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Published by khk, 2023-01-27 04:41:56

QFZ3073 S202223-I

Assignment 2

To study subatomic particles in high-energy particle physics research, to probe matter and analyze many physical, chemical, geological, and biological processes. laboratory xrd CONSTRUCTION X-rays are generated in a cathode ray tube by heating a filament to produce electrons. When electrons have sufficient energy to dislodge inner shell electrons of the target material, x-ray spectra is produced. As the sample and detector are rotated, the intensity of the reflected -rays is recorded. Identify unknown crystalline materials, characterization of crystalline materials, determination of unit cell dimension, and measurement of sample purity. synchrotronxrd OPERATION FUNCTION Electron gun generates electrons. They are ejected to the booster synchrotron, where they get accelerated and start to move in circles in the storage ring. The bending magnets in the storage ring are used to steer the electrons around the ring. As the electrons go through each magnet, it loses energy in the form of light. This light can be then channelled out of the storage ring wall and into the experimental stations called beamlines. REFERENCES He, B., Bob, B., Preckwinkel, U., Smith, K.L. (2000). Fundamentals of two dimensions -ray diffraction. Advances in -ray analysis, 43(8). https://serc.carleton.edu/research_education/geochemsheets/techniques/XRD.html https://collegedunia.com/exams/synchrotron-structure-working-principle-applicationphysics-articleid-4383 AHMAD ZAMIR BIN ZAMRI S63596


SOLID STATE SCIENCE (QFZ3073) CHE IZZAH NADHIRAH BINTI CHE SHABUDDIN (S61566) Components : Source of x-rays, sample stage, detector Components : Electron source, booster ring, storage ring, radio-frequency supply and beamlines L A B O R A T O R Y X R D S Y N C H R O T R O N X R D Function Phase identification of a crystalline material and can provide information on unit cell dimensions. Analyze finely ground, homogenized and average bulk composition flow operation of these XRD Function Enhance micro X-ray fluorescence and micro X-ray absorption fine structure measurements by providing direct structural information on the identify of minerals, their crystallinity, and potential impurities in crystal structures REFERENCES : 1. Wenqian Xu. (2019). Synchrotron x-ray diffraction. Retrieved January 19, 2023, from https://doi.org/handbooks/book/100/chapter-abstract/2122371/Synchrotron-X-Ray-Diffraction-Applications?redirectedFrom=fulltext . 2.Synchrotron X-ray Diffraction (XRD). (2019, November 16). NIST. https://www.nist.gov/laboratories/tools-instruments/synchrotron-x-ray-diffraction-xrd 3.XRD Laboratory. (n.d.). Retrieved January 20, 2023, from https://www.royalholloway.ac.uk/research-and-teaching/departments-and-schools/earth-sciences/research/research-laboratories/x-ray-diffraction-laboratory/


laboratory XRD vs Synchroton XRD M A D E B Y J E S L I N A M O H D S A B R I L E E - S 6 3 6 4 7 C O N S T R U C T I O N O P E R A T I O N F U N C T I O N P R O V I D E T H E I N I T I A L C H A R A C T E R I Z A T I O N O F M A T E R I A L P R O P E R T I E S A N D T Y P I C A L L Y U S E S A P E N E T R A T I V E L Y I N S U F F I C I E N T C O P P E R X - R A Y S O U R C E . P R O V I D E I N F O R M A T I O N O N C R Y S T A L L I N E M A T E R I A L S WI T H G R E A T E R D I F F R A C T I O N P E A K S E N S I T I V I T Y B Y U S I N G P O L Y C H R O M A T I C R A D I A T I O N A S T H E S O U R C E & I S (Both work on the principle of Bragg's law) U S U A L L Y O P E R A T E D A T A F I X E D A N G L E . T H R E E B A S I C E L E M E N T S : A N X - R A Y T U B E , A S A M P L E H O L D E R , A N D A N X - R A Y D E T E C T O R . A T Y P I C A L S Y N C H R O T R O N R A D I A T I O N S O U R C E C O N S I S T S O F : L I N E A R A C C E L E R A T O R , C I R C U L A R S T O R A G E R I N G , & B E A M L I N E I N A C A T H O D E R A Y T U B E , X - R A Y S A R E P R O D U C E D B Y H E A T I N G A F I L A M E N T , WH I C H A C C E L E R A T E S E L E C T R O N S T OWA R D A T A R G E T . T H E I N T E N S I T Y O F T H E R E F L E C T E D X - R A Y S I S M E A S U R E D WH I L E T H E S A M P L E A N D D E T E C T O R S P I N . D U E T O T H E R A D I A L A T T R A C T I O N T H A T D R AWS E L E C T R O N S T O T H E C E N T R E O R R I N G O F T H E S T O R A G E R I N G , M A G N E T I C F I E L D S I N T H E R I N G C A U S E E L E C T R O N S T O D E P A R T .


