Synchrotron light has many applications in industry, helping companies to reach new frontiers in their R&D.
A few industrial applications of synchrotron techniques are described below.
Pharmaceuticals and biotechnology
Pharmaceutical and biotech companies use synchrotron techniques to help develop new products at all stages of research, from drug design and formulation to pre-clinical phases.
1. Drug Design
- Rapid data collection, even from very small crystals (5 µm) and to a higher resolution than conventional X-ray sources
- 3D structure determination of proteins whether they are crystals or semi-crystalline using our powerful and fully automated protein crystallography beamlines
- Phase diagrams of complex formulation by analysing their rheological properties
- Understanding of the physico-chemical properties of a drug with excipients
- Evaluation of the stability, solubility and crystallinity of a new drug for the prototyping of formulations
- High resolution quantitative and qualitative composition of a whole formulation even at ultradilute concentration
- Determination of polymorphism and pseudo-polymorphism of molecule within a whole formulation
3. Pre-clinical tests
- Investigation of the concentration effect of a drug or a marker in mammography or in the diagnosis of asthma
- Targeted irradiation of tumour cells
Press article: "From the ESRF to the Pharmacy"
Automotive industries are concentrating much of their effort in obtaining more efficient catalytic exhaust converters, which simultaneously transform the three main polluting emissions - nitrogen oxides (NOx), carbon monoxide (CO) and unburned hydrocarbons - into nitrogen (N2), carbon dioxide (CO2) and water (H2O). The development of catalytic converters was instigated in the mid-70's when environmental laws pressurised the car industry to cut down the amount of harmful emissions. Nowadays, the direction of this research is mainly dictated by such global environmental legislations that demand higher and higher standards. X-ray Absorption Spectroscopy (XAS) has demonstrated to be a powerful technique to study physical and chemical properties of catalytic surfaces. However, conventional XAS renders data for ex-situ experiments, providing static information. At the ESRF, it is possible to perform dynamic and in-situ experiments, but most important, these experiments can be followed down to the millisecond regime. The combination of these characteristics is a major advantage of the ESRF, one of the most advanced facilities in the world. The capability to study very fast reactions is crucial for the analysis of catalytic converters because the oxidation and reduction cycles at which they are submitted occur in less than one second.
The perfection and purity of the silicon wafers used to produce semiconductors is critical to device performance. Acceptable metallic contamination levels are now below 108 atoms/cm2. Conventional trace element analysis is inadequate for such low levels. The synchrotron techniques of imaging, microtomography, topography, microscopy RX and FTIR microscopy using the high-brilliance ESRF beams, easily exceed this trace detection level and are commonly used for the study of inclusions in surfaces or identification of a defect on silicon wafers.
- Improve the mechanical and temperature resistance of fuel cell membranes (PEMFC, SOFC),
- Improve fuel cell catalysts (Pt, Pd, Rh, Ru)
- Control the degree of hydration of fuel cell membranes
- Reduce the costs of materials by process optimisation
- Improve the conductivity of your materials
Applicable synchrotron techniques:
Synchrotron X-ray diffraction is a unique technique
- To monitor the local structure changes of a fuel cell membrane (SOFC or PEMFC) during oxydation / reduction cycles
- To determine the in situ hydration process in a polymeric membrane (PEMFC) as a function of time
- To monitor thermal evolutions of crystal structures of a fast oxide-ion conductor used as solid electrolytes in SOFC
- To characterise in situ fuel cell catalysts (Pt, Pd, Ru, Rh) by providing information on the oxidation state, local coordination and distance of neighbours surrounding the absorbing atom
- To perform qualitative and quantitative measurements at millisecond time resolution with concentrations ranging from ppm to weight percent
- To study the hydration degree of membranes (PEMFC)
- To characterise nanomaterials (metal oxide or alloy crystallites) and improve catalyst selectivity
- To study the swelling behaviour of fuel cell membranes
- To analyse the nanostructure of membranes during aging
- For 3D images of the inner part of your material, nanoparticles, morphology of pores, fixation sites within a matrix with a 0.28 μm pixel size.
With the 21st century, and the rarefaction of petroleum reserves, the time has arrived to enhance the value of each atom of carbon of each drop of oil. The consequence of such an increase of the value of crude oil is of course a need to enhance our knowledge, if possible down to an atomic scale, of oil products and catalysts. Here, the use of synchrotron radiation has proven to be very useful because of the wide ranging and powerful analytical information they provide.
The different steps where synchrotron radiation applies to the oil industry are:
Synchrotron radiation techniques are used for instance to improve our knowledge of source rocks by infrared microscopy analysis of fluid inclusions, to analyse trace element of crude oil in order to determine the path followed by oil during migration, to determine the behaviour of hydrates in the transport of oil at high pressure and low temperatures as a function of their structure.
