A quantitative analysis of dicalcium silicate synthesized via different sol-gel methods

Calcium silicate (CS) is a main component of Portland cement and is responsible for the strength development. Recent research has shown that dicalcium silicate cement (CSC) is bioactive and is a potential candidate for bone replacement. Traditionally, dicalcium silicate powder is synthesized by a solid state reaction or a sol-gel method. The solid-state reaction, however, usually needs a higher temperature and a longer calcination time. Furthermore, the dicalcium silicate powder made by the sol-gel method is not pure, and contains a significant quantity of CaO which is harmful to the strength and biological properties of the CSC. The Pechini technique is an alternative, low temperature polymeric precursor route for synthesis of high purity powders. In this study, purer CS powder was synthesized via the Pechini method by calcination at 800°C for 3h. DSC-TGA, XRD, SEM were used for characterization of CS powder and the hydrated cement. The DSC-TGA curves showed that the main exothermic peak was at 479°C and the total mass loss was 79.2%. The XRD patterns of CSC after hydration for 7, 14, and 35 days illustrated that dicalcium silicate hydrate (Ca1.5SiO3.5·xH2O, C-S-H) was formed in the hardened CS paste. The XRD peaks on the diffraction pattern of the C-S-H of the day 35 sample were of greater intensity than those at day 7 and day 14. This demonstrates that the hydration speed was slow and complete hydration could take more than one month. Flake-like crystals were observed on scanning electron micrographs following hardening. The degradation study result showed that there was no mass loss of CSC after the samples were soaked into phosphate buffered saline (PBS) for 40 days. The silicon assay revealed that orthosilicic acid could be released from CSC after the samples were soaked in simulated body fluid (SBF). Silicon is known to be critical to skeletal mineralization. The existence of silicon may stimulate the proliferation of bone and activate cells to produce bone. Investigation of cell attachment confirmed that the MC-3T3 cells attached well to the surfaces of CSC after seeding.

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Application of Sol-Gel Method to Investigate the Influence of P2O5 on the Course of Reactions in CaO-SiO2 System

Materials Science Forum ◽

10.4028/www.scientific.net/msf.851.92 ◽

2016 ◽

Vol 851 ◽

pp. 92-97

Author(s):

Jan Baraček ◽

Martin Palou ◽

Jiří Másilko ◽

Jaromír Wasserbauer ◽

František Šoukal ◽

...

Keyword(s):

Calcium Phosphate ◽

Calcium Silicate ◽

Silicon Oxide ◽

Sol Gel ◽

Dicalcium Silicate ◽

Local Analysis ◽

X Ray Diffraction ◽

Sol Gel Process ◽

Calcium Silicates ◽

Sol Gel Synthesis

The effect of P2O5 addition on the calcium silicate phase equilibrium during the sol-gel synthesis of dicalcium silicate was investigated using Scanning electron microscope and X-ray diffraction. It is established that phosphorous oxide can form solid solution with dicalcium silicate, but its causes the formation of phosphatic calcium silicate phases such as Ca14.92 (PO4)2.35(SiO4)5.65 and 5CaO.SiO2.P2O5 also. Local analysis has demonstrated the presence of calcium phosphate epicenters containing silicon oxide and calcium silicate zones with minimum content of phosphorous oxide and intermediary areas of various phosphatic calcium silicates. The formation of two distinct islets of calcium silicate and calcium phosphate is due to the affinity between acid oxides (SiO2, P2O5) and basic one (CaO) during sol-gel process. Then, the formation of various phosphatic calcium silicates result from the diffusion of P2O5 towards calcium silicate and that of SiO2 towards calcium phosphate.