REFERENCES A L D E R T O N , D . ( 2 0 2 1 ) . X - R A Y D I F F R A C T I O N ( X R D ) . E N C Y C L O P E D I A O F G E O L O G Y , 5 2 0 – 5 3 1 . H T T P S : / / D O I . O R G / 1 0 . 1 0 1 6 / B 9 7 8 - 0 - 0 8 - 1 0 2 9 0 8 - 4 . 0 0 1 7 8 - 8 L L EWE L L Y N , A . V . , M A T R U G L I O , A . , B R E T T , D . J . L . , J E R V I S , R . , & S H E A R I N G , P . R . ( 2 0 2 0 , N O V E M B E R 1 6 ) . U S I N G I N - S I T U L A B O R A T O R Y A N D S Y N C H R O T R O N - B A S E D X - R A Y D I F F R A C T I O N F O R L I T H I U M - I O N B A T T E R I E S C H A R A C T E R I Z A T I O N : A R E V I EW O N R E C E N T D E V E L O P M E N T S . M D P I . R E T R I E V E D J A N U A R Y 2 3 , 2 0 2 3 , F R O M H T T P S : / /WWW. M D P I . C O M / 2 4 1 0 - 3 8 9 6 / 5 / 4 / 7 5 # S E C 3 - C O N D E N S E D M A T T E R - 0 5 - 0 0 0 7 5 P A L S I N G H , J . , K U M A R P A I D I , A . , HWA C H A E , K . , S A N G S U L L E E , & D O C H E O N A H N . ( 2 0 2 2 , J U L Y 1 3 ) . S Y N C H R O T R O N R A D I A T I O N B A S E D X - R A Y T E C H N I Q U E S F O R A N A L Y S I S O F C A T H O D E S I N L I R E C H A R G E A B L E B A T T E R I E S . R S C A D V A N C E S . R E T R I E V E D J A N U A R Y 2 3 , 2 0 2 3 , F R O M H T T P S : / / P U B S . R S C . O R G / E N / C O N T E N T / A R T I C L E H T M L / 2 0 2 2 / R A / D 2 R A 0 1 2 5 0 B S H A R M A , A . , & H E S T E R B E R G , D . ( 2 0 2 0 ) . S Y N C H R O T R O N R A D I A T I O N - B A S E D S P A T I A L M E T H O D S I N E N V I R O N M E N T A L B I O G E O C H E M I S T R Y . M U L T I D I M E N S I O N A L A N A L Y T I C A L T E C H N I Q U E S I N E N V I R O N M E N T A L R E S E A R C H , 2 3 1 – 2 6 5 . H T T P S : / / D O I . O R G / 1 0 . 1 0 1 6 / B 9 7 8 - 0 - 1 2 - 8 1 8 8 9 6 - 5 . 0 0 0 0 9 - 0 X - R A Y P OWD E R D I F F R A C T I O N ( X R D ) . T E C H N I Q U E S . ( 2 0 2 3 , J A N U A R Y 2 0 ) . R E T R I E V E D J A N U A R Y 2 3 , 2 0 2 3 , F R O M H T T P S : / / S E R C . C A R L E T O N . E D U / R E S E A R C H _ E D U C A T I O N / G E O C H E M S H E E T S / T E C H N I Q U E S / X R D . H T M L


OPERATION CONSTRUCTION FUNCTIONS REFERENCES LABORATORY XRD vs SYNCHOTRON XRD Identify crystalline phases and orientation Determine structural properties: Measure thickness of thin films and multi-layers Determine atomic arrangement - Lattice parameters - Strain - Grain size - Epitaxy - Phase composition - Preferred orientation providing information on regularly occurring and well defined structures such as crystal lattices or interfaces in multilayer materials. The small, intense beam at BMM is key to probing small areas of a larger sample with macroscopic heterogeneity such as a patterned substrate or device. The brilliance of the source facilitates examination of structural changes due to small concentrations of elements in doping applications that would be prohibitive to measure on a labbased source. Additionally, the use of the tunable energy of the beam provides a route to alter the contrast of elements as the energy approaches the excitation energy of elemental core electrons. The "anomalous" diffraction that results is key to separating the contributions of different elements in many complex materials used across the manufacturing spectrum. Synchrotron X-ray diffraction (SXRD) is another complementary technique that provides more definitive information about crystalline soil minerals. 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: 2dsinθ = nλ Where d is the spacing between diffracting planes, θ is the incident angle, n is an integer, and λ is the beam wavelength. The specific directions appear as spots on the diffraction pattern called reflections. Consequently, X-ray diffraction patterns result from electromagnetic waves impinging on a regular array of scatterers. X-rays are used to produce the diffraction pattern because their wavelength, λ, is often the same order of magnitude as the spacing, d, between the crystal planes (1-100 angstroms) The X-ray diffraction (XRD) end station measures constructive interference of the x-ray wave with repeating atomic and interfacial structure in materials. At the Beamline for Material Measurement, XRD features a tunable, monochromatic, high intensity beam with a beam spot on the order of 100 micrometers. The high energy beam (4.5 keV to 23 keV) is combined with a six-circle Ψ goniometer for measurement of thin films as well as single and polycrystalline materials. KAS NALISHA BINTI KHALIB - S62656 Satpute, N. S., & Dhoble, S. (2021). Role of rare-earth ions for energy-saving LED lighting devices. Energy Materials, 407– 444. https://doi.org/10.1016/b978-0-12- 823710-6.00018-2 Nasrazadani, S., & Hassani, S. (2016). Modern analytical techniques in failure analysis of aerospace, chemical, and oil and gas industries. Handbook of Materials Failure Analysis With Case Studies From the Oil and Gas Industry, 39–54. https://doi.org/10.1016/b978-0-08- 100117-2.00010-8 Sharma, A., & Hesterberg, D. (2020). Synchrotron radiation-based spatial methods in environmental biogeochemistry. Multidimensional Analytical Techniques in Environmental Research, 231–265. https://doi.org/10.1016/b978-0-12-818896-5.00009-0