2. Reservoir Engineering
The key topic here is fluid transport in porous media. Microtomography provides key information on 3D in situ distribution and flow of oil and water in oil-wet matrices.
Future oil discoveries are likely to involve drilling at depths of several kilometres, implying conditions of high temperature and high pressure that have rarely been explored up to now. Understanding transformation mechanisms under extreme conditions is thus another area in which synchrotron radiation studies can help to determine the factors limiting materials performance and in suggesting where the improvements could be made.
Pipelines increasingly transport complex mixtures of fluids (oil, water, gas and sand) from the prevailing high-temperature and high-pressure conditions of reservoirs through, for example, seabed networks. Synchrotron techniques are very useful to study the behaviour of these mixtures when submitted to changes of temperature and pressure during the transport in order to optimise this step. Small-angle X-ray scattering in particular can give information on the size and form of aggregates. Using the high intensities and rapid acquisition times available with synchrotron radiation can help in establishing kinetics of the process.
Also, microtomography promises to provide direct interpretable data to study syntactic foam structures used as a potential solution for long-term insulation of oil during transport or to understand the complexity of nanostructured polymer-clay composites used to make low permeability materials to transport the oil.
5. Refining and Petrochemistry
Crude oil is a complex mixture of many hydrocarbons. Elimination of S, N, Ni, V from crude oil is of major environmental importance. XANES is able to provide clues as to the local co-ordination of these elements and even more interesting on solid heavy oil deposits.
In the field of supported catalysts, synchrotron radiation methods have achieved important synergy in identifying structural and electronic characteristics during in situ catalytic processes. This is particularly representative on systems where the time resolution achieved with synchrotron radiation methods offer a considerable insight for the understanding of the process.
6. CO2 Sequestration
Underground sequestering of CO2 in depleted wells in order to reduce the CO2 impact on the atmosphere is under consideration. In situ synchrotron radiation XRD and microtomography can be used to predict the behaviour of cement seals used to close wells into which the gases would be injected.
C. Pichon and coll. - Oil & Gas Science and Technology - Rev. IFP, Vol 60 (2005), n°5, pp735-746.
Press release: "Growing catalysts"
Maintaining the natural balance Nature is a finely-balanced system. As we become more aware of the potentially harmful effects of many human activities, developing ways to protect our fragile environment is moving higher up society's agenda. Some ESRF users are investigating new types of “cleaner” energy. Others are analysing samples of contaminated soils and water — research that makes it possible, for example, to investigate the spread of radioactive particles resulting from nuclear accidents like Chernobyl. But not all environmental problems are man-made. Scientists at the ESRF are also studying natural phenomena such as volcanoes and avalanches in order to have a better knowledge of them, with the aim of providing a prior warning.
Modelling of snow
An increasing number of fatal accidents at winter sports resorts are caused by avalanches. In order to gain a better understanding of the avalanche phenomenon, meteorologists are carrying out detailed studies of the microscopic structure of the snow grains. Microtomography measurements carried out at the ESRF provide detailed three-dimensional information about the internal structure of the snow “blanket”. These data will be integrated into simulation programs which help in the evaluation of avalanche risks.
Metallic components are subject to considerable mechanical stress during manufacture and throughout their operating life. These stresses cause deformation strain and fatigue of the component, which affect its performance and can lead to failure.
In the aerospace, automotive and construction industries, it is essential to have a perfect knowledge of the stress/strain relationships in many components that are critical for safety and service lifetimes. X-ray strain measurement in scanning mode at the ESRF, which is a well-adapted tool for stress analysis, provides this understanding. This technique reveals the deformation strain in metals by measuring the structural deformation of the metallic lattice at the atomic level in the bulk of the sample. The stress forces are calculated from the strain map to identify zones with critical levels. The intense X-ray beams at the ESRF can be used to analyse steel to a depth of a few mm with a very high dimensional resolution.
Press release: "New insight into aluminium"
Developing new cosmetic products and assessing their effectiveness and safety for future consumers calls for very high-performance characterisation tools. As a complementary technique to electron microscopy, Small and wide-angle X-ray scattering, being non destructive, provides in-depth information on rhelogical properties of beauty creams, hair products, lipsticks or nail varnishes and their tolerance by skin or hair. By examining their nanostructure, the cosmetics engineers are able to develop more stable products with longer-lasting effects. Trace of these products trapped in the skin or in the hair can be detected by using synchrotron X-ray microscopy. X-ray tomography provides unique 3D information of such products in order to make a relation between the macroscopic properties and the micro-structure.
