Industrial Applications of Synchrotron Radiation Non

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Industrial Applications of Synchrotron Radiation
Non-destructive testing
Characteristics of aircraft and automotive components such as strength and resistance to extreme
conditions for welded areas - for example, their response to thermal and mechanical and chemical
strain are investigated using synchrotron radiation. X-ray diffraction (XRD) and high-resolution
microtomography are used to detect implications of residual stress. Synchrotron radiation can also
be used for three-dimensional imaging based in absorption, scattering and phase.
Phase microtomography is able to provide 3D information of nucleation and propagation of small
fatigue cracks in load bearing components such as wings or skins in aircrafts, rails, car wheels,
bearings. For example in cast Al alloys, cracks of length in the 10 μm scale are able to be imaged in
high-resolution, with a voxel size of 0.7 μm.
(J. Baruchel et al, Scripta Materialia 55 (2006) 41 - 46)
These cracks in aircraft aluminium alloys have been observed to arise from atmospheric corrosion
which can begin as pitting and intergranular corrosion and can develop into fatigue cracks, stress
corrosion cracks or exfoliation. Extensive work has been done using x-ray tomography to monitor
the extent of corrosion attack due to different relative humidities and growth of intergranular
corrosion under salt droplets on Al alloys.
(S. Knight et al, Corrosion Science 53 (2011) 727 - 734)
Investigation of porous media is important as they are of interest as lightweight metallic foams or as
open structures in solid oxide fuel cells where they determine the gas flow, as well as for use as
hydrogen storage in metal organic frameworks.
An example of this is the case of syntactic foams used in the oil industry to thermally insulate the
pipes transporting hot oil from the extraction fields at a high depth in the cold sea water. The pipes
have to prevent the oil from cooling down, and must also resist a 30 MPa hydrostatic pressure. They
are composed of a polymer matrix surrounding hollow silica spheres reinforcing the porous
structure and preventing it from collapsing under the applied pressure. As these materials are made
of air, silica and polymer they are very difficult to observe using standard microscopy techniques,
however synchrotron high resolution tomography has been used for this purpose. The determination
of the thickness of the hollow spheres (in general in the range 1 – 3 μm) is very important for
understanding the physical properties of the material and this was able to be measured to 0.28 μm
resolution at ESRF, as shown in Fig. 1.
(J. Baruchel et al, Scripta Materialia 55 (2006) 41 - 46)
Tomographic slice of a polymer foam containing hollow silica spheres using (left) a 0.7 μm
voxel size and (right) a 0.28 μm voxel size.
Figure 1:
Imaging of soft tissues cannot be performed using conventional x-ray transmission radiography,
however a relatively new form of radiography known as Phase-contrast imaging has been
developed using synchrotron radiation which brings additional information by diffraction and
interference effects in the wave-nature properties of photon beams which are induced by traversing
media with varying refractive indices.
This tecnology has been able to create high resolution x-ray images of soft tissue structures such as
insects with structural details visible in the 10 – 100 μm range. Tomographic images of small
structures such as mouse kidneys and termite heads are also able to be generated. Further
developments are possible including in-vivo and time dependant studies in biological species with
applications in dental imaging and mammography.
(J. Jakubek et al, Nucl. Inst. Meth. A, 571 (2007) 69 – 72)
A study was made on the capabilities of phase-contrast imaging for real breast tumours and it was
found that in all cases, phase-contrast images showed a higher quality than those obtained using
conventional x-ray absorption imaging, demonstrating that significant benefits in the detection of
breast tumours can be obtained by means of this technique. It was also found that changing the
beam energy allows the possibility of either reducing the delivered dose while preserving image
quality, or of increasing image quality while keeping the delivered dose, and that a new trade-off
between energy and dose has to be indentified according to the specific requirements.
(A. Olivo et al, Applied Radiation and Isotopes, 67 (2009) 1033 - 1041)
The effects of inhalation of various atmospheric particles on the lungs of mice, phase-contrast
imaging was used to to image lung injuries caused by inhalation of vehicle exhaust fumes and
metallurgic plant emissions in mice. It was found that in vivo studies of living animals can easily be
performed and lung injuries caused by air particles from different areas could be distinguished.