LABORATORY XRD VS SYNCHROTRON XRD MASURI A/P MOHAMED YASIN s62576 TS. DR. KHADIJAH HILMUN KAMARUDIN LABORATORY XRD SYNCHROTRON XRD laboratory XRD is extremely useful for stress measurements as well as for texture analysis. Samples to be analyzed using XRD must be crystalline however the technique can provide the degree of crystallinity in polymer Synchrotron X-ray diffraction (SXRD) is another complementary technique that provides more definitive information about crystalline soil minerals. Similar to conventional laboratory XRD (LXRD), SXRD works on the principle of Bragg's law. what is laboratory xrd: what is synchrotron xrd: how they work: how they work: Synchrotron radiation of an electron beam circulating at high energy in a magnetic field leads to radiative self-polarization of electrons in the beam (Sokolov–Ternov effect). This effect is used for producing highly polarised electron beams for use in various experiments. application of laboratory xrd: application of synchroton xrd: Measure the average spacings between layers of rows of atoms in a substance Determine the orientation of an individual grain or crystal Measure the size, shape and internal stress of small crystalline areas Identify the crystal structure of an unknown substance. references list: Synchrotron X-ray diffraction (XRD) (2019) NIST. Available at: https://www.nist.gov/laboratories/tools-instruments/synchrotron-x-raydiffraction-xrd (Accessed: January 25, 2023). X-ray diffraction (no date) X-Ray Diffraction - an overview | ScienceDirect Topics. Available at: https://www.sciencedirect.com/topics/engineering/x-ray-diffraction (Accessed: January 25, 2023).


Synchrotron X-rays are also used for direct visualization of nanoscale structures at high resolution through X-ray microscopy. The synchrotrons also enabled understanding the ion exchange process which was previously not possible due to insufficient time resolution. Studies of dynamic processes and structural changes in materials, such as phase transitions or chemical reactions, in real-time and at high temporal and spatial resolutions. Provides more definitive information of crystalline structure. Analysis of the microstructure of materials, including the measurement of size, shape, and strain of crystalline domains, and the characterization of defects and impurities. CONSTRUCTION Ren, Y. (2012). High-Energy Synchrotron X-Ray Diffraction and Its Application to In Situ Structural Phase-Transition Studies in Complex Sample Environments. JOM, 64(1), 140–149. https: / /doi.org/10.1007/s11837-011-0218-8 Fatimah, S., Ragadhita, R., Husaeni, D. F. A., & Nandi yanto, A. B. D. (2021). How to Calculate Cr ystallite Size from X-Ray Diffraction (XRD) using Scherrer Method. ASEAN Journal of Science and Engineering, 2(1), 65–76. https: / /doi.org/10.17509/ajse.v2i1.37647 Synchrotron radiation. Synchrotron Radiation - an overview | ScienceDirect Topics. (n.d.). Retrieved Januar y 23, 2023, from https: / /www.sciencedirect.com/ topics/neuroscience/synchrotron-radiation Synchrotron X-rays shine light on energy science | Energy Frontier Research Centers Communit y Website. (n.d.). https: / /www.energy frontier.us/content /synchrotron-x-rays-shine-light-energy -science Synchrotron X-ray Diffraction (XRD). (2019, November 16). NIST. https: / /www.nist.gov/ laboratories/ tools-instruments/synchrotron-x-ray -diffraction-xrd LABORATORY XRD VS SYNCHROTRON XRD FUNCTION REFERENCE LIST MOHAMAD FIRDAUS BIN ROSLI S63788 CONSTRUCTION FUNCTION OPERATION OPERATION Electrons emitted by an electron gun are first accelerated in a linear accelerator (linac) and then transmitted to a circular accelerator (booster synchrotron) where they are accelerated to reach a high energy level. they circulate in a vacuum environment, at a constant energy, for many hours. It works on the principle that energy is emitted when a moving electron changes its direction. The high energy beam (4.5 keV to 23 keV) is combined with a six-circle Ψ goniometer for measurement of thin films as well as single and polycrystalline materials. The Xrays are directed at a sample, and the diffraction pattern created by the interaction of the X-rays with the sample is analyzed to determine the arrangement of atoms in the sample. Determining the crystal structure of a material, including atom arrangement and crystal symmetry. Using diffraction patterns to identify unknown chemicals or minerals. The size, shape, and strain of crystalline domains inside a material are measured. Identifying a sample's purity and crystalline phase. Characterization of polycrystalline materials' crystalline microstructure. Determining crystallite size, which is linked to sample particle size. Obtaining crystal lattice parameters. The sample is bombarded with X-rays, and the resulting diffraction pattern is analyzed to determine the crystal structure. This process involves shining an X-ray beam onto a sample, and measuring the resulting diffraction pattern. The diffraction pattern is then analyzed using Debye Scherrer's equationto determine the crystal structure of the sample. QFZ 3073 SEM 1 2022/2023


Construction conducted in both diamond and multi-anvil cells for penetration with high pressure refer as "white light" due produce variety of energy rays the angle between incident beam and the sample are variable for final result Operation Function Laboratory XRD vs Synchrotron XRD 1 Laboratory XRD 2 Synchrotron XRD conducted in diamond anvil cells for penetration with low intensity and high resolution has monochromatic beam to focus one energy ray the angle between incident beam and the sample are fixed for final result References: 1.David Alderton, X-Ray Diffraction (XRD),Encyclopedia of Geology (Second Edition),Academic Press,2021,Pages 520-531,SBN 9780081029091,https://doi.org/10.1016/B978-0-08-102908-4.00178-8. (https://www.sciencedirect.com/science/article/pii/B9780081029084001788) 2.Burnley. (2022). Synchrotron X-Ray Diffraction. Mineral Physics. Retrieved January 23, 2023, from https://serc.carleton.edu/NAGTWorkshops/mineralogy/mineral_physics/synchrotron_xrd.html 3.Dutrow. (2023). X-ray Powder Diffraction (XRD). Techniques. Retrieved January 23, 2023, from https://serc.carleton.edu/research_education/geochemsheets/techniques/XRD.html 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 same operation as laboratory XRD but emitted electrons are accelerated to give more intense result and can analyzed smaller area of crystallize structure to find the geometry or shape of a molecule has a long range order with x-rays. to measure thickness of thin films and multi-layers to determine structural properties(Phase composition, Lattice parameters, Grain size etc.) to provides more definitive information about crystalline soil minerals to give better sensitivity and resolution of diffraction peaks to measure smaller and more dilute phases, and to get determination of very fine structures Muhammad Danial Arif Bin Mohd Zaini (S63349)


