![19
EDS spectrum of the
mineral crust .]
Most of
these peaks are X-rays
given off as electrons return
to the K electron
shell.(K-alpha and K-beta
lines) One peak is from the
L shell of iron.](https://image.slidesharecdn.com/2019ump6086composite-211204084816/85/Thermal-analysis-and-characterization-of-composite-materials-19-320.jpg)
![30
XRD Benefits and Applications
XRD is a non-destructive technique used to [2]:
Identify crystalline phases and orientation
Determine structural properties:
- Lattice parameters
- Strain
- Grain size
- Epitaxy
- Phase composition
- Preferred orientation
Measure thickness of thin films and multi-layers
Determine atomic arrangement](https://image.slidesharecdn.com/2019ump6086composite-211204084816/85/Thermal-analysis-and-characterization-of-composite-materials-30-320.jpg)
Thermal analysis and characterization of composite materials
- 1. Thermal Analysis and Characterisation of Composite Materials
- 2. Students Rohit (2019UMP6070) Abhishek Agrawal (2019UMP6073) Sudhish Bhambani (2019UMP6074) Abhishek Sharma (2019UMP6085) Aniket Burman (2019UMP6086) Sanjeev Gupta (2019UMP6089) 2
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- 4. 4 ● Measurement of the glass transition temperature of polymers ● Varying the composition of monomers ● Effectively evaluate the miscibility of polymers ● To characterize the glass transition temperature of a material APPLICATIONS OF D.M.A. Dynamic Mechanical Analyser
- 5. 5 Working of DMA ● Preparation of Specimen ● Installation of the selected specimen holder ● Installation of the prepared specimen into the specimen holder inside thermal chamber ● Start temperature, finish temperature, and step ● Application of dynamic excitation (stress or strain) on the specimen by dynamic shaker through entire temperature range ● Then DMA records the response of specimen ● Identify transition temperatures based on noticeable changes in curves
- 6. 6 Materials analyzed by DMA ● Polymers ● Elastomers ● Composites ● Metals and alloys ● Ceramics, glass ● Metals and alloys ● Paint and varnish ● Cosmetics ● Biomaterials ● Leather, skin hair ● Oils
- 7. 7 TGA measures the amount and rate (velocity) of change in the mass of a sample as a function of temperature or time in a controlled atmosphere. The measurements are used primarily to determine the thermal and/or oxidative stabilities of materials as well as their compositional properties. The technique can analyze materials that exhibit either mass loss or gain due to decomposition, oxidation or loss of volatiles (such as moisture). It is especially useful for the study of polymeric materials, including thermoplastics, thermosets, elastomers, composites, films, fibers, coatings and paints. Thermogravimetric Analysis (TGA)
- 8. 8 Types of TGA There are three types of thermogravimetry: 1. Isothermal or static thermogravimetry: In this technique, the sample weight is recorded as a function of time at constant temperature. 2. Quasi Static thermogravimetry: In this technique, the sample temperature is raised in sequential steps separated by isothermal intervals, during which the sample mass reaches stability before the start of the next temperature ramp. 3. Dynamic thermogravimetry: In this technique the sample is heated in an environment whose temperature is changed in a linear manner.
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- 10. 10 Two types of transition occurs 1. Physical transition 2. Chemical transition 1. Physical transition ● Adsorption ● Desorption ● Sublimation ● Evapouration ● Vapourization 2. Chemical transition ● Oxidation ● Reduction ● Chemisorption ● Loss on drying ● Degradation
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- 12. 12 Instrumentation: It consists of: ● The balance ● Sample holders ● Furnace ● Recorder ● Thermobalance The measured mass loss curve provides information on: ❖ Changes in sample composition ❖ Thermal stability ❖ Kinetic parameters for chemical reaction in the sample
- 13. 13 INTRODUCTION Scanning electron microscope ● Principle ● Features ● Construction ● Application ● Advantages ● Disadvantages
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- 16. 16 Applications MATERIALS SCIENCE NANOWIRES FOR GAS SENSING SEMICONDUCTOR INSPECTION FORENSIC INVESTIGATIONS Criminal and other forensic investigations utilise SEMs to uncover evidence and gain further forensic insight. BIOLOGICAL SCIENCES In biological sciences, SEMs can be used on anything from insects and animal tissue to bacteria and viruses SOIL SAMPLING & MEDICAL SCIENCE
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- 18. 18 Energy Despersive and X-ray Analysis (EDX) Energy Dispersive X-Ray Analysis (EDX), referred to as EDS or EDAX, is an x-ray technique used to identify the elemental composition of materials. Applications include materials and product research, troubleshooting, deformulation, and more. EDX systems are attachments to Electron Microscopy instruments (Scanning Electron Microscopy (SEM) or Transmission Electron Microscopy (TEM)) instruments where the imaging capability of the microscope identifies the specimen of interest. The data generated by EDX analysis consist of spectra showing peaks corresponding to the elements making up the true composition of the sample being analysed. Elemental mapping of a sample and image analysis are also possible.
