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INVESTIGATIONS ON SELECTED BIOACTIVE GLASSES AND GLASS-CERAMICS CONTAINING IRON OXIDE

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Introduction 1

General theory of Biomaterials

A more precise definition of a biomaterial was given in 1986 at a consensus conference of the European Biomaterials Association, when a biomaterial was defined [8] as “inanimate material used in a medical device and intended to interact with a biological system”. The response of the material to physical stimuli must be similar to that of the tissue it replaces.

Types of tissue attachment of biomaterials ….…

The larger interface area between the implant and the tissue increases the resistance to movement of the device in the tissue. The concept of bioactivity has been defined as "a bioactive material is one that elicits a specific biological response at the interface of the material leading to the formation of a bond between the tissues and the material" [14].

Bioactive materials

  • Bioglasses
  • Bone minerals
  • Bioglass ceramics

In fact, glass ceramics are widely used as a medical device, but their use as implants in the body is relatively new. Several types of bioactive glass ceramics have been developed, including A/W bioactive glass ceramics, ceravital glass ceramics, and machined glass ceramics.

Tests for biocompatibility

  • In vivo test
  • In vitro test
    • Simulated body fluid (SBF)
    • Mechanism of HCA layer deposition

Furthermore, in 1990, they showed that in vivo apatite formation on the surface of A/W glass ceramics could be reproduced in acellular SBF with ion concentrations almost identical to those in human blood plasma, but not in Tris buffer. solution [44-45]. 46] also independently confirmed the formation of apatite on the surface of Bioglass 45S5 glass treated in SBF.

Survey of literature on bioglass and bioactive glass-ceramics

74] reported the in vitro bioactivity in glass and glass ceramics of the CaO-SiO2-P2O5-MgO-CaF2 system. It was found that the main crystalline phases in glass ceramics are Ca(PO3)2 and Ca2P2O7.

Preparative methods and their characteristics

  • Melt derived bioglass and glass-ceramic
  • Sol-gel bioglass and glass-ceramics
  • Thin film deposition of bioglass and bioglass ceramics

One of the main differences between sol-gel and melt-derived glasses lies in the surface. 104] studied the role of the pressure in pulsed laser deposition (PLD) of SiO2-Na2O- CaO-P2O5 bioactive glass films.

Biomaterials and magnetism

  • Role of magnetism in biomaterials
  • Hyperthermia treatment for cancer
  • Bioactive magnetic glass-ceramics for hyperthermia application

As the magnetic field is reversed, the curve moves to point 'c', the induced magnetization decreases and finally becomes zero at a value of the magnetic field strength called the coercivity or coercivity (Hc). 126] ​​investigated the effect of melting temperature (between C) on magnetic properties in SiO2-Na2O-CaO-P2O5-FeO-Fe2O3 ferrimagnetic glass ceramic samples.

Motivation and preview of the thesis work

The VHN of glass-ceramic samples increases as a function of iron oxide content, as shown in the figure. The dependence of Tg on the composition showed a decrease in the depolarization of the glass skeleton with increasing iron oxide content.

Experimental techniques 43

X-ray diffraction

A standard polycrystalline silicon (Si) sample, supplied with the instrument, was used for the calibration of the instrument. The average crystallite size (d) of the fine crystallites present in the sample was estimated from the peak broadening using the Scherrer's formula [139].

Differential Scanning Calorimetry

Some of the endothermic transitions are the glass transition, reduction, dehydration and some decomposition reactions. The Tg values ​​reported in the current studies correspond to the onset of the glass transition (Fig. 2.2.2).

Density

Microhardness

From equation (2.9) it is clear that VHN decreases when the elastic modulus of the glass decreases. As the number of non-bridging oxygen in a glass increases, the elastic modulus of the glass decreases [145]. Low field measurements (± 500 Oe) were used to evaluate the power loss (or heat generation capability) of the sample at fields amenable to clinical conditions.

Temperature dependence of the mutual magnetic susceptibility of paramagnetic materials (glass samples) shows a Curie-Weiss type behavior that can be expressed as [148], . This equation implies that the splitting of the energy levels is directly proportional to the strength of the magnetic field, as shown in the diagram Fig.