From the images of excised tissues, not only hemorrhage spots could be seen, but also the changes
of detailed structures such as alveoli and blood vessels. The lung inflammation caused by particles
collected in a traffic tunnel was the most serious, followed by those from an industrial area and
those from a suburban area. The lung injury process caused by such particles is alveolus wall
thickening, hemorrages appearing, alveolus structures damaging and finally fibrosis. These results
suggest that phase-contrast imaging is a promising technique for diagnosis of pnemonia.
(W. Yue et al, Nucl. Inst. Meth. B, 262 (2007) 304 – 312)
Phase-contrast was recently used to study the respirator system of insects which has in the past been
very difficult to understand due to the immense variation and complexity in insect anatomy and
fundamental questions regarding the relative roles of convection and diffusion as a function of body
size, phylogeny, development and life history were unanswered. Synchrotron x-ray imaging was
Figure 2: High quality phase-contrast x-ray image of an ant worker. The round structures in the ant's abdomen are air bubbles.
able to observe in real time the tracheal system of intact, living insects and is a powerful tool for
understanding the internal dynamics involved in respiration. It enables the direct visualisation of the
insides of living animals with high spatial and temporal resolution and data collection can be
relatively quick and simple. An example is shown in Fig. 2.
(J. Socha et al, Respiratory Physiology & Neurobiology 173S (2010) S65 - S73)
Phase-contrast imaging was applied to material science with high resolution imaging of an
aerospace material comprising two thin sheets of aluminium separated by an epoxy film adhesive,
with voids in the adhesive of size 100 μm clearly visible. Furthermore images of a 50 μm Ni foil
containing air bubbles and thin glass fibres were recorded as well as a 75 μm thick polyimide film
with a 40 μm period structure of depth 20 μm. Further objects of interest included a section of a
succulent leaf and a feather showing very highly resolved features.
(A. Stevenson et al, Nucl. Inst. Meth. A 199 (2003) 427 – 435)
Industrial uses of synchrotron imaging in the rapidly growing field of nanotechnology include
detection of microcracks, voids and failures in electronics, products of the metallurgy industry,
aerospace and automobile components, new products from energy companys, building materials,
petroleum and mining equipment. Nano- and micromorphology in functional glasses and glassceramics, buliding materials, plastics, cosmetics, wood and pulp, foods, drugs and tissues are also of
interest.
X-ray Fluorescence (XRF)
X-ray Fluorescence (XRF) using synchrotron radiation can be used to perform trace element
analysis to determine concentrations of impurity elements in materials of interest with a wide range
of application.
Such analysis is important in silicon circuit technology as metallic impurities can lead to leakage
current, gate insulator breakdown or poor threshold voltage control, and the semiconductor industry
has certain requirements with respect to trace-element concentrations in their components.
Measurements have been performed at Hasylab (Beam L) to quantify the concentration of Ni
impurities in Si-wafers with a detection limit of 15 fg (1 fg = 10 -15 g) ie 109 atoms cm-2. An example
is shown in Fig. 3. This technique has become so valuable that a joint ESRF/industry initiative is
funding a specially dedicated experimental station for these investigations.
(P. Wobrauschek et al, Spectrochimica Acta Part B 52 (1997) 901 - 906)
Figure 3:
XRF spectrum of 10 pg of Ni on a Si-wafer.
Trace elemental analysis for low-Z elements is also very important in Si wafer surfaces and
synchrotron radiation has been used for total reflection x-ray fluorescence analysis (TXRF) to
measure concentrations of Na, Mg and Al impurities. These atoms are very difficult to detect with
conventional x-ray sources as the x-ray emission energies are far higher than the element's
absorption edges, and also due to interference from heavier element's overlapping secondary
absorption edges. It was reported that using synchrotron radiation, the detection limits for Mg are
0.07 pg / 1.7 x 109 atoms/cm-2 compared to 90 pg / 2.3 x 109 atoms/cm-2 for conventional Cr-tube xray sources and 7 pg / 1.8 x 1011 atoms/cm-2 for Si-tube x-rays. Trace elemental concentrations of
Na, Mg and Al in Si wafer surfaces were thereby measured using TXRF and lower detection levels
of 200, 125 and 500 fg were obtained respectively. Angle-dependant TXRF was also used to
measure depth profiles of Al impurities in Si wafers in the range 5 – 20 nm.