The food industry is constantly developing new food products to satisfy consumer trends in terms of novelty, ease of preparation and nutritional value, whilst maintaining high standards of quality. To respond to this challenge , the sector is moving away from traditional cooking towards rationalised processing. This implies a huge nutritional research effort since foods are very complex mixtures of different components with widely diverse thermal, mechanical, rheological and ageing properties. Several food companies have chosen to take advantage of the X-rays provided by the ESRF to improve existing products and explore the potential of new developments for chocolate, bread, butter, creams and drinks. Analysis of food product by X-ray tomography and Small and wide-angle X-ray scattering provide both qualitative and quantitative results which help to correlate the macroscopic properties and the micro-structure of your sample in static or dynamic mode.
Press release: "Structure of chocolate unravelled at the ESRF"
Material Science represents a wide field of research and the micro-structural characterisation of materials is needed in order to better understand the main phenomena that occur during the forming or during the use of a material. The microstructure characterisation must be carried out at the relevant scale, depending on the scientific problem. Synchrotron X-ray techniques are unique to achieve spacial resolution below the micron. The prediction of the performance of building materials exposed to aggressive environments is economically and technically important. Only by understanding the mechanisms behind the degradation can the right curative or preventive action be taken. In most cases water plays a crucial role, either directly or as a vector for other agents. Modelling water-induced ageing processes, in order to develop more resistant materials, requires a knowledge of transport coefficients. These can easily be measured for dry materials but not for wet materials. An alternative approach is to predict them from the organisation of the grains and the connectivity of the porous network. X-ray microtomography measurements at the ESRF open new and promising opportunities for visualising porous materials.
Although the discovery of hydraulic cement dates back to the early 19th century, the setting process is still not well understood. The setting of cements and concretes is a complex process involving many intermediate phases, and the understanding of the roles played by these intermediates is important for developing cements and concretes for special applications. The early stages of hydration of Portland cement are greatly influenced by the behaviour of its most reactive component, tricalcium aluminate. On contact with water, this mineral forms several hydrates and intermediate compounds, but the resulting hydration reaction is quite variable. It can be extremely rapid, but the presence of gypsum retards the process. Today, cements are somewhat empirically formulated, in order to find a compromise between fluidity and setting time. To put cement formulation onto a more scientific basis, essential for the development of new, high performance products and processes, cement companies are now engaged in extensive research efforts.
Case study: Cement
Real-time monitoring of cement hydration by X-ray diffraction
Until recently, the intermediate reaction phases formed during the setting of cements had not been directly observed because of their transient lifetime. Using the intense X-ray beams at the ESRF, Industrialists have followed the early stages of cement hydration in real time. Since the start of hydration is so fast, mixing was performed in situ in a 10 mm thick « mini cement mixer ». A series of X-ray diffraction patterns, taken at intervals of a few seconds, clearly shows that reactions start in the first few seconds after mixing. The tricalcium aluminate content decreases and transient phases form rapidly. Only 150 seconds after mixing, the transient phase has disappeared and has been replaced by the final hydrate form. The transient phase was identified from the diffraction data, which demonstrates the benefits of real-time monitoring in casting new light on old problems.
Press release: "On the way to the perfect glass"
Bulk chemical synthesis
The chemical industry is seeking for more efficient and more environmentally compatible processes for the manufacture of raw materials, monomers used in the polymer industry. Reducing the number of steps in the process together with optimising the catalytic reactions has now become a priority for companies involved in the bulk chemical synthesis. Heterogeneous Catalysis controls about 90% of the world's chemical manufacturing processes, and contributes substantially to the GNP of large industrialised economies. Yet fundamental chemical and physical mechanisms are often not completely understood and its study remains largely empirical, awaiting for a systematic investigation. Accordingly, it is in the industries' interest to invest in research in this field in order to reduce costs via improved chemical and energy efficiencies while reducing the environmental impact of chemical operations.
Synchrotron techniques at the ESRF play a major role in this context as they offer a unique way to understand the behaviour of catalytic systems.
X-ray Absorption Spectroscopy (EXAFS, XANES) provides information on the atomic organisation and chemical bonding around an absorbing atom in whatever medium it is embedded (solid, liquid, gas, surface). Qualitative and quantitative measurements during a catalysis are possible at millisecond time resolution with concentration ranging from ppm to weight percent. Our unique facility allows you to follow homogeneous or heterogeneous catalysis coupled with FT-IR and Mass spectroscopy of UV spectrophotometry to get the best of your sample.
Small-Angle and Wide-Angle X-ray Scattering provides unique information to analyse the shape, size and density of nanoparticles and the potential of interaction between particles in catalysts manufacturing processes.
X-ray Microtomography is an imaging technique useful to provide a 3D imaging of matrices and detect trace of elements at a high resolution.
X-ray Microscopy is often used to determine quantitative oxidation states of species even at ultradilute concentration.