OPERATION LABORATORY XRD VS SYNCHROTRON XRD CONSTRUCTION Consist of an X-ray tubes, a sample holder, a detector and a data acquisition system. An X-ray tubes(Cu-anode), which generates X rays A sample holder, where the sample is placed. A detector, which record the diffraction pattern A computer, which process the data and generates the diffraction pattern. Consist of a synchrotron, a beamline and a detector. A synchrotron source, which generates intense A beamlines, which transport the X-rays from the synchrotron to the experimental station A detector, which records the diffraction pattern A computer, which processes the data and generates the diffraction pattern. Uses a conventional x-ray source, such as a Cu anode X-ray tube. The operator loads the sample onto the sample holder and aligns it with the X-ray beam. Then the diffractometer adjusted to the appropriate angle and X-ray directed to the sample. The diffraction would be detected by detector and being processes by computer. Uses x-rays generated by a synchrotron. The operator load the sample into the sample environment and aligns it with the X-ray beam. The beamlines transport the X-rays from the synchrotron to the experimental station. Then the diffractometer adjusted to the appropriate angle and X-ray directed to the sample. The diffraction would be detected by detector and being processes by computer. FUNCTIONS Used for determining the crystal structure of known materials, the identification of unknown compounds and for the analysis of powders, thin film and single crystals. Measuring the purity and crystalline perfection of materials Measuring the amount of a particular phase in a sample Used for the analysis of small crystal, low dimensional materials, surfaces, interfaces and dynamic processes. Determining the crystal structure of materials at high pressures and temperatures Determining the crystal structure of powder and amorphous materials Determining the crystal structure of samples that are sensitive to radiation damage. REFERENCES: Sharma, A., & Hesterberg, D. (2020). Synchrotron radiation-based spatial methods in environmental biogeochemistry. Multidimensional Analytical Techniques in Environmental Research, 231–265. https://doi.org/10.1016/b978-0-12- 818896-5.00009-0 X-ray Diffraction (XRD) laboratory - Technical facility - Staffordshire University. (n.d.). https://www.staffs.ac.uk/about/facilities/technical/x-ray-diffraction-xrd-laboratory Synchrotron X-ray Diffraction (XRD). (2019, November 16). NIST. https://www.nist.gov/laboratories/tools instruments/synchrotron-x-ray-diffraction-xr


Consist of a synchrotron, a beamline and a detector. A synchrotron source, which generates intense A beamlines, which transport the X-rays from the synchrotron to the experimental station A detector, which records the diffraction pattern A computer, which processes the data and generates the diffraction pattern. Consist of an X-ray tubes, a sample holder, a detector and a data acquisition system. An X-ray tubes(Cu-anode), which generates Xrays A sample holder, where the sample is placed. A detector, which record the diffraction pattern A computer, which process the data and generates the diffraction pattern. Uses a conventional x-ray source, such as a Cu anode X-ray tube. The operator loads the sample onto the sample holder and aligns it with the X-ray beam. Then the diffractometer adjusted to the appropriate angle and X-ray directed to the sample. The diffraction would be detected by detector and being processes by computer. Uses x-rays generated by a synchrotron. The operator load the sample into the sample environment and aligns it with the X-ray beam. The beamlines transport the X-rays from the synchrotron to the experimental station. Then the diffractometer adjusted to the appropriate angle and X-ray directed to the sample. The diffraction would be detected by detector and being processes by computer. Used for determining the crystal structure of known materials, the identification of unknown compounds and for the analysis of powders, thin film and single crystals. Measuring the purity and crystalline perfection of materials Measuring the amount of a particular phase in a sample Used for the analysis of small crystal, low dimensional materials, surfaces, interfaces and dynamic processes. Determining the crystal structure of materials at high pressures and temperatures Determining the crystal structure of powder and amorphous materials Determining the crystal structure of samples that are sensitive to radiation damage. 02 Operation LABORATORY XRD 01 03 04 Construction Functions Muhammad Zulhasnan bin Mohd Zahari S63665 Synchrotron La Xrd boratory Xrd SYNCHROTRON XRD Laboratory Xrd Synchrotron Xrd Laboratory Xrd Synchrotron Xrd References Sharma, A., & Hesterberg, D. (2020). Synchrotron radiation-based spatial methods in environmental biogeochemistry. Multidimensional Analytical Techniques in Environmental Research, 231–265. https://doi.org/10.1016/b978-0-12- 818896-5.00009-0 X-ray Diffraction (XRD) laboratory - Technical facility - Staffordshire University. (n.d.). https://www.staffs.ac.uk/about/facilities/technical/x-ray-diffraction-xrd-laboratory Synchrotron X-ray Diffraction (XRD). (2019, November 16). NIST. https://www.nist.gov/laboratories/toolsinstruments/synchrotron-x-ray-diffraction-xrd