Bioactivity test

  • Preparation of SBF and in vitro test
  • Analysis of samples treated in SBF
    • Glancing incidence X-ray Diffraction
    • Scanning Electron Microscopy
    • Fourier transforms infrared spectroscopy

The GI-XRD patterns of the glass sample with x = 8 mol % Fe2O3 are shown in the figure. The composition dependence of the EPR parameters of the glass-ceramic is shown in Fig. Intensities of the (002) and (211) reflections rise monotonically with an increase in the accumulation of Ca2+ and PO43-.

Fig.4.2.7.1 (b)] with an increase in the concentration of Ca2+ and PO43- ions on the surface of the glass immersed in SBF for several days. XRD patterns of the glass-ceramic samples with different iron oxide contents are shown in Figs.

Preparation of glasses and glass-ceramics

The melt was then poured onto a copper plate at room temperature and pressed with a copper plate to form glass samples of a few millimeters thickness. Identical preparation conditions such as furnace temperature and quenching procedure were followed while preparing the entire series of glasses. The glass plates obtained by the method described above were placed on alumina boats and heat treated at 1050 °C for 3 hours and slowly cooled to room temperature to form glass ceramic samples.

The heat treatment temperature was chosen to ensure the complete crystallization of the two phases observed in thermograms of the glass samples (which will be discussed in section 3.2.2 of this chapter).

Characterization of the glasses

  • XRD studies
  • DSC studies
  • Density
  • Microhardness
  • EPR studies
  • Magnetic susceptibility
  • In vitro bioactivity test of glass samples
    • GI-XRD studies of the glass samples soaked in SBF
    • FT-IR spectroscopy of the glass samples soaked in SBF…
    • SEM-EDS studies of the glass samples soaked in SBF

A decrease in the number of non-bridging oxygens in these glasses with the addition of Fe2O3 results in depolarization of the glass skeleton. The density of the glass increases and the molar volume decreases as the iron oxide mole % content increases. Upon immersion in SBF for a day or more, crystalline peaks appear in the GI-XRD patterns, indicating the formation of a crystalline layer on the surface of the glass.

The formation of a hydroxyapatite layer on the glass surface indicates that the glass samples are bioactive. The formation of a HA layer on the glass surface indicates that the glass samples are bioactive.

Characterization of glass-ceramics samples

  • XRD studies of glass-ceramics samples
  • Microhardness studies of glass-ceramics samples
  • EPR studies of glass-ceramics samples
  • Magnetic properties of glass-ceramics samples
  • In vitro bioactivity test of glass-ceramics samples
    • GI-XRD studies of the glass-ceramics samples soaked

Microhardness of the above-mentioned glass-ceramics was measured according to the procedure detailed in the second chapter. An increase in the VHN can then be interpreted as a result of the increase in the percentage of the crystalline phases in the glass ceramic as a function of iron oxide content. From the nature of the curves it can be deduced that the samples with x = 2 and 4 mol % Fe2O3.

Surface structural changes of glass-ceramic samples treated in SBF were analyzed by X-ray powder diffraction (GI-XRD), Fourier transform infrared reflectance spectroscopy (FT-IR) and scanning electron microscopy (SEM). . The formation of the hydroxyapatite layer on the glass-ceramic surface indicates that the glass-ceramic samples are bioactive.

Summary

The increase in the intensity of the absorption at g ≈ 2.1 as a function of the iron oxide concentration supports this conclusion. TN increase with increase in iron oxide concentration may be correlated with the corresponding increase in the intensity of the g ≈ 2.1 resonance line [Fig. Formation of the HA layer over the glass-ceramic surface shows that the glass-ceramic samples are bioactive.

The density of the glass increases and the molar volume decreases with increasing mole % content of zinc-iron oxide. The increase in the intensity of the g ≈ 2.1 resonance line as a function of zinc-iron oxide concentration lends support to this conclusion.

Preparation of bioactive glasses and glass-ceramics

The melts were then poured into a copper plate and pressed into a 2-3 mm thick plate at room temperature to form glass samples. The glass plates obtained by the method described above were placed on aluminum plates and heat treated at 1050°C for 3 hours and slowly cooled to room temperature to obtain glass-ceramic samples.