(C. Streli et al, Spectrochimica Acta Part B 54 (1999) 1433 - 1441)
XRF has also been used to perform trace elemental analysis on large synthetic diamonds grown in
Japan from metallic solvents. Commonly incorporated metallic impurities are Cr, Mn, Fe, Co and
Ni and these have received great attention for obtaining impurity controlled crystals. In one article,
measurements are described in which the concentrations of Co in synthetic diamonds were
compared for diamonds grown with different starting conditions, and XANES measurements were
also performed to identify the lattice positions which the Co impurities occupy within the diamond
matrix.
(S. Hayakawa et al, Journal of Crystal Growth 210 (2000) 388 – 394)
XRF measurements were made on aerosol particles found in air samples obtained from an urban
site in Switzerland. For the evaluation of the influence of atmospheric aerosols on human health (eg
the toxicity of a material when inhaled) and the dispersion via atmospheric transport, knowledge
about the composition and size distribution is required. Such particles (around 0.1 – 1.0 μm in
diameter) deposit slowly within a few days of precipitation and can therefore be transported over
long distances, having effects in regions remote from the source. Furthermore, particle size and
shape are key factors that control the extent of the penetration into the human respiratory system.
Samples of air from central Zürich were analysed to measure via XRF the concentrations of 23
elements within aerosol particles of various sizes in the range 0.1 – 1.0 μm. Elements with Z = 13 –
24 were measured at the Swiss Light Source whereas elements with Z = 25 – 82 were measured at
beamline L at Hasylab. Eight different sources were identified for the particles – secondary sulfate,
wood combustion, fireworks, road traffic, mineral dust, de-icing salt, industrial and anthropogenic
activities and many conclusions could be made about the distances travelled and daily variation of
their concentration levels.
(A. Richard et al. Atmos. Chem. Phys., 11 (2011) 8945 - 8963)
XRF has been used for biological studies, for example in the investigation of the causes of
Alzheimer's Disease (AD) which is characterised by the misfolding and plaque-like accumulation of
a naturally occurring peptide in the brain called amyloid beta (Aβ). The Aβ peptide ranges in length
from 39 - 43 animo acids, and in AD plaques it is the major constituent. These plaques are formed
due to the transformation of Aβ from a soluable form to an aggregated, fibrillary structure that is
neurotoxic and there is increasing evidence that interactions between Aβ and metals such as Cu and
Fe play a role in this transformation. It is thought that the strongly redox-active Aβ reduces Fe3+ and
Cu2+ which produces H2O2 in the presence of oxygen. H2O2 is a source of toxicity in neuronal
damage, however it has also been found that the presence of the redox-inert Zn binds the Aβ,
preventing the reduction of Cu2+ and reducing the formation of H2O2. Therefore a direct anaylsis of
Aβ and metal ions in AD patients is essential to fully understand this process of AD development
and for potential future preventions and treatments.
XRF was used to image trace-elements of Ca, Fe, Cu and Zn in areas of brain tissue from patients
with confirmed AD, which had been previously imaged with synchrotron Fourier transform infrared
microspectroscopy (FTIRM – which is used for imaging fibrillary Aβ deposits in brain tissue). A
homogeneous distribution of Zn, Cu, Fe and Ca were found in the AD brain tissue, exhibiting “hot
spots” of high metal content. A strong correlation was found between Cu, Zn and Aβ location which
are consistant for a protective role for Zn2+ in AD, where plaques form as the result of an
antioxidant response for the underlying oxidative attack. These results and further studies involving
analysis of earlier stages of the disease will be useful in accessing the sequence of events that leads
to co-localisation of Cu, Zn in Aβ plaques in AD.