Laboratory XRD constructions Name :Nuha Raihana Husni Binti Asrul Husni Matric No. : S61561 Synchrotron XRD operations functions [1] Gotame, R.C. (2021). XRD Working and Application. Physics Feed. Retrived from https://physicsfeed.com/post/xrd-working-and-application/ [2] FAQ - XRD/XRF. (2022, April 29). James Cook University. Retrieved from https://www.jcu.edu.au/advanced-analytical-centre/resources/faqxrdxrf Identify crystalline phases and orientation Measure thickness of thin films and multi-layers Determine atomic arrangement Determine structural properties such as ohase composition, size, preferred orientation Provides more definitive information about crystalline soil minerals. Commonly used in medical and pharmaceutical research. Tuneable to different wavelengths, they have high intensities and thus sensitivity is increased, the spectral resolution is high, the X-rays can be focussed to very small areas (μXRD), and the analysis can be rapid. [3] Synchrotron X-ray Diffraction (XRD). (2019, November 16). NIST. Retrieved from https://www.nist.gov/laboratories/tools-instruments/synchrotron-x-raydiffraction-xrd [4] What is X-Ray Diffraction Analysis (XRD) and How Does it Work? (n.d.). TWI. Retrieved from https://www.twi-global.com/technical-knowledge/faqs/x-ray-diffraction References Crystal atoms primarily interact with their electrons to scatter incident Xrays. The electron is the scatterer in this event, which is referred to as elastic scattering. A regular array of spherical waves results from a regular array of scatterers. These waves interfere destructively in the vast majority of directions, but according to Bragg's law, they add constructively in the following few directions: 2dsinθ = nλ According to Bragg's law, high-energy x-rays that penetrate a component are diffracted by the crystallographic planes within its material grains. This method uses the material's polycrystalline lattice as an atomic strain gauge. The method depends on precise measurement of the change in atomic lattice plane separation brought on by stress in polycrystalline materials. Synchrotron X-rays have excellent geometric definition and can frequently produce beam diameters of the m level. Since the high energy x-rays are produced inside a synchrotron ring, the technology cannot be transported.


Provide more definitive information on crystalline structure at high pressures & temperatures (inc measurement of size, shape & strain of crystalline domains) & the characterization of defects & impurities. analysis of small crystal, low dimensional materials, surfaces, interfaces & dynamic processes. X-rays are directed at sample, and diffraction pattern is created by the interaction of X-rays with sample. Electrons emitted by electron gun are accelerated in linear accelerator, then transmitted to circular accelerator (to accelerate at extremely high energy and combined with six-circle Ψ goniometer for measurement of thin films as well as single & polycrystalline materials). They circulate in a vacuum environment (at constant energy). CONSTRUCTION FUNCTION OPERATION d - spacing between diffracting planes θ - incident angle n - integer λ - beam wavelength Primary characterization of material properties like crystallite size, strain & crystal structure (inc atom arrangement & crystal symmetry). Identify purity & crystalline phase of sample. Identify unknown solid using diffraction patterns. Obtain crystal lattice parameters. Irradiating a material with incident X-rays, then measuring intensities & scattering angles of X-rays that leave the material. A regular array of scatterers (atom's electrons) produces regular array of spherical waves. Directions of these waves cancel each other out through destructive interference. They add constructively in a few specific directions, according to Bragg’s law: X-ray diffraction patterns result from EM waves impinging on regular array of scatterers. CONSTRUCTION FUNCTION OPERATION 2dsinθ = nλ Synchrotron X-ray diffraction. (n.d.). Retrieved January 25, 2023, from https://www.sciencedirect.com/topics/chemistry/synchrotron-x-ray-diffraction X ray diffraction. (n.d.). Retrieved January 25, 2023, from https://www.sciencedirect.com/topics/nursing-and-health-professions/x-raydiffraction#:~:text=X%2Dray%20diffraction%20(XRD),due%20to%20its%20wide%20application. Admin. (2022, May 31). Synchrotron - principle of operation, definition and example. Retrieved January 25, 2023, from https://byjus.com/physics/synchrotron/ NUR JANNATI BINTI ZAHRIN (S63705) QFZ3073 SOLID STATE SCIENCE LABORATORY XRD VS SYNCHROTRON XRD REFERENCES 1 2 3


Synchrotron XRD operation Function Researchers use synchrotron radiations, which are electromagnetic waves, to study subatomic particles in high-energy particle physics research. Synchrotron radiation is created using electron synchrotrons. Nuclear physics research employs heavy-ion synchrotrons. Many types of measurements are aided by synchrotron light. Synchrotron technology is used in many fields of science, including material engineering, pharmacology, biology, geology, chemistry, physics, nanotechnology, and medicine. Synchrotrons operate on the concept that when a moving electron changes direction, it emits energy. As such, charged particles emit electromagnetic radiation when they are accelerated. So a synchrotron's job is basically to accelerate electrons to extremely high energies and then cause them to change direction on a regular basis. The process begins with the production of electron particles in an electron gun. The particles are then ejected into the booster synchrotron, where they accelerate and begin to move in circles around the storage ring. The electrons are now guided around the storage ring by the bending magnets. Each magnet loses energy in the form of light as electrons pass through it. The experimental stations known as beamlines can then receive this light by channelling it out of the storage ring wall. Laboratory XRD construction Function operation Interference is produced when atoms in crystals interact with X-ray waves. Each plane of atoms in crystal structures will reflect incident Xrays differently because of their presence. Allow two monochromatic X-ray beams (of a specific wavelength) to collide with a crystal structure at an incoming angle of theta. Ray 1 reflects from the top atomic plane, while Ray 2 reflects from the bottom atomic plane. Ray 2 travels 2a farther than Ray 1 because it has to cross deeper into the atomic plane. Rays 1 and 2 will constructively interfere after exit the crystal if their distances 2a and n*lambda, the integral number of the wavelengths of the two waves, are equal. The way that x-rays reveal the atomic structure of crystals is based on Bragg’s law. Determine structural properties: Measure thickness of thin films and multi-layers Determine atomic arrangement Determine the orientation of an individual grain or crystal Measure the size, shape and internal stress of small crystalline areas Identify the crystal structure of an unknown substance. - Lattice parameters - Strain - Grain size X-ray cathode tube - produces X-rays by heating a filament. By adding a voltage, this generates electrons that are subsequently guided in the direction of a target. These assault the target material, displacing the electrons in its inner shell, which causes the substance to emit x-rays. Sample holder - The sample is subsequently exposed to the x-rays. The device's source and x-ray detector both spin. When this geometric movement meets the requirements of Bragg's law for the phenomenon being studied, constructive interference takes place, leading to an intensity peak. X-ray detector - his signal is captured by the detector, which then converts it into a count rate for output to a computer. typical plot of intensity versus theta. h Storage Ring - A storage ring is a polygon tube made of straight sections and angles connected by bending magnets. By providing a magnetic field, it allows electrons to circle at close to the speed of light. The tube is kept at a very low temperature of 10-9 bar. Booster Synchrotron - A 300-meter-long pre-accelerator. Electrons are accelerated here before being injected into the storage ring. Electronic gun - Electrons are created here for injection into the booster synchrotron. Beamlines: The X-ray beams that the electrons emit are directed toward the storage ring by the beamlines. The beamlines were designed so that they could be used for specific types of research. construction Suman, S. (n.d.). Synchrotron: Structure, Working Principle, & Applications. Collegeduania. What is X-Ray Diffraction Analysis (XRD) and How Does it Work? (n.d.). TWI. https://www.twi-global.com/technical-knowledge/faqs/x-ray-diffraction References