Characterization of bioactive glasses

  • XRD studies
  • DSC studies
  • Density and molar volume
  • Microhardness
  • EPR studies
  • Magnetic susceptibility
  • In vitro bioactivity test of glass samples
    • GI-XRD studies of the glass samples soaked in SBF
    • FT-IR spectroscopy of the glass samples soaked in SBF
    • SEM-EDS studies of the glass samples soaked in SBF

The decrease in the molar volume of the samples can be attributed to the increase in the probability of formation of FeO4 group in glass, which. As the number of non-bridging oxygen in a glass decreases, the elastic modulus of the glass increases [145]. Composition dependence of the Curie constant (CM) is shown on the right lateral axis in Fig.

The composition dependence of the Curie constant (CM) and the effective magnetic moment (µexp) is given in Table 4.2.6. With further increase of the immersion time, the intensity of the bands related to the CO32 group increases.

Characterization of glass-ceramics samples

  • XRD studies of glass-ceramics samples
  • Microhardness studies of glass-ceramics samples
  • EPR studies of glass-ceramics samples…
  • Magnetic properties of glass-ceramics samples
  • In vitro bioactivity test of glass-ceramics samples
    • GI-XRD studies of the glass-ceramics samples
    • FT-IR studies of the glass-ceramics samples soaked in SBF…
    • SEM-EDS studies of the glass-ceramics samples

Hydroxyapatite and wollastonite are bone minerals and their presence indicates the biocompatible nature of glass-ceramics. The average crystallite size (d) of the magnetite phase increased in the samples as the iron oxide concentration increased from 5 to 20 wt. Surface structural changes of glass-ceramic samples treated in SBF were analyzed by GI-XRD, FT-IR spectroscopy and SEM.

The intensity of (002) and (211) reflections of the HA phase increases with an increase in the accumulation of Ca2+ and PO43 ions on the surface of the glass ceramic soaked in SBF. 4.3.5.1(d) shows the GI-XRD patterns obtained from the surfaces of the glass ceramics after soaking in SBF for 30 days.

Preparation of glasses and glass-ceramics

A systematic study of ZnO-Fe2O3-SiO2-CaO-P2O5-Na2O glasses by changing the zinc-iron oxide content and the glass ceramics obtained from them is presented in this chapter. Physical properties and in vitro bioactivity assay were performed on these glasses and glass ceramic samples. We expect this to be an improvement over the other two glass-ceramic systems studied in this thesis.

The melts were poured between thick copper blocks that were kept at room temperature and pressed into a 2-3 mm thick plate to form the glass samples. The glass plates obtained by the method described above were placed on alumina plates and heat treated at 800 °C for 1 h and slowly cooled to room temperature to form glass ceramic patterns.

Characterization of the glasses

  • XRD studies
  • DSC studies
  • Density
  • Microhardness
  • EPR studies
  • Magnetic susceptibility
  • In vitro bioactivity test of glass samples
    • GI-XRD studies of the glass samples soaked in SBF
    • FT-IR spectroscopy of the glass samples soaked in SBF
    • SEM-EDS studies of the glass samples soaked in SBF

The Tg of these glasses decreased as the zinc-iron oxide content increased (Table 5.2.2). The glass transition temperature (Tg) of these glasses decreases with an increase in the zinc iron oxide content. The overall intensity of the absorption line Jg ≈ 2.1 shows an increasing trend as the zinc-iron oxide content increases, as depicted in Fig.

It can be observed that the decrease in signal intensity at g ≈ 4.3 is accompanied by the appearance of a broad signal centered at g ≈ 2.1. The absolute magnitude of the θp values ​​increases with the increase of zinc-iron oxide content in the glasses (Fig. 5.2.6.2).

Characterization of glass-ceramics samples

  • XRD studies of glass-ceramics samples
  • Microhardness studies of glass-ceramics samples
  • EPR studies of glass-ceramics samples
  • Magnetic properties of glass-ceramics samples
  • In vitro bioactivity test of glass-ceramics samples
    • GI-XRD studies of the glass-ceramics samples
    • FT-IR studies of the glass-ceramics samples soaked in SBF…
    • SEM-EDS studies of the glass-ceramics samples

Summary

Conclusion and scope for future work 220

Conclusion

Referensi

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