(L. Miller et al., Journal of Structural Biology 155 (2006) 30 - 37)
A second group has performed trace element distribution analysis in the brain sections of rats using
XRF with the aim of measuring the effects of iodine deficiency on concentrations of trace elements
of P, S, Cl, K, Ca, Fe, Cu, Zn, Br, Rb in the thalamus, cerebral cortex and hippocampus. The study
found several interesting effects, for example that Zn is concentrated along the hippocampal fissure
in rat brain and that iodine deficiency leads to marked alterations in the spatial distribution of Zn
and Ca during brain development stages, but more experiments were planned to confirm and
explain such observations.
(Liu et al., Spectrochimica Acta Part B 59 (2004) 255 - 260)
Trace element analysis using synchrotron XRF also finds application in forensic science, for
example the analysis of minute glass fragments found at crime scenes which can serve as one of the
most important evidentiary materials in identification of the culprit in criminal cases such as hitand-run, theft and murder. Measurements were made at the Japanese synchrotron and the lower
limits of detection for the elements of Ca, Fe, Sr, Zr, Sn, Ba, Ce, Sm, Hf were measured and range
from 0.5 – 50 ng in a spot-size smaller than the beam diameter of 500 μm x 500 μm. Small
fragments of six different types of glass were successfully discriminated using this method
demonstrating the power of XRF in forensic science.
(T. Nakanishi et al., Forensic Science International 175 (2008) 227 - 234)
XRF is also used in ecological studies, for example in the study of the life histories of yellow and
silver eels collected in marine and fresh water in Asia which can provide a key to understanding the
evolutionary process of fish migration as well as providing a record of changes in the elements
present in the environment during a fish's lifespan. This is performed by analysis of the inner ear of
a fish which contains two tiny particles of CaCO3 called otoliths which function as the organ of
equilibrium. The otoliths increase in size as the fish age, and the water environment is the source of
Ca and CO3 that constitute their makeup. It is thought that CaCO3 precipitates together with traceelements from the environment during daily growth increments. It is known that the Sr content of
seawater is more than 100 times higher than that in freshwater, therefore Sr/Ca ratios were
measured for common eels found at different locations. It was observed that the otoliths of a typical
Japanese eel found in the Uono river have a Sr-rich core and a Sr-deficient region in the outer layers
which indicates the juvenile fish migrated from the sea to fresh water for the remainder of its life.
Conversely, all specimens collected in the East China Sea and the North Sea show a secondary
peripheral region of elevated Sr which was not observed in the river specimens, indicating that the
fish did not spend their juvenile and adult lives in freshwater. It is thought that sea-residency of
freshwater eels would occur more frequently at higher latitudes where the food availability in
freshwater habitats is lower than in adjacent coastal regions.
(I. Nakia et al, Spectrochimica Acta Part B, 54 (1999) 167 - 170)
Figure 4: 2D XRF imaging of trace elements in otolith. The XRF intensity of each element was normalised to that of Ca with black being highest and
white the lowest intensities. (Left) Sr/Ca and (centre) P/Ca ratio of an otolith of an eel collected at Uono river and (right) Sr/Ca ratio of otolith of an
eel caught in the East China sea.
A popular use of XRF analysis is for the study of ancient and historical items. XRF is used for
elemental analysis of specimens while X-ray absorption spectroscopy (XAS) gives information on
local structure around selected elements. These methods have been combined to perform
investigations on items of cultural heritage (paintings, statues, ceramics), for example:
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identification of materials used, how to preserve them
to detect fraud or alterations to a specimen
analysis of inks used in a particular area and time period
origin of stones used in statues
techniques used in early steel making
restoration of faded/erased ink in old manuscripts
Industrial uses of synchrotron XRF in the rapidly growing field of nanotechnology include
determination of the distribution of elements in electronics, products from energy company,
building materials, plastics, cosmetics, wood and pulp, foods, pharmeceuticals and biological
structures.
X-ray Absorption Spectroscopy
X-ray Absorption Spectroscopy (XAS) and the related X-ray Absorption Near Edge Structure
(XANES) and Extended X-ray Absorption Fine Structure (EXAFS) are useful tools for
characterising the local environment (coordination number and interatomic distance) and the
electronic state of an element within a sample of interest.
These techniques find application in the development of catalysts for a very broad range of
chemical reactions. The ultimate goal is to obtain significant structural and electronic characteristics
which can be correlated to the catalytic activity in a given reaction.