Laboratory XRD vs Synchrotron XRD When using XRD, a material is exposed to incoming X-rays, and the intensity and scattering angles of the X-rays that escape the material are then measured. To evaluate the structure and crystallinity of solid materials. Functions Construction Operation What is X-Ray Diffraction Analysis (XRD) and How Does it Work? (n.d.). What Is X-Ray Diffraction Analysis (XRD) and How Does It Work? - TWI. https://www.twiglobal.com/technicalknowledge/faqs/x-ray-diffraction.aspx X Ray Diffraction - an overview | References ScienceDirect Topics. (n.d.). X Ray Diffraction - an Overview | ScienceDirect Topics. https://www.sciencedirect.com/topic s/nursing-and-health-professions/xray-diffraction Gives more precise details on crystalline soil minerals Synchrotron X-Ray Diffraction - an overview | ScienceDirect Topics. (n.d.). Synchrotron X-Ray Diffraction - an Overview | ScienceDirect Topics. https://www.sciencedirect.com/topics/chemistr y/synchrotron-x-raydiffraction#:~:text=Synchrotron%20X%2Dray%2 0diffraction%20(SXRD,the%20principle%20of% 20Bragg’s%20law. Bragg's law is the foundation of SXRD. In XRD analysis, interferences that happen when scattered waves are in phase or out of phase result in bright (high intensity) spots on an aerial detector or peaks in a scanned diffraction pattern. A synchrotron is composed of five main components: electron source, booster ring, storage ring, RF (radiofrequency) supply, and beamlines. Synchrotron X-ray Diffraction (XRD). (2019, February 12). NIST. https://www.nist.gov/laboratories/toolsinstruments/synchrotron-x-ray- diffraction-xrd X-ray diffractometers consist of three basic elements: an X-ray tube, a sample holder, and an Xray detector X-ray Powder Diffraction (XRD). (n.d.). Techniques. https://serc.carleton.edu/research_ed ucation/geochemsheets/techniques/X RD.html X-ray Powder Diffraction (XRD). (n.d.). Techniques. https://serc.carleton.edu/research_education/ geochemsheets/techniques/XRD.html Bharti, A., & Goyal, N. (2019, February 8). Fundamental of Synchrotron Radiations. Fundamental of Synchrotron Radiations | IntechOpen. https://www.intechopen.com/state.ite m.id NURIN AUNI LATHIFA S61568


Function Laboratory XRD QFZ3073 NURLIYANA BINTI MOHD ZAID (S63815) Synchroton XRD Construction Operation REFERENCES high-energy x-ray beams that are a million times more intense and penetrate much deeper. Low 2θ scattering angles are the result of relatively high energy beams, which typically range from 4° to 10°. The “ white ” beam must be monochromated for diffraction. Capable to form 3D maps of the strain distribution in engineered parts with a high spatial resolution and down to millimeter depths. Give more definitive information about crystalline soil minerals Characterize crystal preferred orientation distributions Measuring the lattice mismatch between film and substrate to define stresses and strains Identify the crystal structure of an unknown substance. Measure the size, shape and internal stress of small crystalline areas Analysing rocking curves to determine dislocation density and film quality Generated by a cathode ray tube, filtered to produce monochromatic radiation, collimated to concentrate, and directed toward the sample. Constructive or destructive interferences occurring when scattered waves are in phase or out of phase Steuwer, A., Santisteban, J.R., Turski, M., Withers, P.J., Buslaps, T., “High-resolution strain mapping in bulk samples using full-profile analysis of energy dispersive synchrotron X-ray diffraction data”, Nuclear Instruments and Methods in Physics Research, B 238, 200-204, 2005 Lutterotti, Luca & Vasin, Roman & Wenk, Hans-Rudolf. (2014). Rietveld texture analysis from synchrotron diffraction images. I. Calibration and basic analysis. Powder Diffraction. 29. 76-84. 10.1017/S0885715613001346. Bunaciu, Andrei A. & UdriŞTioiu, Elena & Aboul-Enein, Hassan. (2015). X-Ray Diffraction: Instrumentation and Applications. Critical reviews in analytical chemistry / CRC. 45. 10.1080/10408347.2014.949616. Ling. C. (2007). Synchrotron X-ray Powder Diffraction. The University of Sydney. Retrieved from http://archive.synchrotron.org.au/images/AOF2017/14-Powder-XRD-Basics-Chris-Ling.pdf 1. 2. 3. 4.