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An Improved Quantitative Image Analyser

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100078663 ◽

1977 ◽

Vol 35 ◽

pp. 226-227

Author(s):

J.P. Fallon ◽

P.J. Gregory ◽

C.J. Taylor

Keyword(s):

Feature Extraction ◽

Quantitative Analysis ◽

Frequency Content ◽

General Sense ◽

Physical Measurements ◽

Quantitative Image ◽

Image Analyser ◽

Automatic Methods ◽

Quantitative Results

Quantitative image analysis systems have been used for several years in research and quality control applications in various fields including metallurgy and medicine. The technique has been applied as an extension of subjective microscopy to problems requiring quantitative results and which are amenable to automatic methods of interpretation.Feature extraction. In the most general sense, a feature can be defined as a portion of the image which differs in some consistent way from the background. A feature may be characterized by the density difference between itself and the background, by an edge gradient, or by the spatial frequency content (texture) within its boundaries. The task of feature extraction includes recognition of features and encoding of the associated information for quantitative analysis.Quantitative Analysis. Quantitative analysis is the determination of one or more physical measurements of each feature. These measurements may be straightforward ones such as area, length, or perimeter, or more complex stereological measurements such as convex perimeter or Feret's diameter.

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Quantification of Silica Uptake by Alveolar Macrophages - An Emperical Scanning Electron Microprobe Method

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100054297 ◽

1982 ◽

Vol 40 ◽

pp. 332-333

Author(s):

V. V. Damiano ◽

R. P. Daniele ◽

H. T. Tucker ◽

J. H. Dauber

Keyword(s):

Quantitative Analysis ◽

Alveolar Macrophages ◽

Bulk Sample ◽

Silica Particles ◽

Empirical Method ◽

Phagocytic Cells ◽

Calibration Standards ◽

X Ray ◽

Accurate Quantitative Analysis ◽

Scanning Electron

An important example of intracellular particles is encountered in silicosis where alveolar macrophages ingest inspired silica particles. The quantitation of the silica uptake by these cells may be a potentially useful method for monitoring silica exposure. Accurate quantitative analysis of ingested silica by phagocytic cells is difficult because the particles are frequently small, irregularly shaped and cannot be visualized within the cells. Semiquantitative methods which make use of particles of known size, shape and composition as calibration standards may be the most direct and simplest approach to undertake. The present paper describes an empirical method in which glass microspheres were used as a model to show how the ratio of the silicon Kα peak X-ray intensity from the microspheres to that of a bulk sample of the same composition correlated to the mass of the microsphere contained within the cell. Irregular shaped silica particles were also analyzed and a calibration curve was generated from these data.

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Lateral resolution of the electron microbeam analysis

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100109859 ◽

1978 ◽

Vol 36 (1) ◽

pp. 542-543

Author(s):

H.J. Dudek

Keyword(s):

Quantitative Analysis ◽

Depth Resolution ◽

Lateral Resolution ◽

Cylindrical Particle ◽

Correction Procedure ◽

X Ray ◽

Element Concentrations ◽

Microbeam Analysis ◽

The Matrix

The chemical inhomogenities in modern materials such as fibers, phases and inclusions, often have diameters in the region of one micrometer. Using electron microbeam analysis for the determination of the element concentrations one has to know the smallest possible diameter of such regions for a given accuracy of the quantitative analysis.In th is paper the correction procedure for the quantitative electron microbeam analysis is extended to a spacial problem to determine the smallest possible measurements of a cylindrical particle P of high D (depth resolution) and diameter L (lateral resolution) embeded in a matrix M and which has to be analysed quantitative with the accuracy q. The mathematical accounts lead to the following form of the characteristic x-ray intens ity of the element i of a particle P embeded in the matrix M in relation to the intensity of a standard S

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An example of spectrum imaging used for comparison of EELS quantitative analysis techniques on Al-Li

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s042482010008794x ◽

1991 ◽

Vol 49 ◽

pp. 726-727

Author(s):

John A. Hunt

Keyword(s):

Quantitative Analysis ◽

Large Data ◽

Difference Spectrum ◽

Large Data Sets ◽

Foil Thickness ◽

Data Sets ◽

Analysis Techniques ◽

Spectrum Imaging ◽

Normal Spectrum ◽

Electron Energy Loss

Spectrum-imaging is a useful technique for comparing different processing methods on very large data sets which are identical for each method. This paper is concerned with comparing methods of electron energy-loss spectroscopy (EELS) quantitative analysis on the Al-Li system. The spectrum-image analyzed here was obtained from an Al-10at%Li foil aged to produce δ' precipitates that can span the foil thickness. Two 1024 channel EELS spectra offset in energy by 1 eV were recorded and stored at each pixel in the 80x80 spectrum-image (25 Mbytes). An energy range of 39-89eV (20 channels/eV) are represented. During processing the spectra are either subtracted to create an artifact corrected difference spectrum, or the energy offset is numerically removed and the spectra are added to create a normal spectrum. The spectrum-images are processed into 2D floating-point images using methods and software described in [1].