One example has been the analysis of Co based catalysts for Fischer-Tropsch synthesis which is a
series of chemical reactions that convert a mixture of CO and H into liquid hydrocarbons and
produces a synthetic lubrication oil and synthetic fuel, typically from coal, natural gas or biomass.
Several studies have been focussed on the catalytic nature of Co species using many experimental
techniques but little has been concluded about the electronic state of the Co ions, even though this is
a key issue in understanding the mechanism of the CO hydrogenation. In one study, Co containing
catalysts were analysed using L-edge XANES and the absorption spectra were compared to those
obtained for several Co containing reference samples. It was found that one catalyst sample was
associated with the presence of large clusters of Co3O4 whereas another had an amorphous structure
similar to Co2SiO4. Heating of the Co3O4 containing sample in a reducing atmosphere up to 500 °C
resulted in a reduction of the Co3O4 clusters as well as a disappearance of the fine structure of the
Co absorption spectrum which could be caused by disorder in the first coordination sphere of Co
atoms. The significant information gained from this particular result can be utilised to link structural
characteristics to the catalytic activity as well as being a challenge for theoretical physics.
A further example was the investigation of the environment of sulfur in organic substances in
experiments designed to emulate the maturation of organic matter in petroleum reservoirs at
moderate temperatures over geological time scales. These emulations are performed at high
temperatures for a faster maturation time, and in the case of iron containing kerogenes (organic
chemical compounds that make up a portion of the organic matter in sedimentary rocks and are a
source of fossil fuels) the quantity of H2S may be increased or decreased due to a number of factors
and so sulfur K-edge XANES was used to fingerprint the forms of sulfur in these organic
compounds. Elemental analysis and percentage of sulfur in different forms were thereby measured
and some insight was given into the processes governing hydrocarbon formation in petroleum
reserves.
(D. Bazin et al, Applied Catalysis A: General, 213 (2001) 147 - 162)
XAS was also used to investigate the environments of Cr, Cu and Zn in corroded and uncorroded
aluminium alloys used in aerospace frames, skins and structural members. It is of interest to extend
the life of aerospace components as much as possible, so samples of an aluminium alloy (7175
T736 aluminium) were analysed with XAS in an uncorroded form as well as a sample which had
been stored for 9.8 years in an uncontrolled environment. It was found that only the Cu site
significantly changed during corrosion, however no chemical shift was observed and nor was the
presence of Cu compounds found. Using XANES and EXAFS it was concluded that about 20% of
the Cu atoms sampled was present as disordered, metallic Cu after corrosion, and furthermore in the
surfaces of corroded areas, high concentrations of Al2O3/Al(OH)3 are present. These findings are
consistent with galvanic corrosion due to the presence of water.
(R. Greegor et al. Corrosion Science, 39, 12 (1997) 2095 - 2116)
XANES spectroscopy was also used in the analysis of rubber tyres in which the state of sulfurcrosslink distribution and crosslink density can be characterised. These arise during the
vulcanisation process and oxidative-aging processes take place at the cross-links.
(Hormes et al Nucl. Inst. Meth. A 467-468 (2001) 1179 – 1191)
XAS was used in conjunction with XRD and XRF to investigate the chemistry of yellow ancient
tile glazes (17th – 19th century) which have deteriorated due to atmospheric conditions and should
be restored, therefore a concise knowledge about the basic materials and colourants is used so that
only conformable new products are used. The measurements were able to show the presence of Pb
and Sb in fragments of tile glazes and the general conclusion about the constitution of the yellow
glazes of the ancient tiles is that Pb is hosted in the glassy matrix while the actual colouring agent
being a dispersed Sb-pyrochlore phase.