Laboratory XRD Synchrotron XRD A technique that provides more definitive information about crystalline soil minerals. References Operation Construction Function QFZ3073 S O L I D S T A T E S C I E N C E NURULLJANNAH BINTI MOHAMAD NOR (S62642) SXRD have a high flux, tunable welldefined wavelength, and better collimation of synchroton radiation, which also improves the identification of minor minerals A rapid analytical technique primarily used for phase identification of a crystalline material and can provide information on unit cell dimensions. David Alderton (2020). X Ray Diffraction (XRD). Retrieved from https://doi.org/10.1016/B978-0-08- 102908-4.00178-8 Llewellyn AV, Matruglio A, Brett DJL, Jervis R, Shearing PR. Using In-Situ Laboratory and SynchrotronBased X-ray Diffraction for Lithium-Ion Batteries Characterization: A Review on Recent Developments. Condensed Matter. 2020; 5(4):75. https://doi.org/10.3390/condmat5040075 NIST (2019) Synchrotron X-ray Diffraction (XRD) Retrieved from https://www.nist.gov/laboratories/tools-instruments/synchrotron-x-ray-diffraction-xrd Singh, B., Markus, G.,Navdeep Kaur, N., Andrea Liese, (2010) Applications of Synchrotron-Based X-Ray Diffraction and X-Ray Absorption Spectroscopy to the Understanding of Poorly Crystalline and MetalSubstituted Iron Oxides (volume 34) https://doi.org/10.1016/S0166-2481(10)34008-6 Synchrotron radiation is emitted by electrons that are accelerated to near light speed in a circular storage ring.


Q F Z 3 0 7 3 S O L I D S T A T E S C I E N C E REN, Y. (2012). HIGH-ENERGY SYNCHROTRON X-RAY DIFFRACTION AND ITS APPLICATION TO IN SITU STRUCTURAL PHASE-TRANSITION STUDIES IN COMPLES SAMPLE ENVIRONMENTS. JOM, 64(1), 140-149. HTTPS://DOI.ORG/10.1007/S11837-011-0218-8 FATIMAH. S. RAGADHITA, R., HUSSENI, D. F. A., & NANDIYANTO, A. B. D. (2021). HOW TO CALCULATE CRYSTALLITE SIZE FROM X-RAY DIFFRACTION (XRD) USING SCHERRER METHOD. ASEAN JOURNAL OF SCIENCE AND ENGINEERING, 2(1), 65-76. HTTPS://DOI.ORG/10.17509/AJSE V2I1.37647 -SYNCHROTRON RADIATION SYNCHROTRON RADIATION- AN OVERVIEW | SCIENCEDIRECT TOPICS (N.D.). RETRIEVED JANUARY 23, 2023, FROM HTTPS://WWW.SCIENCEDIRECT.COM/TOPICS/NEUROSCIENCE/SYNCHROTRONRADIATION SYNCHROTRON X-RAYS SHINE LIGHT ON ENERGY SCIENCE | ENERGY FRONTIER RESEARCH CENTERS COMMUNITY WEBSITE (N.D.). HTTPS://WWW.ENERGYFRONTIER.US/CONTENT/SYNCHROTRON-A-RAYS-SHINE-LIGHT-ENERGYSCIENCE SYNCHROTRON X-RAY DIFFRACTION (XRD) (2019, NOVEMBER 16). NIST HTTPS://WWW.NIST.GOV/LABORATORIES/TOOLS-INSTRUMENTS/SYNCHROTRON-A-RAY DIFFRACTISE-WID CONSTRUCTION LABORATORY XRD SYNCHROTRON XRD FUNCTION OPERATION DETERMINING THE CRYSTAL STRUCTURE OF A MATERIAL, INCLUDING ATOM ARRANGEMENT AND CRYSTAL SYMMETRY. USING DIFFRACTION PATTERNS TO IDENTIFY UNKNOWN CHEMICALS OR MINERALS. THE SIZE, SHAPE, AND STRAIN OF CRYSTALLINE DOMAINS INSIDE A MATERIAL ARE MEASURED. IDENTIFYING A SAMPLE'S PURITY AND CRYSTALLINE PHASE. CHARACTERISATION OF POLYCRYSTALLINE MATERIALS' CRYSTALLINE MICROSTRUCTURE. DETERMINING CRYSTALLITE SIZE, WHICH IS LINKED TO SAMPLE PARTICLE SIZE. OBTAINING CRYSTAL LATTICE PARAMETERS. USED FOR DIRECT VISUALISATION OF NANOSCALE STRUCTURES AT HIGH RESOLUTION THROUGH X-RAY MICROSCOPY. ENABLED UNDERSTANDING THE ION EXCHANGE PROCESS WHICH WAS PREVIOUSLY IMPOSSIBLE DUE TO INSUFFICIENT TIME RESOLUTION. STUDIES OF DYNAMICS PROCESSES AND STRUCTURAL CHANGES IN MATERIALS SUCH AS PHASE TRANSITION OR CHEMICAL REACTIONS, IN REAL TIME AMD AT HIGH TEMPORAL AND SPATIAL RESOLUTIONS. PROVIDES MORE DEFINITIVE INFORMATION OF CRYSTALLINE STRUCTURE. ANALYSIS OF THE MICROSTRUCTURE OF MATERIALS, INCLUDING THE MEASUREMENTOF SIZE, SHAPE, AND STRAIN OF CRYSTALLINE DOMAINS, AND THE CHARACTERISATION OF DEFECTS AND IMPURITIES. NURHIDAYAH KASIM S62153 THE SAMPLE IS BOMBARDED WITH X-RAYS, AND THE RESULTING DIFFRACTION PATTERN IS ANALYSED TO DETERMINE THE CRYSTAL STRUCTURE. THIS PROCESS INVOLVES SHINING AN X-RAY BEAM ONTO A SAMPLE AND MEASURING THE RESULTING DIFFRACTION PATTERN. THE DIFFRACTION PATTERN IS THEN ANALYSED USING DE-BYE SCHERRER'S EQUATION TO DETERMINE THE CRYSTAL STRUCTURE OF THE SAMPLE. ELECTRONS EMITTED BY AN ELECTRON GUN ARE FIRST ACCELARATED IN A LINEAR ACCELERATOR (LINAC) AND THEN TRANSMITTED TO A CIRCULAR ACCELERATOR (BOOSTER SYNCHROTRON) WHERE THEY ARE ACCELERATED TO REACH A HIGH ENERGY LEVEL. THEY CIRCULATE IN A VACUUM ENVIRONMENT, AT A CONSTANT ENERGY, FOR MANY HOURS. IT WORKS ON THE PRINCIPLE THAT ENERGY IS EMITTED WHEN A MOVING ELECTRON CHANGES ITS DIRECTION. THE HIGH ENERGY BEAM (4.5 KEV TO 23 KEV) IS COMBINED WITH A SIX-CIRCLE Ψ GONIOMETER FOR MEASUREMENT OF THIN FILMS AS WELL AS SINGLE AND POLYCRYSTALLINE MATERIALS. THE X-RAYS ARE DIRECTED AT A SAMPLE AND THE DIFFRACTION PATTERN CREATED BY THE INTERACTION OF THE X-RAYS WITH THE SAMPLE IS ANALYSED TO DETERMINE THE ARRANGEMENT OF ATOMS IN THE SAMPLE.


