the injectable calcium phosphate cements (CPCs) to improve their mechanical strength. Different mass fractions of ZrO2 (5 %, 10 %, 15 %, 20%) were mixed with the powder components consisted of tricalcium phosphate (α-TCP) and hydroxyapatite (HA). Then formed the paste via adding the liquid component consisted of citric acid. The compressive strength, the injectability, the initial setting time and finial time of CPC were measured, respectively. X-ray diffraction (XRD) was employed to analyse the phase of as-prepared CPC. Scanning Electron Microscope (SEM) and Energy dispersive spertrum (EDS) were used to observe the morphology and indicate the element components of CPC. The compressive strength of ZrO2-CPC was higher than that of CPC without added ZrO2. The compressive strength got the maximal when the mass fraction of ZrO2 was 15%. It had no effect on the injectability with adding ZrO2, which were 89 % to 92 %. It had a slight down-regulation of the initial and final setting time with adding ZrO2. SEM showed that there was amounts needle-like substance in CPC, which might be related to the improvement of compressive strength of CPC. XRD showed that there were HA, a few of α-TCP and ZrO2 diffraction peaks in CPCs. The present results indicate that it is feasible to improve the compressive strength of injectable CPC via adding ZrO2.

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.

Development of a New Injectable Calcium Phosphate Cement That Contains Modified Starch

2007 ◽  
Vol 330-332 ◽  
pp. 843-846 ◽  
Author(s):  
Ling Chen ◽  
Hong Xiang ◽  
Xiao Xi Li ◽  
Jian Dong Ye ◽  
Xiu Peng Wang ◽  
...  
Keyword(s):  
Compressive Strength ◽  
Calcium Phosphate ◽  
Calcium Phosphate Cement ◽  
Setting Time ◽  
Phase Evolution ◽  
Modified Starch ◽  
Compact Structure ◽  
Acicular Crystal ◽  
Significant Difference ◽  
Performance Setting

In this study modified starch were used as anti-washout promoters of injectable calcium phosphate cement (CPC) and the effects of the modified starch on the injectability, anti-washout performance, setting time, compressive strength, phase evolution and microstructure of this cement were investigated. The injectability of the cement was improved by adding the modified starch (0.5-2.0%). After mixing with modified starch (0.5-2.0%), the cement showed better anti-washout performance than that without modified starch after immersed and shaken in SBF. Especially, when the content of the modified starch was 1.0%, the remaining percentage of the cement was reached to 92.6%, but only 5.9% of the CPC paste remained and set for the sample without modified starch after shaken for 2 hrs. The compressive strength of cements significantly increased from 44 MPa to 54 MPa when 0.5% of modified starch was added. And a slight increase on the mechanical strength can be observed for other concentrations. Powder X-ray diffraction analysis revealed no significant difference for the conversion of the cement to hydroxyapatite for any concentrations of modified starches. The influence of the modified starch on the microstructure of the set cement was also studied. The results showed the modified starch would reduce the acicular crystal size of hydroxyapatite accompanied with little flaky crystals generation and made a compact structure. It is concluded that modified starch, a suitable anti-washout promoter, improved the performance of CPC.

Preparation and Characterization of Silk Fibroin/Hydroxyapatite Bilayer Scaffolds

2011 ◽  
Vol 415-417 ◽  
pp. 1810-1815 ◽  
Author(s):  
Jian Bing Liu ◽  
Qiang Tang ◽  
Shen Zhou Lu ◽  
Ceng Zhang ◽  
Ming Zhong Li
Keyword(s):  
Silk Fibroin ◽  
Electron Excitation ◽  
Mouse Bone Marrow ◽  
High Porosity ◽  
X Ray Diffraction ◽  
Tissue Engineering Scaffolds ◽  
Molding Method ◽  
Isostatic Compaction ◽  
Fibroin Solution

When the articular cartilage defect accompanies with the subchondral bone defect, using bilayer scaffolds which can integrate with surrounding host cartilage and bone tissue respectively as the tissue engineering scaffolds will be conducive to the repair of tissue defects. This paper reports a new method for preparing bilayer scaffolds. Firstly, hydroxyapatite (HA)/silk fibroin(SF) composite porous materials which have high porosity were prepared by a isostatic compaction molding method, then it was fully immersed in silk fibroin solution, and finally SF/HA bilayer scaffolds were obtained by freeze-drying. The structure of the bilayer scaffolds were investigated through scanning electron microscopy, X-ray diffraction, Fourier transform-infrared spectroscopy, electron excitation spectroscopy and electron microprobe. The results indicated that the upper layer of SF/HA bilayer scaffolds is porous SF component, the under layer is the porous HA/SF composite component and the interface of the two layer is closely connected. Furthermore, mesenchymal stem cells from mouse bone marrow were seeded into the bilayer scaffolds and the results showed that the cells had a well adhesion and growth after culturing for 3 days.

Sign in / Sign up

Export Citation Format

Share Document