(M. Figueiredo et al, Nucl. Inst. Meth. B, 238 (2005) 134 –137)
The famous Maya blue pigmentation developed by the Mayan people has been studied in depth due
to its brilliant Caribbean sea blue colour which has exhibited remarkable durability for over 1000
years despite exposure to the harsh environmental conditions of the Yucatan peninsula and is
resistant to acids, alkalis, organic solvents and biological degradation. This pigmentation has been
emulated in modern times by heating a mixture of palygotskite clay with indigo at 150 °C for two
days which produces a Maya blue color with identical physical and chemical properties to field
samples. It is of interest to study these systems not just for the ability to produce blue pigmentation
from environmentally safer starting materials, but also to gain insight to the technology transfer
within the Mayan civilisation. Samples of ancient and synthetic samples were analysed with
XANES and EXAFS to study the chemical nature of iron and iron nanoparticles detected using
Transmission Electron Microscopy. It was found in that in authentic Maya blue samples Fe3+ is the
dominant oxidation state and one sample contained 25% Fe2O3 + 75% FeO(OH) and approximately
100% FeO(OH) in a second. Simulation analysis of Fe EXAFS from the latter sample found a
disordered structure in which coordination spheres with noticeable differences from those observed
in authentic FeO(OH). It was concluded that the Fe oxide phase present in this sample is probably
incompletely hydrated and is transitional from Fe2O3 to FeO(OH). The original Maya blue may
have contained only Fe2O3 that was converted to FeO(OH) due to heat and ambient moisture in the
Yucatan region.
(L. Polette et al, Microchemical Journal, 71 (2002) 167 - 174)
Industrial uses of synchrotron absorption spectroscopy in the rapidly growing field of
nanotechnology include analysis of surfaces and local chemical environments in electronics,
products of the metallurgy industry, functional glasses and glass-ceramics and plastics; aging
processes in products from energy companys and building materials. Characterisation of catalysis
processes in petrochemistry is also of interest.
Synchrotron X-ray Diffraction (XRD)
X-ray diffraction (XRD) using synchrotron radiation is advantageous over conventional x-ray
sources as higher resolution patterns can be obtained which can be used to resolve more difficult
space group or symmetry problems, or can more easily identify minority phases present in samples.
Structural properties of Mg and Mg alloys are of interest due to their potential application as
lightweight materials for air-space, aviation and automotive-industry applications, for example
Volkswagen proposed a prototype of a weight reduced car (about 290 kg) with much lower gasoline
consumption. To begin such a project, several different types of Mg alloy and Mg reinforced
composites were prepared from Mg grains of size 30 μm compacted into cylindrical rods and global
and local texture measurements were made using synchrotron XRD at DESY.
(H.-G. Brokmeier et al, ICDD 2003 – Advances in X-ray Analysis 46)
Further examples of studied materials and applications of XRD:
The Boeing Corporation used synchrotron XRD to develop lightweight components in the form of
polyethyl ether Ketone resins substituted with Al with no strength loss, resulting in significant
weight reductions in its 757 aircraft.
Chemical companies use synchrotron radiation to investigate the synthesis and properties of new
catalysts which are used in almost all chemical engineering processes. Fine particles can be
observed down to the nanoscale which is useful in the study of chemical processes such as
combustion in real time. Two examples of this are:
Analysis of Ni exchanged zeolite Y (a catalyst for production of benzene from acetylene)
which needs to be heated to 200 °C for approx. 2 hours to begin to catalyse. High resolution XRD
was performed on the sample during the heating process and the migration of Ni 2+-ions from a
catalytically inactive lattice site to a catalytically active “supercage” site was observable (using
Rietveld refinement) which demonstrates not only the power of the powder diffraction technique
but also how physical chemists are approaching a better understanding of the catalytic process.
Analysis of rare-earth doped oyrochore catalysts used in converting CO2 and CH4
greenhouse gases into useful chemical feedstock.
Synchrotron powder diffraction is very useful for rapid diffraction data capture on time dependant
systems, such as hydration of various systems. For example, a study on hydration properties in
cement mixes was performed in which diffraction date was obtained every 10 s on a “mini cement
mixer” setup in the experimental station and conclusions were able to be made about the rate at
which the main hydration product in cement (a calcium sulfo-aluminate hydrate or “ettringite”)
starts to form (ie within the first 10 s of mixing). The unit cell a-parameter of this crystal phase
observed to increase by a factor of 0.7% over a longer time period which is consistent with a
substitution of 50 - 70% of the sulfate groups by hydroxy/carboxy groups, demonstrating how such
measurements can be used to clarify the nature of complex hydration processes.