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Microstructural characterization of laser-melted/roller-quenched dicalcium silicate

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100104972 ◽

1988 ◽

Vol 46 ◽

pp. 582-583

Author(s):

C. J. Chan ◽

K. R. Venkatachari ◽

W. M. Kriven ◽

J. F. Young

Keyword(s):

Particle Size ◽

Raw Materials ◽

Shape Change ◽

Microstructural Characterization ◽

Particle Size Effect ◽

Dicalcium Silicate ◽

Laser Melting ◽

Uniform Size ◽

Cell Shape Change ◽

Wide Range

Dicalcium silicate (Ca2SiO4) is a major component of Portland cement. It has also been investigated as a potential transformation toughener alternative to zirconia. It has five polymorphs: α, α'H, α'L, β and γ. Of interest is the β-to-γ transformation on cooling at about 490°C. This transformation, accompanied by a 12% volume increase and a 4.6° unit cell shape change, is analogous to the tetragonal-to-monoclinic transformation in zirconia. Due to the processing methods used, previous studies into the particle size effect were limited by a wide range of particle size distribution. In an attempt to obtain a more uniform size, a fast quench rate involving a laser-melting/roller-quenching technique was investigated.The laser-melting/roller-quenching experiment used precompacted bars of stoichiometric γ-Ca2SiO4 powder, which were synthesized from AR grade CaCO3 and SiO2xH2O. The raw materials were mixed by conventional ceramic processing techniques, and sintered at 1450°C. The dusted γ-Ca2SiO4 powder was uniaxially pressed into 0.4 cm x 0.4 cm x 4 cm bars under 34 MPa and cold isostatically pressed under 172 MPa. The γ-Ca2SiO4 bars were melted by a 10 KW-CO2 laser.

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The use of a Bent Grid to Improve the take-Off Angle for Electron Probe Analysis

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100091780 ◽

1976 ◽

Vol 34 ◽

pp. 360-361

Author(s):

Delbert E. Philpott ◽

David Leaffer

Keyword(s):

Quantitative Analysis ◽

Tilt Angle ◽

Count Rate ◽

Electron Probe ◽

Open Area ◽

Electron Probe Analysis ◽

Background Ratio ◽

Probe Analysis

There are certain advantages for electron probe analysis if the sample can be tilted directly towards the detector. The count rate is higher, it optimizes the geometry since only one angle need be taken into account for quantitative analysis and the signal to background ratio is improved. The need for less tilt angle may be an advantage because the grid bars are not moved quite as close to each other, leaving a little more open area for observation. Our present detector (EDAX) and microscope (Philips 300) combination precludes moving the detector behind the microscope where it would point directly at the grid. Therefore, the angle of the specimen was changed in order to optimize the geometry between the specimen and the detector.

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Solving the mechanisms responsible for organelle behavior in vivo by same-cell correlative light and electron microscopy

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100120473 ◽

1992 ◽

Vol 50 (1) ◽

pp. 14-15

Author(s):

Conly L. Rieder

Keyword(s):

Electron Microscopy ◽

Quantitative Analysis ◽

Light Microscopy ◽

Living Cell ◽

Light And Electron Microscopy ◽

Time Behavior ◽

Dynamic Interactions ◽

Positive Identification ◽

Cellular Components

The behavior of many cellular components, and their dynamic interactions, can be characterized in the living cell with considerable spatial and temporal resolution by video-enhanced light microscopy (video-LM). Indeed, under the appropriate conditions video-LM can be used to determine the real-time behavior of organelles ≤ 25-nm in diameter (e.g., individual microtubules—see). However, when pushed to its limit the structures and components observed within the cell by video-LM cannot be resolved nor necessarily even identified, only detected. Positive identification and a quantitative analysis often requires the corresponding electron microcopy (EM).

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