- 19. 19 EDS spectrum of the mineral crust .] Most of these peaks are X-rays given off as electrons return to the K electron shell.(K-alpha and K-beta lines) One peak is from the L shell of iron.
- 20. 20 In a multi-technique approach EDX becomes very powerful, particularly in contamination analysis and industrial forensic science investigations. The technique can be qualitative, semi-quantitative, quantitative and also provide spatial distribution of elements through mapping. The EDX technique is non-destructive and specimens of interest can be examined with little or no sample preparation. ● Product deformulation and competitor analysis ● Adhesion, bonding, delamination investigations ● Optical appearance, haze and colour problems ● Disputed claim investigations and expert witness ● Failure investigations, identification of cause ● Catalyst quality, poisoning and elemental distribution ● Product imperfections and defect analysis EDX analysis applications:
- 21. 21 Benefits from EDX analysis: ● Improved quality control and process optimisation ● Rapid identification of contaminant and source ● Full control of environmental factors, emissions etc ● Greater on-site confidence, higher production yield ● Identifying the source of the problem in process chain
- 22. 22 Atomic force microscopy (AFM) or scanning force microscopy (SFM) is a very-high-resolution type of scanning probe microscopy (SPM), which works by scanning a probe over the sample surface, building up a map of the height or topography of the surface as it goes along ATOMIC FORCE MICROSCOPY
- 23. 23 Construction 1. Microscope stage: Moving AFM tip, Sample holder (platform), Vibration. Force Sensor 2. Control electronics: Optical Microscope, controller 3. Computer: The control electronics usually takes the form of a large box interfaced to both the microscope stage and the computer.
- 24. 24 Working 1. The AFM consists of a cantilever with a sharp tip (probe) at its end that is used to scan the specimen surface. 2. When the tip is brought into proximity of a sample surface, forces between the tip and the sample lead to a deflection of the cantilever according to Hooke's law. 3. The sample on the platform has to be moved along all 3-axes (x, y, z - axis) and thus the platform has to be moved, for this Cantilever has to be deflected. 4. This deflection is done by the application of piezoelectric elements, which enables the electric potential to mechanical motion
- 25. 25 Modes of Operation 1. Contact mode strong (repulsive) constant force or constant height. Tip always touching the sample 2. Non-Contact Mode Weak (attractive) vibrating probe 3. Tapping Mode Strong (repulsive) vibrating probe
- 26. 26 Advantages of AFM ● 3D IMAGES ● HIGH RESOLUTION ● NO VACCUM ● NO ILLUMINATION ● CONDUCTIVITY OF SAMPLE Disadvantages of AFM ● SCAN TIME ● SAMPLE DISTORTION
- 27. 27 Applications The AFM has been applied to problems in a wide range of disciplines of the Natural sciences, including 1. solid-state physics 2. molecular engineering 3. cell biology 4. semiconductor science and technology 5. polymer chemistry 6. surface chemistry 7. molecular biology 8. medicine
- 28. 28 X-ray diffraction analysis (XRD) X-ray diffraction analysis (XRD) is a technique used in materials science to determine the crystallographic structure of a material. XRD works by irradiating a material with incident X-rays and then measuring the intensities and scattering angles of the X-rays that leave the material A primary use of XRD analysis is the identification of materials based on their diffraction pattern. As well as phase identification, XRD also yields information on how the actual structure deviates from the ideal one, owing to internal stresses and defects
- 29. 29 How Does it Work? Crystals are regular arrays of atoms, whilst X-rays can be considered as waves of electromagnetic radiation. Crystal atoms scatter incident X-rays, primarily through interaction with the atoms’ electrons. This phenomenon is known as elastic scattering; the electron is known as the scatterer. A regular array of scatterers produces a regular array of spherical waves. In the majority of directions, these waves cancel each other out through destructive interference, however, they add constructively in a few specific directions, as determined by Bragg’s law
- 30. 30 XRD Benefits and Applications XRD is a non-destructive technique used to [2]: Identify crystalline phases and orientation Determine structural properties: - Lattice parameters - Strain - Grain size - Epitaxy - Phase composition - Preferred orientation Measure thickness of thin films and multi-layers Determine atomic arrangement