Laboratory XRD vs. Synchrotron XRD Laboratory XRD Synchrotron XRD Produce monochromatic Less intense ray Less sensitive Low depth of penetration Low spatia; resolution X-Ray is produced from X-Ray accelerated electron in cathode ray tube. Produce white X-Ray (variety of energies) More intense ray Highly sensitive High depth of penetration High spatial resolution X-Ray is produced from accelerated electron near the speed of light in a storage ring. Aderton, D. (2021). X-ray diffraction (XRD). Encyclopedia of Geology (2nd Ed.). Academic Press, 520-531. https://doi.org/10.1016/B978-0-08-102908-4.00178-8. Retrieved from https://www.veqter.co.uk/residual-stress-measurement/synchrotron-diffraction . Reference: 1. 2.


Consist of an X-ray tubes, a sample holder, a detector and a data acquisition system. An X-ray tubes(Cu-anode), which generates X rays. A sample holder, where the sample is placed. A detector, which record the diffraction pattern A computer, which process the data and generates the diffraction pattern. Consist of a synchrotron, a beamline and a detector. A synchrotron source, which generates intense A beamlines, which transport the X-rays from the synchrotron to the experimental station A detector, which records the diffraction pattern A computer, which processes the data and generates the diffraction pattern. Uses a conventional x-ray source, such as a Cu anode X-ray tube. The operator loads the sample onto the sample holder and aligns it with the X-ray beam. Then the diffractometer adjusted to the appropriate angle and X-ray directed to the sample. The diffraction would be detected by detector and being processes by computer. Uses x-rays generated by a synchrotron. The operator load the sample into the sample environment and aligns it with the X-ray beam. The beamlines transport the X-rays from the synchrotron to the experimental station. Then the diffractometer adjusted to the appropriate angle and X-ray directed to the sample. The diffraction would be detected by detector and being processes by computer. Used for determining the crystal structure of known materials, the identification of unknown compounds and for the analysis of powders, thin film and single crystals. Measuring the purity and crystalline perfection of materials Measuring the amount of a particular phase in a sample Used for the analysis of small crystal, low dimensional materials, surfaces, interfaces and dynamic processes. Determining the crystal structure of materials at high pressures and temperatures Determining the crystal structure of powder and amorphous materials Determining the crystal structure of samples that are sensitive to radiation damage. LABORATORY XRD SYNCHROTRON XRD Construction OPERATION FUNCTIONS REFFERENCES : de Matos, P. R., Neto, J. S. A., Jansen, D., Angeles, G., Kirchheim, A. P., & Campos, C. E. (2022). In-situ laboratory X-ray diffraction applied to assess cement hydration. Cement and Concrete Research, 162, 106988. Liu, L., Chen, L., Huang, X., Yang, X. Q., Yoon, W. S., Lee, H. S., & McBreen, J. (2004). Electrochemical and In Situ Synchrotron XRD Studies on Al2 O 3-Coated LiCoO2 Cathode Material. Journal of The Electrochemical Society, 151(9), A1344. REFFERENCES : S 6 3 6 2 7 A M I N B I N A N N A S


Laboratory XRD vs. Synchrotron XRD 1. Burnley, P. (n.d.). Synchrotron X-Ray Diffraction. Teach the Earth. https://serc.carleton.edu/NAGTWorkshops/mineralogy/mineral_physics/synchrotron_xrd.html 2. Dutrow, B. L., & Clark, C. M. (n.d.). X-ray Powder Diffraction (XRD). Integrating Research and Education. https://serc.carleton.edu/research_education/geochemsheets/techniques/XRD.html 3. Introduction to Synchrotron Powder Diffraction. (n.d.). Course Index for Powder Diffraction on the Web. http://pd.chem.ucl.ac.uk/pdnn/inst2/intro.htm Cathode ray tube Synchrotron (cyclic particle accelerator) X-ray generation Lower Beam intensity Higher pre-sample monochromator Monochromatisation Beam-path monochromator No need for focussing geometry (inaccurate at low angles) highly selective wavelength without fearing intensity insufficiency relatively divergent Beam resolution Nearly parallel (generally) unambiguous Function mineral determination More precise characterisation of crystalline materials QFZ3073 Solid State Science Assignment 2 Lim Wei Liang (S61613)


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