(R. Cernik et al, Rad. Phys. Chem 45 (3) (1995) 445 - 457)
More recently, hydration processes of ordinary portland cement (OPC) have been investigated using
high-resolution synchrotron XRD to analyse the early formation of ettringite and the effects of
additives such as retarding admixtures and superplasticisers (which optimise the flow properties of
cement and reduce the water/cement ratio providing higher compressive strength) on the
millisecond timescale. These additives have been found to be most influential during the first
minutes of hydration.
Measurements were made on pure OPC as well as OPC containing polycarboxylate ethers (PCEs)
with differing charge densities. PCEs are commonly used superplasticisers with strong dispersion
effects which arise from charge and adsorption effects during the cement hydration.
During the measurements, XRD measurements were performed every few milliseconds and the
(100) diffraction peak of ettringite was observed for each sample. It was found that in pure OPC,
the concentration of ettringite increases exponentially over the whole time of hydration whereas for
those containing PCEs, the rate of increase is significantly decreases while liquid water remained in
the mixture and was not absorbed by the cement. Using this method, a model of the inhibition of the
ettringite formation process by PCEs was able to be formulated.
(M.-C. Schlegel et al, Angew. Chem. Int. Ed. 51 (2012) 1 - 5)
Industrial uses of synchrotron XRD in the rapidly growing field of nanotechnology include analysis
of stress and detection of point defects in electronics, detection of stress gradients and nanoclusters
in alloys, local crystalline ordering in advanced glasses and glass-ceramics, phase identification and
corrosion processes in new products from energy companies, identification of deposits and colloidal
particles in oils and observations of chemical transformation and crystallisation in petrochemistry.
Nanomorphology of gels and emulsions for cosmetics and their effects in tissues on the molecular
level are also of interest, as well as stability and aging of foods and protein-drug interactions.
Studies of crystals with large unit cell dimensions (biological molecules)
Pharmaceutical companies use synchrotron radiation for the determination of biological structures
ranging from small peptides to the ribosome to entire viruses which is essential for the
understanding of biological processes and for developing treatment of diseases and the design of
many drugs.
Brilliant synchrotron sources offer major advantages over laboratory sources for the study of
crystals with large cell dimension (eg exceeding 1000 Å). Using protein crystallography
techniques,the crystal structures of more than 61840 proteins, nucleic acids and other biological
molecules have been determined, compared to the next most widely used technique, nuclear
magnetic resonance, which has resolved 8759 chemical structures. For example, the structure of
many viruses have been solved at high resolution, eg the human rhino virus 3 at 3.0 Å resolution,
the human rhino virus 16 at 2.15 Å resolution, the bacteriophage Qβ at 3.5 Å resolution, the simian
virus 40 at 3.1 Å resolution among many others.
(K. Moffat et al, Current Opinion in Structural Biology 7 (1997) 689-696)
UV-VIS Spectroscopy
Dedicated synchrotron generated UV beamlines like SUPERLUMI at DESY is heavily used in the
development of luminescent materials used for radiation detectors, new light sources, lamp
phosphors and persistant phosphors. Such measurements are required for the understanding of
intrinsic and extrinsic luminescent mechanisms and optimisation of luminescence characteristics
such as luminescence intensity, scintillation lifetime and radiation stability. New scintillator
materials for x-ray and gamma detection are constantly being tested and many scintillator crystal
companies have a need for optimisation of their materials which can be performed at stations like
SUPERLUMI.
Summary
Synchrotron radiation has a very wide range of industrial application, ranging from trace-elemental
analysis in Si-wafers used in the semiconductor industry using XRF, to quality control in aircraft
components using x-ray microtomography, XRD and XAS to real time analysis of structural
changes in materials using XRD, the use of protein crystallography for structural analysis of a host
of biological molecules and many examples of the analysis of ancient and historical materials.
The first industrial partners that should be contacted are therefore members of the aerospace,
aviation and automotive industries, the oil industry, manufacturers of electronics, pharmaceutical
companies and perhaps to a lesser extent cement manufacturers, forensics labs, medical research
companies, manufacturers of luminescent materials.
Graham Appleby
19.04.2012
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